Green and Scalable Production of Nanocrystalline Cellulose Driven by a Biomass-Derived Deep Eutectic Solvent

Green and Scalable Production of Nanocrystalline Cellulose Driven by a Biomass-Derived Deep Eutectic Solvent | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Green and Scalable Production of Nanocrystalline Cellulose Driven by a Biomass-Derived Deep Eutectic Solvent Niuniu Deng, Qiang Li, Wenjie Wang, Gengsheng Ji This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7700269/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract Agricultural residues represent a valuable renewable resource for producing sustainable functional materials. Here, we report a biomass-derived DES (Deep Eutectic Solvent) system, composed of CA–EG (Citric acid and Ethylene glycol) DES, for the selective extraction of CNC (Cellulose Nanocrystal) from agricultural straw. Operating under mild conditions, the DES efficiently disrupts the lignocellulosic network, yielding CNC with high crystallinity (72.3%) and uniform nanoscale morphology. The process achieves over 85% solvent recovery, significantly reducing chemical input and waste generation, and offers clear advantages in conversion efficiency, operational simplicity, and environmental compatibility compared to other green strategies such as [DMIM][DMP] (1,3-Dimethylimidazolium dimethyl phosphate), enzymatic hydrolysis, and TEMPO oxidation. Comprehensive structural characterization confirmed the high-quality CNC obtained, while techno-economic evaluation demonstrated the cost-effectiveness and industrial scalability of the process. This work provides an integrated, resource-efficient, and environmentally benign platform for transforming agricultural waste into high-value nanomaterials, contributing to circular material systems and the advancement of sustainable manufacturing. Agricultural Straw Biomass-Derived Deep Eutectic Solvent (DES) High Solvent Recovery Cellulose Nanocrystal Sustainable materials Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Introduction Agricultural straw, as the most abundant lignocellulosic residue generated during crop cultivation, is frequently subjected to open burning or landfill disposal, thereby exacerbating air pollution and greenhouse gas emissions 1 . Nonetheless, due to its inherent richness in cellulose, hemicellulose, and lignin, straw represents a highly promising renewable feedstock for the synthesis of advanced biomaterials. Nanocellulose (NCC) has garnered extensive interest for its remarkable crystallinity, nanoscale dimensions, and superior mechanical strength. Moreover, NCC exhibits excellent thermal stability, low density, and intrinsic biocompatibility, rendering it an ideal candidate for applications spanning high-performance composites, biomedical devices, food additives, and environmental remediation 2 . Given the urgent need to reduce reliance on fossil-based materials and mitigate environmental burdens, the development of sustainable, efficient, and economically viable routes for producing NCC from biomass residues such as straw has become increasingly important 3 . Traditionally, strong acid hydrolysis—particularly sulfuric acid—has been the most common approach for preparing NCC. Although this technique reliably produces high-crystallinity NCC, it has notable drawbacks for industrial implementation 4 . Corrosive acids inflict equipment and pipeline damage, resulting in high maintenance costs. Managing waste acids also remains challenging, as neutralization, separation, and purification are required to meet environmental discharge standards. These factors drive up operational expenses and undermine process sustainability. Consequently, researchers have investigated alternative methods—including ionic liquids, cellulases, and TEMPO (2,2,6,6-tetramethylpiperidine-1-oxyl) oxidation—that reduce corrosivity 5 , enable selective dissociation, and allow for functional modification. Nevertheless, their high solvent or enzyme costs, complex regeneration processes, and viscosity challenges hinder large-scale production 6 . Deep eutectic solvents (DES) are emerging as an attractive solution, offering low toxicity, easy preparation, and recyclability 7 . Unlike conventional ionic liquids, DES can be synthesized from inexpensive 8 , readily available materials. In comparison to traditional strong acid systems, DES typically exhibit lower corrosivity, simpler post-treatment, and reduced environmental burden. These solvents can induce cellulose swelling and, under certain conditions, dissolve cellulose by disrupting hydrogen bonds between cellulose molecules, allowing lignin and hemicellulose removal, ultimately leading to NCC production 9 . Moreover, many DES components are derived from renewable biomass or food-grade substances, further augmenting their environmental appeal 10 . Recent studies illustrate the efficacy of DES in pretreating lignocellulosic materials under mild conditions, effectively breaking hydrogen bonds among cellulose, hemicellulose, and lignin. By fine-tuning DES composition and reaction parameters, cellulose can be dissolved to facilitate subsequent chemical modifications and derivatization 11 . This results in cellulose-based materials with improved properties. Additionally, cellulose treated with DES can be converted into NCC, which demonstrates excellent dispersion and homogeneity, opening opportunities for use in composites, packaging, and medical applications 12 . Ongoing research employing structural characterization, thermal analysis, and molecular simulations continues to unveil how DES interact with cellulose, providing valuable guidance for process optimization 13 . Despite this progress, certain challenges persist. High-viscosity DES formulations can hinder mass transfer, necessitating higher temperatures or extended reaction times 14 , which may elevate energy requirements and risk excessive cellulose degradation 15 . Furthermore, impurities such as lignin and hemicellulose can accumulate during solvent recycling, altering DES composition and diminishing its performance 16 . Additionally, variations in feedstock composition create difficulties in developing a universal DES formulation suitable for all straw, wood, and pure cellulose sources. Consequently, further work is required to optimize DES systems for large-scale use, centering on process scalability, cost reduction, and environmental performance. This work focuses on evaluating the feasibility of using straw to produce NCC by comparing four methods: DES, ionic liquids, cellulases, and TEMPO oxidation. The primary objective is to evaluate the possibility of each strategy for large-scale production based on factors including energy consumption, environmental impact, and recyclability. A key aspect is refining both the composition and reaction conditions of a co-DES system—comprising citric acid and ethylene glycol—for processing straw powder. Notably, citric acid and ethylene glycol enable a more economically sustainable approach. The resultant NCC is assessed on yield, morphology, and crystallinity, while an economic analysis addresses solvent and reagent recycling, capital equipment outlays, and waste treatment methods. This holistic evaluation underscores the industrial viability and sustainability potential of each technique. Materials and Methods Materials Wheat straw was collected from Muxiang County, Suqian City, Jiangsu Province. The straw was processed with a high-speed multifunctional grinder and passed through a 100–200 mesh sieve. The sieved powder was washed 2–3 times with warm water at 50°C, allowed to settle, filtered, dried in an electric thermostatic blower drying oven, and stored in a sealed container. Chemicals including TEMPO, NaBr, NaClO, and cellulase were purchased from China National Pharmaceutical Group Chemical Reagent Co.Ltd. (Shanghai, China). The preparation method of the eutectic solvent and [DMIM][DMP] is provided in the Supplementary Materials. Methods 1. Investigation of Conversion Efficiency for Preparing NCC from Wheat Straw via Eutectic Solvent Treatment 1.1 Single-factor Experiments 1.1.1 Effect of the Citric Acid-to-Ethylene Glycol Molar Ratio on NCC Conversion Efficiency One gram of straw powder was mixed with a eutectic solvent at a solid-to-liquid ratio of 1:30. The molar ratio of citric acid to ethylene glycol in the solvent was set to 1:1, 1:2, 1:3, and 1:4, respectively. The reaction was conducted at 90 °C with stirring for 4 hours. Upon completion, the resulting NCC was separated by centrifugation, thoroughly washed with water to remove residual solvent, dried, and weighed to determine the conversion efficiency. (The details are shown in Supplementary information 1) 1.1.2 Effect of Reaction Time on NCC Conversion Efficiency Reactions were performed at 90 °C with a citric acid-to-ethylene glycol molar ratio of 1:2 and a solid-to-liquid ratio of 1:30. The reaction times were set to 2, 4, 8, 12, and 24 hours to evaluate the influence of reaction duration on NCC conversion efficiency. 1.1.3 Effect of Reaction Temperature on NCC Conversion Efficiency The reaction conditions included a 4-hour reaction time, a citric acid-to-ethylene glycol molar ratio of 1:2, and a solid-to-liquid ratio of 1:30. Reaction temperatures were varied (80, 90, 100, 110, and 120 °C) to investigate their impact on NCC conversion efficiency. 1.1.4 Effect of Solid-to-Liquid Ratio on NCC Conversion Efficiency The reaction was conducted at 90°C for 4 hours with a citric acid-to-ethylene glycol molar ratio of 1:2. The solid-to-liquid ratios tested were 10:1, 20:1, 30:1, 40:1, and 50:1. The influence of the solid-to-liquid ratio on NCC conversion efficiency was evaluated. 1.2 Response Surface Optimization Based on single-factor experiment results (showing no significant differences in NCC conversion efficiency at citric acid-to-ethylene glycol molar ratios of 1:1, 1:3, and 1:4), reaction time, reaction temperature, and solid-to-liquid ratio were selected for optimization. Design Expert 13.0 software was used to perform a response surface analysis with a three-factor, three-level design. NCC conversion efficiency was set as the response variable. Factor levels are provided in the Table 1 below. 2. Comparative Work on the Conversion Efficiency of Wheat Straw and Cellulose to NCC by Eutectic Solvent, ionic liquids [DMIM][DMP], Cellulase, and TEMPO Oxidant Treatments 2.1 Preparation of NCC from Wheat Straw Powder via Eutectic Solvent Treatment A eutectic solvent was prepared by mixing citric acid and ethylene glycol at a molar ratio of 1:2 and heating the mixture to 100 °C. Under continuous stirring, 2 g of wheat straw powder was gradually added to 30 g of eutectic solvent, maintaining a solid-to-liquid ratio of 1:30. The mixture was kept at 100°C and stirred for 12 hours to ensure complete dissolution of the material. After the reaction, NCC was separated from the solution through centrifugation or filtration, washed multiple times with distilled water to remove residual solvent, dried, and stored for further analysis. The conversion efficiency was calculated accordingly. 2.2 Preparation of NCC from Wheat Straw Powder via ionic liquids [DMIM][DMP]Treatment The [DMIM][DMP] was heated to 80 °C (the details are shown in Supplementary information 2). Subsequently, 2 g of wheat straw powder was gradually introduced into 30 g of the ionic liquids [DMIM][DMP] under constant stirring. The mixture was heated and stirred until the cellulose was fully dissolved within 4 hours 17 . NCC was then separated by centrifugation, washed three times with distilled water to remove residual ionic liquid, dried, and stored. The conversion efficiency was determined based on the resulting product. 2.3 Preparation of NCC from Wheat Straw Powder via Cellulase Treatment Two grams of pretreated wheat straw powder was placed in a beaker and mixed with a cellulase solution at an activity level of 200 u/g, ensuring thorough contact between the enzyme and straw powder. The mixture was incubated at approximately 55°C for 240 minutes in a thermostatic shaker or water bath 18 . Upon completion, the enzyme was deactivated by heating the reaction mixture in a boiling water bath for 10 minutes. The precipitate was then collected through centrifugation, washed repeatedly with distilled water to remove residual enzymes and unreacted cellulose, redispersed in distilled water, and treated with ultrasound for 20 minutes to improve dispersion. The final sample was dried and stored. 2.4 Preparation of NCC from Wheat Straw Powder via TEMPO Oxidant Treatment Two grams of wheat straw powder was dispersed in distilled water under stirring to form a homogeneous suspension. TEMPO (0.016 g per gram of cellulose) and NaBr (0.1 g per gram of cellulose) were then added, followed by the dropwise addition of NaClO solution (10 mmol per gram of cellulose) under continuous stirring 19 . The pH of the reaction mixture was adjusted to 10–11 using NaOH and HCl and maintained at this level at room temperature for 1–2 hours. The reaction was terminated with ethanol or HCl, and the solution pH was adjusted to neutral. Solid cellulose was separated through vacuum filtration, washed multiple times with distilled water to remove excess reagents, and homogenized until the nanofibers were uniformly dispersed. The sample was dried and stored, and the conversion efficiency was calculated. 2.5 Comparative Work of NCC Conversion Efficiencies The conversion efficiencies of NCC from wheat straw powder and cellulose were compared across the four treatment methods. For each sample, the dry mass of the obtained NCC was denoted as m (g) and the dry mass of the raw material (cellulose or straw powder) was denoted as M (g). The conversion efficiency, D, was calculated as: 2.6 Characterization of NCC 2.6.1 Fourier Transform Infrared Spectroscopy (FTIR) FTIR spectroscopy was used to analyze the functional group changes in wheat straw powder and cellulose treated by eutectic solvents, ionic liquids, cellulase, and TEMPO oxidation. FTIR spectra were collected in the range of 4000–400 cm⁻¹ before and after treatment. Characteristic absorption peaks and functional group changes, such as those of hydroxyl, carboxyl, and ester groups, were examined to assess the chemical modifications imparted by different treatments. 2.6.2 X-ray Diffraction (XRD) XRD was performed to investigate the crystalline structure of NCC prepared via eutectic solvent, ionic liquid, cellulase, and TEMPO treatments. A Cu-Kα radiation source was used with an accelerating voltage of 40 kV and a current of 40 mA. The samples were scanned over a range of 5–60° at a rate of 10°/min. 2.6.3 Scanning Electron Microscopy (SEM) SEM analysis was conducted to observe the surface morphology of the prepared NCC. Samples were coated with platinum tAo prevent charging effects. SEM images were acquired under an accelerating voltage of 5 kV, allowing for the assessment of microstructural features and surface characteristics resulting from different treatment methods. 3. Economic and environmental feasibility work of NCC production In evaluating the feasibility of NCC (NCC) production processes, economic efficiency and environmental impact were identified as two critical factors. From an economic perspective, the target production yield was set at 1 ton of NCC, and key cost components, including chemical reagent procurement, electricity consumption, and raw material costs, were calculated. Additionally, equipment depreciation, labor costs, and solvent recovery rates were considered to provide a comprehensive assessment of the cost structure across different processes. By comparing the total production costs, the most economically competitive method was identified, providing essential insights for large-scale industrial applications. From an environmental perspective, the feasibility of each process was analyzed based on four key dimensions: energy consumption (ECS), carbon footprint (CF), solvent recovery rate (SR), and pollutant emissions (PE). A scoring system (5 as the best and 1 as the worst) was applied to quantify the environmental performance of different processes. In this system, a score of 5 represented the highest environmental compatibility, whereas a score of 1 indicated the poorest performance. For example, processes with low energy consumption, minimal carbon footprint, high solvent recovery efficiency, and minimal pollutant emissions received a score of 5, whereas those characterized by high energy consumption, significant carbon emissions, low solvent recovery, or costly pollutant treatment scored only 1 or 2. By integrating the economic efficiency and environmental impact evaluations, a comprehensive comparison of different production processes was conducted, providing valuable insights for process optimization, sustainability improvements, and industrial-scale implementation. Result and Analysis 1. Investigation of Conversion Efficiency for Preparing NCC from Wheat Straw via Eutectic Solvent Treatment 1.1 Response Surface Optimization 1.1.1 Effect of the Citric Acid-to-Ethylene Glycol Molar Ratio on NCC Conversion Efficiency The influence of the eutectic solvent (citric acid and ethylene glycol) molar ratio on NCC conversion efficiency is shown in Fig. 1. As the ethylene glycol content in the eutectic solvent system increased, NCC conversion efficiency initially rose and then declined. This trend was primarily attributed to the balance between the hydrogen-bonding network strength of the eutectic solvent, the dissolution capability for straw powder, and reaction selectivity 20 .When the molar ratio of citric acid to ethylene glycol was 1:2, the hydrogen-bonding network in the solvent system was optimal 21 ，This condition effectively disrupted the crystalline structure of the straw powder while maintaining a favorable reaction environment, resulting in the highest NCC conversion efficiency (60.2%).However, when the molar ratio increased to 1:3, the excessive ethylene glycol led to a more sparse hydrogen-bonding network and an overly strong dissolution capacity. This caused the straw powder to depolymerize excessively into soluble oligomers and disrupted the selectivity of the reaction, ultimately lowering NCC conversion efficiency and reducing the stability of the crystalline structure. 22 1.1.2 Effect of reaction time on NCC conversion The effect of reaction time on NCC conversion efficiency is presented in Fig. 2. During shorter reaction times (2–8 hours), the NCC conversion efficiency remained relatively stable, indicating that the reaction had not yet reached completion. When the reaction time was extended to 12 hours, the NCC conversion efficiency peaked at 67.6%, suggesting that the reaction was most complete at this point, with optimal depolymerization of straw powder and NCC formation. However, when the reaction time exceeded 12 hours, the conversion efficiency slightly decreased 23 . This decline might have been due to the over-depolymerization or further dissolution of straw powder into oligomers, which inhibited NCC production efficiency. 1.1.3 Effect of Reaction Temperature on NCC Conversion Efficiency The impact of reaction temperature on NCC conversion efficiency is shown in Fig. 3. The conversion efficiency exhibited a rise followed by a decline as the reaction temperature increased, indicating that temperature played a critical role in the solvent’s depolymerization capability and the conversion efficiency of straw powder. As the temperature increased from 80°C to 100°C, NCC conversion efficiency rose from 65 % to 71.6 %. This improvement was attributed to the enhanced molecular activity of the solvent at higher temperatures 24 , leading to stronger interactions with straw powder molecules and promoting depolymerization and conversion. However, as the temperature increased to 110 °C, the conversion efficiency dropped to 69.5%, likely due to nonselective degradation of straw powder or partial dissolution into oligomers at higher temperatures, reducing NCC yield and purity. When the temperature was further increased to 120 °C, the conversion efficiency slightly recovered to 70.2 %, but it did not exceed the peak value of 71.6 % observed at 100 °C. These results indicated that 100 °C was the optimal reaction temperature, achieving a balance between solvent activity and straw powder stability to maximize conversion efficiency. In contrast, temperatures that were too low or too high reduced reaction efficiency. 1.1.4 Effect of the Solid-to-Liquid Ratio of Straw Powder and Eutectic Solvent on NCC Conversion Efficiency The influence of the eutectic solvent-to-straw powder ratio on NCC conversion efficiency is illustrated in Fig. 4. As the ratio increased, the NCC conversion efficiency first rose and then fell. At a solid-to-liquid ratio of 1:30, the conversion efficiency reached its maximum value of 70.2 %, indicating that a higher ratio provided sufficient solvent molecules to fully interact with straw powder molecules. This enhanced the solvent’s ability to disrupt the crystalline structure of straw powder, promoting efficient NCC production. However, as the ratio increased to 1:40 and 1:50, the conversion efficiency decreased to 67 % and 59.7 %, respectively. This decline was likely due to excessive dilution of the reaction system, which weakened the interaction strength between the solvent and straw powder molecules. Additionally, higher ratios may have led to the over-dissolution of straw powder into oligomers 25 , inhibiting selective conversion to NCC and thereby reducing the overall conversion efficiency. 1.2 Response Surface Optimization Experimental Design Development and Analysis of Regression Models A three-factor, three-level Box-Behnken experimental design was employed to optimize the NCC conversion efficiency (Y), considering reaction time (A), reaction temperature (B), and the solid-to-liquid ratio of eutectic solvent to straw powder (C). The design included 29 experimental runs, as shown in Table 2. The data from Table 2 were analyzed using Design Expert 13.0 software to fit a regression model that describes the relationship between NCC conversion efficiency and the selected factors. The resulting regression model is presented below: Y=71.96+0.0304 A-0.0508 B-0.0347 C+1.08AB-0.1203 AC+1.17 BC-1.77 A²-3.69 B²-5.95C ² The regression analysis (Table 3) indicated that the response surface model was highly significant (P 0.05). These results suggest that the model is appropriate for analyzing and predicting the effects of different treatment conditions on NCC conversion efficiency. Among the tested factors, reaction temperature (B) had the most significant impact, followed by the solid-to-liquid ratio (C) and reaction time (A). Optimization and Validation of Process Conditions Response surface plots illustrating the interactions between the factors (reaction time, reaction temperature, and solid-to-liquid ratio) are shown in Fig. 5. The response surface analysis revealed that reaction time, reaction temperature, and the solid-to-liquid ratio directly or indirectly influenced NCC conversion efficiency. As seen in Fig. 5a, both reaction time and temperature exhibited an initial increase in NCC conversion efficiency, followed by a decrease. During the early stages of the reaction, longer times and higher temperatures effectively accelerated the reaction rate, leading to greater product yield. However, when reaction times exceeded 12 hours or temperatures surpassed 100°C, NCC conversion efficiency began to decline. This reduction may have been caused by the degradation of the target product over extended reaction durations and the occurrence of side reactions at elevated temperatures, such as the decomposition of sugars in the straw powder, resulting in the formation of byproducts and reduced overall conversion efficiency 26 . Fig. 5b illustrates the combined effects of reaction time and solid-to-liquid ratio on NCC conversion efficiency. The efficiency increased as reaction time and solid-to-liquid ratio rose, peaking at a ratio of approximately 30–35 and a reaction time of 12–13 hours. At short reaction times (<12 hours) or lower ratios (12 hours) or high ratios (>35) suppressed further improvements in conversion efficiency. Prolonged reaction times increased the likelihood of side reactions, while excessive solvent diluted the reactant concentration, thus hindering the reaction 27 . The optimal conditions were identified as a reaction time of 12–13 hours and a solid-to-liquid ratio of 30~35, yielding a peak NCC conversion efficiency of 71~72 %. As shown in Fig. 5c, the impact of solid-to-liquid ratio and reaction temperature on NCC conversion efficiency was also highly significant. At low ratios (<20), insufficient contact between the reactants and solvent limited the reaction. When the ratio reached 30, the reaction system achieved an ideal balance of solvent and solid, allowing for full diffusion and efficient reaction, which resulted in the highest conversion efficiency. At higher ratios (>35), however, excessive solvent diluted the reactant concentration, reducing reaction efficiency and lowering the conversion rate 28 . Similarly, reaction temperature followed a similar trend. At lower temperatures (<90°C), the reaction rate was too slow, and activation energy was insufficient, restricting NCC formation. The efficiency increased with temperature, peaking at around 102 °C. Beyond this, higher temperatures (>114°C) led to degradation of the target product or intensified side reactions 29 , Similarly, reaction temperature followed a similar trend. At lower temperatures (<90 °C), the reaction rate was too slow and activation energy was insufficient, restricting NCC formation. The efficiency increased with temperature, peaking at around 102°C. Beyond this, higher temperatures (>114 °C) led to degradation of the target product or intensified side reactions. 2.Comparative Work of Conversion Efficiency of Wheat Straw and Cellulose to NCC Using DES, Ionic Liquid, Cellulase, and TEMPO Treatments 2.1Conversion Efficiency of Different Treatments The conversion efficiency of different agents in producing NCC from wheat straw powder is shown in Fig. 6. The results reveal significant differences, which are closely related to the reaction mechanisms of each agent and the raw material properties. DES demonstrated the highest conversion efficiency at 72.3 %, attributed to its ability to dissolve cellulose and partially remove non-cellulosic components, thereby significantly increasing cellulose exposure 30 ，In comparison, the [DMIM][DMP] improved reaction activity by disrupting the hydrogen bonding network of cellulose 31 , achieving a conversion efficiency of 67.0 %. Cellulase directly degraded cellulose into NCC by hydrolyzing β-1,4-glycosidic bonds1 32 ，but due to the complex matrix of wheat straw powder, its conversion efficiency was limited to 54.0 %. TEMPO oxidant selectively oxidized the C6 hydroxyl groups to carboxyl groups 33 ，but its conversion efficiency was also hindered by lignin and hemicellulose, resulting in a conversion efficiency of 56.7 %. Overall, DES emerged as the most promising treatment method for producing NCC from wheat straw powder due to its higher conversion efficiency and broader applicability. 2.2 FTIR Analysis of NCC Produced by Different Treatments The FTIR spectra (Fig. 7) of NCC prepared from wheat straw powder and MCC revealed significant differences and trends in chemical structure and derivatization. Untreated wheat straw (Fig. 7a) showed broad –OH absorption bands (~3400 cm ⁻¹ ), strong C=O absorption peaks (~1730 cm ⁻¹ ), and aromatic C=C peaks (~1600 cm ⁻¹ ), indicative of abundant lignin and hemicellulose. MCC (Fig. 7b), being more purified, exhibited a narrower –OH band, weaker C=O peaks, and stronger C–O–C absorption bands near 1100 cm ⁻¹ . DES-treated wheat straw powder (Fig. 7c) displayed nearly complete disappearance of lignin and hemicellulose peaks, along with a pronounced enhancement of C–O–C absorption bands. This change indicates that DES effectively removed non-cellulosic components from wheat straw, significantly increasing cellulose purity and crystallinity 34 .treatment (Fig. 7d) also resulted in enhanced C–O–C absorption, but since cellulase mainly hydrolyzes β-1,4-glycosidic bonds, it caused minimal changes to the chemical structure, and the C=O absorption bands remained relatively unchanged. This method maintained the fundamental cellulose framework while improving crystallinity 18 . TEMPO oxidation (Fig. 7e) demonstrated pronounced derivatization effects. The carboxyl absorption peak (~1730 cm ⁻¹ ) was significantly enhanced, while the –OH absorption band (~3400 cm ⁻¹ ) was relatively reduced, indicating that TEMPO selectively oxidized C6 hydroxyl groups into carboxyl groups and increased functionalization levels 35 . [DMIM][DMP] treatment (Fig. 7f) mainly disrupted intra- and intermolecular hydrogen bonding within cellulose, promoting physical reorganization and crystallization. The FTIR spectra showed a weakening of –OH absorption and an enhancement of C–O–C bands, while the C=O peaks remained stable, suggesting no significant chemical derivatization 36 . In summary, producing NCC from wheat straw powder requires efficient impurity removal to eliminate lignin and hemicellulose. DES effectively enhances crystallinity and purity, cellulase treatment is mild and retains the native properties of cellulose while improving crystallinity, TEMPO oxidation greatly increases carboxylation levels, and [DMIM][DMP] excels in physical reorganization and crystallization. DES stands out for its excellent impurity removal capability and improvement of cellulose crystallinity, making it a promising method for producing NCC from wheat straw powder. 2.3 XRD Analysis of NCC Crystallinity XRD patterns (Fig. 8A) reveal clear differences in the crystallinity improvement and structural changes of NCC prepared from wheat straw powder after different treatments. Untreated wheat straw powder (Fig. 8a) displayed broad and weak diffraction peaks (2θ = 15.1° and 22°), indicating low crystallinity due to the presence of amorphous lignin and hemicellulose 37 . MCC (Fig. 8b), which inherently has higher crystallinity, showed sharp diffraction peaks at 2θ = 22.5°, reflecting minimal amorphous content. Among the treatments, DES (Fig. 8f) showed the most significant improvement in crystallinity. The diffraction peak at 2θ = 22.5° was sharp and intense, suggesting that DES efficiently removed amorphous components (e.g., lignin, hemicellulose) through strong hydrogen bonding and acid-base interactions, thereby greatly enhancing crystallinity 38 [DMIM][DMP] treatment (Fig. 8d) also demonstrated a notable increase in crystallinity by breaking cellulose hydrogen bonds and promoting molecular rearrangement, as evidenced by stronger diffraction peaks and reduced amorphous content 39 . TEMPO oxidation (Fig. 8c), focusing on chemical derivatization, selectively oxidized cellulose’s C6 hydroxyl groups into carboxyl groups, conferring new functional groups 40 .However, its effect on enhancing crystallinity was relatively limited. Cellulase treatment (Fig. 8e) increased crystallinity to a lesser extent, as it hydrolyzed β-1,4-glycosidic bonds 41 , partially removing amorphous regions. However, its milder action left some amorphous components intact, resulting in lower crystallinity improvement compared to DES and [DMIM][DMP]. In conclusion, due to its low initial crystallinity and high amorphous content, wheat straw powder has significant potential for modification. DES and [DMIM][DMP] were the most effective treatments for achieving high-quality crystalline cellulose. TEMPO oxidation is better suited for applications requiring high functionalization, while cellulase treatment is ideal for preserving the inherent characteristics of cellulose. Considering the desired performance and processing requirements, DES treatment offers the greatest improvement in crystallinity and optimal crystalline structure when producing NCC from wheat straw powder. 2.4 SEM Analysis of NCC Morphology and Crystallinity High impurity content in wheat straw powder significantly affected the ability of different agents to modify morphology and enhance crystallinity (Fig. 9 Table 4) (the details are shown in Supplementary information 3、4). TEMPO oxidation selectively introduced carboxyl groups by oxidizing C6 hydroxyl groups in cellulose, adding functionalized modifications. However, it showed limited effectiveness in optimizing morphology and controlling size. The NCC produced from wheat straw powder (Fig. 9a) had particle sizes of 93.4–54.4 nm, with larger and unevenly distributed particles, indicating that the high impurity content interfered with TEMPO’s ability to modify cellulose fiber morphology. [DMIM][DMP] treatment disrupted hydrogen bonds within cellulose and promoted molecular rearrangement, improving crystallinity and some degree of morphological regularity 42 . The NCC produced from wheat straw powder (Fig. 9c) exhibited particle sizes of 92.1–44.7 nm, with improved crystallinity, though the morphology remained irregular, and agglomeration was evident. This suggests that ionic liquids have limited tolerance to high impurity levels. Cellulase treatment, being a mild modification method, preserved the original characteristics of cellulose and increased crystallinity but showed weaker effects on morphology and size optimization. The NCC produced from wheat straw powder (Fig. 9e) had particle sizes of 82.8–47.5 nm, with significant agglomeration. The enzymatic hydrolysis was insufficient to completely remove lignin and hemicellulose, making it difficult to obtain regular NCC morphology. DES treatment dissolved lignin, hemicellulose, and other non-cellulosic components, breaking cellulose hydrogen bonds and significantly enhancing crystallinity and morphology 43 The NCC produced from wheat straw powder (Fig. 9g) had particle sizes of 98.8–52.2 nm. While still irregular in shape, it showed notable improvement compared to the raw material. This highlights DES’s excellent ability to remove non-cellulosic components and enhance cellulose crystallinity and morphology 44 . Overall, for wheat straw powder with high impurity content, DES and [DMIM][DMP] both performed well in removing non-cellulosic components and improving crystallinity, with DES demonstrating greater advantages. DES not only achieved higher crystallinity but also partially improved cellulose morphology. [DMIM][DMP], while also promoting crystallization, showed slightly lower tolerance to high impurity levels. TEMPO oxidation effectively increased functionalization levels but had limited control over morphology and size. Cellulase treatment was suitable for mild modifications that preserved the native cellulose properties, though its morphological optimization was less effective than DES and [DMIM][DMP] treatments. Ultimately, the choice of treatment agent should consider multiple performance criteria, including functionalization, crystallinity, and morphology. DES’s excellent impurity removal and crystallinity enhancement capabilities make it a superior choice for processing high-impurity wheat straw powder. 3. Recyclable Process Design and Environmental Evaluation of NCC Production In this work, the production processes of NCC were evaluated by comparing two primary indicators: economic efficiency and environmental feasibility (the details are shown in Supplementary information 5). Initially, four methods—DES, [DMIM][DMP], Cellulase, and TEMPO—were examined regarding their respective requirements for straw, chemical reagents, and electricity in the production of one ton of NCC (Table 5). The results indicated that DES demonstrates a pronounced economic advantage, whereas [DMIM][DMP]—due to the high cost of ionic liquids—fails to achieve significant economic returns in large-scale production. By comparison, the Cellulase approach entails relatively lower chemical reagent expenses, while the TEMPO oxidation route incurs considerable costs owing to the use of expensive oxidizing agents. Beyond economic considerations, this work also assessed the four methods from the perspectives of Energy Consumption (ECS), Carbon Footprint (CF), Solvent Recovery (SR), and Wastewater Treatment (WWT) (Fig.10). The findings show that both Cellulase and DES perform well in terms of energy consumption and wastewater management, thereby exhibiting favorable environmental compatibility. In contrast, [DMIM][DMP] exhibits notable environmental challenges arising from the complexity of synthesizing, recovering, and disposing of ionic liquids, while TEMPO oxidation faces similar issues due to its reliance on oxidizing agents and the associated by-product handling, thus necessitating thorough evaluation of its environmental impact in practical applications. Taking both economic and environmental factors into account, DES stands out as the most viable option, offering low production costs and strong environmental performance, thereby making it particularly suitable for industrial-scale manufacturing and sustainable development. Nevertheless, the Cellulase, TEMPO, and [DMIM][DMP] processes retain their unique value for producing high-quality or functionalized cellulose products, although their potentially high costs and environmental implications call for more prudent consideration when selecting an appropriate process route. Conclusion This study systematically addresses the technical, economic, and environmental challenges in producing CNC from straw by comparing four methods: CA–EG DES, the [DMIM][DMP], cellulase hydrolysis, and TEMPO oxidation. Each method’s conversion efficiency, structural characterization, and economic and environmental feasibility were evaluated. Results indicate that the CA–EG DES process exhibits pronounced advantages in terms of yield, cost-effectiveness, and environmental compatibility, highlighting its potential for large-scale industrial deployment in line with sustainable development goals. Under optimized temperature, reaction duration, and solid–liquid ratio conditions, CA–EG DES effectively removes non-cellulosic components, thereby increasing the yield and crystallinity of CNC while reducing energy consumption and environmental burden. These findings align with the recent trend of “green solvents” in the production of cellulose-based nanomaterials. By contrast, although ionic liquids significantly enhance cellulose crystallinity, their high cost and difficult solvent recovery hinder extensive industrial application. Meanwhile, cellulase treatment preserves cellulose integrity under mild conditions but exhibits lower efficiency in multi-component straw systems and requires high substrate purity and enzyme activity. TEMPO oxidation enables selective oxidation and functionalization yet encounters notable challenges in cost and wastewater treatment. From a comprehensive process, economic, and environmental perspective, the CA–EG DES method clearly stands out due to its lower raw material and energy requirements, readily recyclable solvent, mild reaction parameters, and reduced wastewater treatment needs. Future work can focus on tailoring CA–EG DES formulations for various types of lignocellulosic feedstocks, while further technological improvements—such as lowering solvent viscosity and energy demands, enhancing recovery rates, and accommodating diverse biomass sources—could foster a more efficient, greener CNC production framework. This strategy ultimately supports the high-value-added utilization of agricultural straw and other renewable biomasses, laying a foundation for the development of novel bio-based materials. Declarations Funding We wish to express our thanks for the support from the Postgraduate Research & Practice Innovation Program of Jiangsu Province (KYCX25_4409), the Zhenjiang Carbon Peaking & Neutrality Project (No. CN2022001) and Jiangsu Overseas Research & Training Program for University Prominent Young & Middle-aged Teachers and Presidents. Author Contributions Niuniu Deng Conceptualization; Data curation; Formal analysis; Writing – original draft. 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Crops Prod. 223 , 120173 (2025). https://doi.org:10.1016/j.indcrop.2024.120173 Tables Table 1: response surface experimental factor levels Factor Coding level -1 0 1 A Time（h） 2 12 24 B Temperature（°C） 90 100 120 C Solid-liquid ratio（g/ml） 1:20 1:30 1:40 Table 2 box Behnken test design and results Test No Factor NC conversion% a b c 1 0 1 -1 65 2 1 -1 0 62.7 3 -1 0 1 68.2 4 1 1 0 71.6 5 0 -1 1 64.2 6 0 0 0 66.8 7 -1 1 0 72 8 -1 -1 0 70.2 9 0 0 0 64.8 10 0 0 0 62.8 11 1 0 1 62.2 12 0 0 0 66 13 1 0 -1 60.2 14 0 -1 -1 72.3 15 -1 0 -1 71.8 16 0 0 0 64 17 0 1 1 63.7 Note: "*" has significant difference (p<0.05), The difference of "* *" was extremely significant (p<0.01) Table 3 Variance Analysis of regression model Source Sum of Squares df Mean Square F-value p-value Model 238.98 9 26.55 28.48 0.0001 ** A 0.007 1 0.007 0.0075 0.9333 B 0.0206 1 0.0206 0.0221 0.8861 C 0.0091 1 0.0091 0.0098 0.924 AB 4.97 1 4.97 5.33 0.0544 AC 0.0582 1 0.0582 0.0624 0.81 BC 5.82 1 5.82 6.25 0.041 * A² 12.86 1 12.86 13.79 0.0075 ** B² 42.84 1 42.84 45.95 0.0003 ** C² 148.96 1 148.96 159.76 < 0.0001 ** Residual 6.53 7 0.9324 Lack of Fit 3.88 3 1.29 1.95 0.2631 not significant Pure Error 2.65 4 0.662 Cor Total 245.5 16 Table 4: size comparison under SEM of NCC prepared by straw powder treated with different reagents TEMPO [DMIM][DMP] cellulase DES Size of NCC (Length- width)/nm 93.4-54.4 92.1-44.7 82.8-47.5 98.8-52.2 Table 5: Comparison of Material Requirements and Cost Estimates for Producing 1 Ton of NCC Across Four Treatment Methods Straw dosage(t) Straw（CNY） Chemical (CNY) Electricity (CNY) All-in cost（CNY） All-in cost（USD） DES 1.38 61.16 7356.7 1067.6 ¥8485.46/t $1164.96 [DMIM][DMP] 1.5 66 157300 1577 ¥158943/t $21823.6 Cellulase 1.9 83.6 31588.6 1171.8 ¥32760.4/t $4498.16 TEMPO 1.8 79.2 72630 1328 ¥74037.2/t $10165.67 Additional Declarations No competing interests reported. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-7700269","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":572874309,"identity":"be57ffe2-c346-4b1e-84bf-51f4a58c3a42","order_by":0,"name":"Niuniu Deng","email":"","orcid":"","institution":"Jiangsu University of Science and Technology","correspondingAuthor":false,"prefix":"","firstName":"Niuniu","middleName":"","lastName":"Deng","suffix":""},{"id":572874310,"identity":"e9f83e84-60dc-46d0-8da1-826738031f3f","order_by":1,"name":"Qiang 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reagents\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003ea:\u003c/strong\u003eStraw, \u003cstrong\u003eb: \u003c/strong\u003eCellulose, \u003cstrong\u003ec: \u003c/strong\u003eNCC prepared by TEMPO treatment, \u003cstrong\u003ed: \u003c/strong\u003eNCC prepared by [DMIM] [DMP] treatment, \u003cstrong\u003ee: \u003c/strong\u003eNCC produced by cellulase treatment, \u003cstrong\u003ef:\u003c/strong\u003e NCC produced by DES treatment\u003c/p\u003e","description":"","filename":"8.png","url":"https://assets-eu.researchsquare.com/files/rs-7700269/v1/3d3d98f74da6ee675254bd1d.png"},{"id":101752800,"identity":"1948dc92-a872-4b3a-b252-564b9c1eb8d2","added_by":"auto","created_at":"2026-02-03 10:32:39","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":636182,"visible":true,"origin":"","legend":"\u003cp\u003eSEM of NCC prepared by straw powder treated with different reagents\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003ea: \u003c/strong\u003eprepared by TEMPO treatment NCC, b\u003cstrong\u003e: \u003c/strong\u003eprepared by [DMIM][DMP] treatment NCC, c\u003cstrong\u003e: \u003c/strong\u003eprepared by cellulase treatment of straw powder, \u003cstrong\u003ed: \u003c/strong\u003eprepared by DES treatment of straw powder\u003c/p\u003e","description":"","filename":"9.png","url":"https://assets-eu.researchsquare.com/files/rs-7700269/v1/ae382449ff9286fbe318d10e.png"},{"id":101751667,"identity":"557a73c2-0082-4c43-8ed9-c2bcf62681e6","added_by":"auto","created_at":"2026-02-03 10:22:07","extension":"png","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":67916,"visible":true,"origin":"","legend":"\u003cp\u003eEnvironmental Feasibility Analysis of Four Treatment Methods—Scoring Based on Energy Consumption, Carbon Footprint, Solvent Recovery Rate, and Wastewater Treatment\u003c/p\u003e","description":"","filename":"10.png","url":"https://assets-eu.researchsquare.com/files/rs-7700269/v1/d3da63b0865de61d8aa0ca94.png"},{"id":104402164,"identity":"5219bd98-3a5b-4c70-8e14-186b12ca2b01","added_by":"auto","created_at":"2026-03-11 12:14:32","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":3126062,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7700269/v1/909dee6f-d5ce-4be9-a04f-e37834b7e9db.pdf"},{"id":101752047,"identity":"ad93cc6f-c65e-425e-a9ab-e4983c18ac95","added_by":"auto","created_at":"2026-02-03 10:25:05","extension":"docx","order_by":0,"title":"","display":"","copyAsset":false,"role":"supplement","size":517724,"visible":true,"origin":"","legend":"","description":"","filename":"SupplementaryMaterial.docx","url":"https://assets-eu.researchsquare.com/files/rs-7700269/v1/bf50e3f12280c92726ab143b.docx"}],"financialInterests":"No competing interests reported.","formattedTitle":"Green and Scalable Production of Nanocrystalline Cellulose Driven by a Biomass-Derived Deep Eutectic Solvent","fulltext":[{"header":"Introduction","content":"\u003cp\u003eAgricultural straw, as the most abundant lignocellulosic residue generated during crop cultivation, is frequently subjected to open burning or landfill disposal, thereby exacerbating air pollution and greenhouse gas emissions \u003csup\u003e1\u003c/sup\u003e.\u0026nbsp;Nonetheless, due to its inherent richness in cellulose, hemicellulose, and lignin, straw represents a highly promising renewable feedstock for the synthesis of advanced biomaterials. Nanocellulose (NCC) has garnered extensive interest for its remarkable crystallinity, nanoscale dimensions, and superior mechanical strength. Moreover, NCC exhibits excellent thermal stability, low density, and intrinsic biocompatibility, rendering it an ideal candidate for applications spanning high-performance composites, biomedical devices, food additives, and environmental remediation \u003csup\u003e2\u003c/sup\u003e. Given the urgent need to reduce reliance on fossil-based materials and mitigate environmental burdens, the development of sustainable, efficient, and economically viable routes for producing NCC from biomass residues such as straw has become increasingly important\u0026nbsp;\u003csup\u003e3\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eTraditionally, strong acid hydrolysis—particularly sulfuric acid—has been the most common approach for preparing NCC. Although this technique reliably produces high-crystallinity NCC, it has notable drawbacks for industrial implementation\u0026nbsp;\u003csup\u003e4\u003c/sup\u003e. Corrosive acids inflict equipment and pipeline damage, resulting in high maintenance costs. Managing waste acids also remains challenging, as neutralization, separation, and purification are required to meet environmental discharge standards. These factors drive up operational expenses and undermine process sustainability. Consequently, researchers have investigated alternative methods—including ionic liquids, cellulases, and TEMPO (2,2,6,6-tetramethylpiperidine-1-oxyl) oxidation—that reduce corrosivity\u0026nbsp;\u003csup\u003e5\u003c/sup\u003e, enable selective dissociation, and allow for functional modification. Nevertheless, their high solvent or enzyme costs, complex regeneration processes, and viscosity challenges hinder large-scale production\u0026nbsp;\u003csup\u003e6\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eDeep eutectic solvents (DES) are emerging as an attractive solution, offering low toxicity, easy preparation, and recyclability\u0026nbsp;\u003csup\u003e7\u003c/sup\u003e. Unlike conventional ionic liquids, DES can be synthesized from inexpensive\u0026nbsp;\u003csup\u003e8\u003c/sup\u003e, readily available materials. In comparison to traditional strong acid systems, DES typically exhibit lower corrosivity, simpler post-treatment, and reduced environmental burden. These solvents can induce cellulose swelling and, under certain conditions, dissolve cellulose by disrupting hydrogen bonds between cellulose molecules, allowing lignin and hemicellulose removal, ultimately leading to NCC production\u0026nbsp;\u003csup\u003e9\u003c/sup\u003e. Moreover, many DES components are derived from renewable biomass or food-grade substances, further augmenting their environmental appeal\u0026nbsp;\u003csup\u003e10\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eRecent studies illustrate the efficacy of DES in pretreating lignocellulosic materials under mild conditions, effectively breaking hydrogen bonds among cellulose, hemicellulose, and lignin. By fine-tuning DES composition and reaction parameters, cellulose can be dissolved to facilitate subsequent chemical modifications and derivatization\u0026nbsp;\u003csup\u003e11\u003c/sup\u003e. This results in cellulose-based materials with improved properties. Additionally, cellulose treated with DES can be converted into NCC, which demonstrates excellent dispersion and homogeneity, opening opportunities for use in composites, packaging, and medical applications\u0026nbsp;\u003csup\u003e12\u003c/sup\u003e. Ongoing research employing structural characterization, thermal analysis, and molecular simulations continues to unveil how DES interact with cellulose, providing valuable guidance for process optimization\u0026nbsp;\u003csup\u003e13\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eDespite this progress, certain challenges persist. High-viscosity DES formulations can hinder mass transfer, necessitating higher temperatures or extended reaction times\u0026nbsp;\u003csup\u003e14\u003c/sup\u003e, which may elevate energy requirements and risk excessive cellulose degradation\u0026nbsp;\u003csup\u003e15\u003c/sup\u003e. Furthermore, impurities such as lignin and hemicellulose can accumulate during solvent recycling, altering DES composition and diminishing its performance\u0026nbsp;\u003csup\u003e16\u003c/sup\u003e. Additionally, variations in feedstock composition create difficulties in developing a universal DES formulation suitable for all straw, wood, and pure cellulose sources. Consequently, further work is required to optimize DES systems for large-scale use, centering on process scalability, cost reduction, and environmental performance.\u003c/p\u003e\n\u003cp\u003eThis work focuses on evaluating the feasibility of using straw to produce NCC by comparing four methods: DES, ionic liquids, cellulases, and TEMPO oxidation. The primary objective is to evaluate the possibility of each strategy for large-scale production based on factors including energy consumption, environmental impact, and recyclability. A key aspect is refining both the composition and reaction conditions of a co-DES system—comprising citric acid and ethylene glycol—for processing straw powder. Notably, citric acid and ethylene glycol enable a more economically sustainable approach. The resultant NCC is assessed on yield, morphology, and crystallinity, while an economic analysis addresses solvent and reagent recycling, capital equipment outlays, and waste treatment methods. This holistic evaluation underscores the industrial viability and sustainability potential of each technique.\u003c/p\u003e"},{"header":"Materials and Methods","content":"\u003cp\u003e\u003cstrong\u003eMaterials\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eWheat straw was collected from Muxiang County, Suqian City, Jiangsu Province. The straw was processed with a high-speed multifunctional grinder and passed through a 100\u0026ndash;200 mesh sieve. The sieved powder was washed 2\u0026ndash;3 times with warm water at 50\u0026deg;C, allowed to settle, filtered, dried in an electric thermostatic blower drying oven, and stored in a sealed container. Chemicals including TEMPO, NaBr, NaClO, and cellulase were purchased from China National Pharmaceutical Group Chemical Reagent Co.Ltd. (Shanghai, China). The preparation method of the eutectic solvent and [DMIM][DMP] is provided in the Supplementary Materials.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eMethods\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1. Investigation of Conversion Efficiency for Preparing NCC from Wheat Straw via Eutectic Solvent Treatment\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.1 Single-factor Experiments\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.1.1 Effect of the Citric Acid-to-Ethylene Glycol Molar Ratio on NCC Conversion Efficiency\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eOne gram of straw powder was mixed with a eutectic solvent at a solid-to-liquid ratio of 1:30. The molar ratio of citric acid to ethylene glycol in the solvent was set to 1:1, 1:2, 1:3, and 1:4, respectively. The reaction was conducted at 90 \u0026deg;C with stirring for 4 hours. Upon completion, the resulting NCC was separated by centrifugation, thoroughly washed with water to remove residual solvent, dried, and weighed to determine the conversion efficiency. (The details are shown in Supplementary information 1)\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.1.2 Effect of Reaction Time on NCC Conversion Efficiency\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eReactions were performed at 90 \u0026deg;C with a citric acid-to-ethylene glycol molar ratio of 1:2 and a solid-to-liquid ratio of 1:30. The reaction times were set to 2, 4, 8, 12, and 24 hours to evaluate the influence of reaction duration on NCC conversion efficiency.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.1.3 Effect of Reaction Temperature on NCC Conversion Efficiency\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe reaction conditions included a 4-hour reaction time, a citric acid-to-ethylene glycol molar ratio of 1:2, and a solid-to-liquid ratio of 1:30. Reaction temperatures were varied (80, 90, 100, 110, and 120 \u0026deg;C) to investigate their impact on NCC conversion efficiency.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.1.4 Effect of Solid-to-Liquid Ratio on NCC Conversion Efficiency\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe reaction was conducted at 90\u0026deg;C for 4 hours with a citric acid-to-ethylene glycol molar ratio of 1:2. The solid-to-liquid ratios tested were 10:1, 20:1, 30:1, 40:1, and 50:1. The influence of the solid-to-liquid ratio on NCC conversion efficiency was evaluated.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.2 Response Surface Optimization\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eBased on single-factor experiment results (showing no significant differences in NCC conversion efficiency at citric acid-to-ethylene glycol molar ratios of 1:1, 1:3, and 1:4), reaction time, reaction temperature, and solid-to-liquid ratio were selected for optimization. Design Expert 13.0 software was used to perform a response surface analysis with a three-factor, three-level design. NCC conversion efficiency was set as the response variable. Factor levels are provided in the Table 1 below.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2. Comparative Work on the Conversion Efficiency of Wheat Straw and Cellulose to NCC by Eutectic Solvent, ionic liquids [DMIM][DMP], Cellulase, and TEMPO Oxidant Treatments\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.1 Preparation of NCC from Wheat Straw Powder via Eutectic Solvent Treatment\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eA eutectic solvent was prepared by mixing citric acid and ethylene glycol at a molar ratio of 1:2 and heating the mixture to 100 \u0026deg;C. Under continuous stirring, 2 g of wheat straw powder was gradually added to 30 g of eutectic solvent, maintaining a solid-to-liquid ratio of 1:30. The mixture was kept at 100\u0026deg;C and stirred for 12 hours to ensure complete dissolution of the material. After the reaction, NCC was separated from the solution through centrifugation or filtration, washed multiple times with distilled water to remove residual solvent, dried, and stored for further analysis. The conversion efficiency was calculated accordingly.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.2 Preparation of NCC from Wheat Straw Powder via ionic liquids [DMIM][DMP]Treatment\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe [DMIM][DMP] was heated to 80 \u0026deg;C (the details are shown in Supplementary information 2). Subsequently, 2 g of wheat straw powder was gradually introduced into 30 g of the ionic liquids [DMIM][DMP]\u0026nbsp;under constant stirring. The mixture was heated and stirred until the cellulose was fully dissolved within 4 hours \u003csup\u003e17\u003c/sup\u003e. NCC was then separated by centrifugation, washed three times with distilled water to remove residual ionic liquid, dried, and stored. The conversion efficiency was determined based on the resulting product.\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.3 Preparation of NCC from Wheat Straw Powder via Cellulase Treatment\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eTwo grams of pretreated wheat straw powder was placed in a beaker and mixed with a cellulase solution at an activity level of 200 u/g, ensuring thorough contact between the enzyme and straw powder. The mixture was incubated at approximately 55\u0026deg;C for 240 minutes in a thermostatic shaker or water bath\u003csup\u003e18\u003c/sup\u003e. Upon completion, the enzyme was deactivated by heating the reaction mixture in a boiling water bath for 10 minutes. The precipitate was then collected through centrifugation, washed repeatedly with distilled water to remove residual enzymes and unreacted cellulose, redispersed in distilled water, and treated with ultrasound for 20 minutes to improve dispersion. The final sample was dried and stored.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.4 Preparation of NCC from Wheat Straw Powder via TEMPO Oxidant Treatment\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eTwo grams of wheat straw powder was dispersed in distilled water under stirring to form a homogeneous suspension. TEMPO (0.016 g per gram of cellulose) and NaBr (0.1 g per gram of cellulose) were then added, followed by the dropwise addition of NaClO solution (10 mmol per gram of cellulose) under continuous stirring \u003csup\u003e19\u003c/sup\u003e. The pH of the reaction mixture was adjusted to 10\u0026ndash;11 using NaOH and HCl and maintained at this level at room temperature for 1\u0026ndash;2 hours. The reaction was terminated with ethanol or HCl, and the solution pH was adjusted to neutral. Solid cellulose was separated through vacuum filtration, washed multiple times with distilled water to remove excess reagents, and homogenized until the nanofibers were uniformly dispersed. The sample was dried and stored, and the conversion efficiency was calculated.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.5 Comparative Work of NCC Conversion Efficiencies\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe conversion efficiencies of NCC from wheat straw powder and cellulose were compared across the four treatment methods. For each sample, the dry mass of the obtained NCC was denoted as m (g) and the dry mass of the raw material (cellulose or straw powder) was denoted as M (g). The conversion efficiency, D, was calculated as:\u003c/p\u003e\n\u003cp\u003e\u003cimg src=\"data:image/png;base64,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\"\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.6 Characterization of NCC\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.6.1 Fourier Transform Infrared Spectroscopy (FTIR)\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eFTIR spectroscopy was used to analyze the functional group changes in wheat straw powder and cellulose treated by eutectic solvents, ionic liquids, cellulase, and TEMPO oxidation. FTIR spectra were collected in the range of 4000\u0026ndash;400 cm⁻\u0026sup1; before and after treatment. Characteristic absorption peaks and functional group changes, such as those of hydroxyl, carboxyl, and ester groups, were examined to assess the chemical modifications imparted by different treatments.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.6.2 X-ray Diffraction (XRD)\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eXRD was performed to investigate the crystalline structure of NCC prepared via eutectic solvent, ionic liquid, cellulase, and TEMPO treatments. A Cu-K\u0026alpha; radiation source was used with an accelerating voltage of 40 kV and a current of 40 mA. The samples were scanned over a range of 5\u0026ndash;60\u0026deg; at a rate of 10\u0026deg;/min.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.6.3 Scanning Electron Microscopy (SEM)\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eSEM analysis was conducted to observe the surface morphology of the prepared NCC. Samples were coated with platinum tAo prevent charging effects. SEM images were acquired under an accelerating voltage of 5 kV, allowing for the assessment of microstructural features and surface characteristics resulting from different treatment methods.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e3.\u003c/strong\u003e\u003cstrong\u003e\u0026nbsp;Economic and environmental feasibility work of NCC production\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eIn evaluating the feasibility of NCC (NCC) production processes, economic efficiency and environmental impact were identified as two critical factors. From an economic perspective, the target production yield was set at 1 ton of NCC, and key cost components, including chemical reagent procurement, electricity consumption, and raw material costs, were calculated. Additionally, equipment depreciation, labor costs, and solvent recovery rates were considered to provide a comprehensive assessment of the cost structure across different processes. By comparing the total production costs, the most economically competitive method was identified, providing essential insights for large-scale industrial applications.\u003c/p\u003e\n\u003cp\u003eFrom an environmental perspective, the feasibility of each process was analyzed based on four key dimensions: energy consumption (ECS), carbon footprint (CF), solvent recovery rate (SR), and pollutant emissions (PE). A scoring system (5 as the best and 1 as the worst) was applied to quantify the environmental performance of different processes. In this system, a score of 5 represented the highest environmental compatibility, whereas a score of 1 indicated the poorest performance. For example, processes with low energy consumption, minimal carbon footprint, high solvent recovery efficiency, and minimal pollutant emissions received a score of 5, whereas those characterized by high energy consumption, significant carbon emissions, low solvent recovery, or costly pollutant treatment scored only 1 or 2.\u003c/p\u003e\n\u003cp\u003eBy integrating the economic efficiency and environmental impact evaluations, a comprehensive comparison of different production processes was conducted, providing valuable insights for process optimization, sustainability improvements, and industrial-scale implementation.\u003c/p\u003e"},{"header":"Result and Analysis","content":"\u003cp\u003e\u003cstrong\u003e1. Investigation of Conversion Efficiency for Preparing NCC from Wheat Straw via Eutectic Solvent Treatment\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.1 Response Surface Optimization\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.1.1 Effect of the Citric Acid-to-Ethylene Glycol Molar Ratio on NCC Conversion Efficiency\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe influence of the eutectic solvent (citric acid and ethylene glycol) molar ratio on NCC conversion efficiency is shown in Fig. 1. As the ethylene glycol content in the eutectic solvent system increased, NCC conversion efficiency initially rose and then declined. This trend was primarily attributed to the balance between the hydrogen-bonding network strength of the eutectic solvent, the dissolution capability for straw powder, and reaction selectivity\u003csup\u003e20\u003c/sup\u003e.When the molar ratio of citric acid to ethylene glycol was 1:2, the hydrogen-bonding network in the solvent system was optimal\u003csup\u003e21\u003c/sup\u003e，This condition effectively disrupted the crystalline structure of the straw powder while maintaining a favorable reaction environment, resulting in the highest NCC conversion efficiency (60.2%).However, when the molar ratio increased to 1:3, the excessive ethylene glycol led to a more sparse hydrogen-bonding network and an overly strong dissolution capacity. This caused the straw powder to depolymerize excessively into soluble oligomers and disrupted the selectivity of the reaction, ultimately lowering NCC conversion efficiency and reducing the stability of the crystalline structure.\u003csup\u003e22\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.1.2 Effect of reaction time on NCC conversion\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe effect of reaction time on NCC conversion efficiency is presented in Fig. 2. During shorter reaction times (2\u0026ndash;8 hours), the NCC conversion efficiency remained relatively stable, indicating that the reaction had not yet reached completion. When the reaction time was extended to 12 hours, the NCC conversion efficiency peaked at 67.6%, suggesting that the reaction was most complete at this point, with optimal depolymerization of straw powder and NCC formation. However, when the reaction time exceeded 12 hours, the conversion efficiency slightly decreased\u003csup\u003e23\u003c/sup\u003e. This decline might have been due to the over-depolymerization or further dissolution of straw powder into oligomers, which inhibited NCC production efficiency.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.1.3 Effect of Reaction Temperature on NCC Conversion Efficiency\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe impact of reaction temperature on NCC conversion efficiency is shown in Fig. 3. The conversion efficiency exhibited a rise followed by a decline as the reaction temperature increased, indicating that temperature played a critical role in the solvent\u0026rsquo;s depolymerization capability and the conversion efficiency of straw powder. As the temperature increased from 80\u0026deg;C to 100\u0026deg;C, NCC conversion efficiency rose from 65 % to 71.6 %. This improvement was attributed to the enhanced molecular activity of the solvent at higher temperatures \u003csup\u003e24\u003c/sup\u003e, leading to stronger interactions with straw powder molecules and promoting depolymerization and conversion. However, as the temperature increased to 110 \u0026deg;C, the conversion efficiency dropped to 69.5%, likely due to nonselective degradation of straw powder or partial dissolution into oligomers at higher temperatures, reducing NCC yield and purity. When the temperature was further increased to 120 \u0026deg;C, the conversion efficiency slightly recovered to 70.2 %, but it did not exceed the peak value of 71.6 % observed at 100 \u0026deg;C. These results indicated that 100 \u0026deg;C was the optimal reaction temperature, achieving a balance between solvent activity and straw powder stability to maximize conversion efficiency. In contrast, temperatures that were too low or too high reduced reaction efficiency.\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e1.1.4 Effect of the Solid-to-Liquid Ratio of Straw Powder and Eutectic Solvent on NCC Conversion Efficiency\u003c/p\u003e\n\u003cp\u003eThe influence of the eutectic solvent-to-straw powder ratio on NCC conversion efficiency is illustrated in Fig. 4. As the ratio increased, the NCC conversion efficiency first rose and then fell. At a solid-to-liquid ratio of 1:30, the conversion efficiency reached its maximum value of 70.2 %, indicating that a higher ratio provided sufficient solvent molecules to fully interact with straw powder molecules. This enhanced the solvent\u0026rsquo;s ability to disrupt the crystalline structure of straw powder, promoting efficient NCC production. However, as the ratio increased to 1:40 and 1:50, the conversion efficiency decreased to 67 % and 59.7 %, respectively. This decline was likely due to excessive dilution of the reaction system, which weakened the interaction strength between the solvent and straw powder molecules. Additionally, higher ratios may have led to the over-dissolution of straw powder into oligomers \u003csup\u003e25\u003c/sup\u003e, inhibiting selective conversion to NCC and thereby reducing the overall conversion efficiency.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e1.2 Response Surface Optimization Experimental Design\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eDevelopment and Analysis of Regression Models\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eA three-factor, three-level Box-Behnken experimental design was employed to optimize the NCC conversion efficiency (Y), considering reaction time (A), reaction temperature (B), and the solid-to-liquid ratio of eutectic solvent to straw powder (C). The design included 29 experimental runs, as shown in Table 2.\u003c/p\u003e\n\u003cp\u003eThe data from Table 2 were analyzed using Design Expert 13.0 software to fit a regression model that describes the relationship between NCC conversion efficiency and the selected factors. The resulting regression model is presented below:\u003c/p\u003e\n\u003cp\u003eY=71.96+0.0304 A-0.0508 B-0.0347 C+1.08AB-0.1203\u0026nbsp;\u0026nbsp;AC+1.17 BC-1.77 A\u0026sup2;-3.69 B\u0026sup2;-5.95C\u003csup\u003e\u0026sup2;\u003c/sup\u003e\u003c/p\u003e\n\u003cp\u003eThe regression analysis (Table 3) indicated that the response surface model was highly significant (P \u0026lt; 0.0001), with non-significant lack of fit (P \u0026gt; 0.05). These results suggest that the model is appropriate for analyzing and predicting the effects of different treatment conditions on NCC conversion efficiency. Among the tested factors, reaction temperature (B) had the most significant impact, followed by the solid-to-liquid ratio (C) and reaction time (A).\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eOptimization and Validation of Process Conditions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eResponse surface plots illustrating the interactions between the factors (reaction time, reaction temperature, and solid-to-liquid ratio) are shown in Fig. 5.\u003c/p\u003e\n\u003cp\u003eThe response surface analysis revealed that reaction time, reaction temperature, and the solid-to-liquid ratio directly or indirectly influenced NCC conversion efficiency. As seen in Fig. 5a, both reaction time and temperature exhibited an initial increase in NCC conversion efficiency, followed by a decrease. During the early stages of the reaction, longer times and higher temperatures effectively accelerated the reaction rate, leading to greater product yield. However, when reaction times exceeded 12 hours or temperatures surpassed 100\u0026deg;C, NCC conversion efficiency began to decline. This reduction may have been caused by the degradation of the target product over extended reaction durations and the occurrence of side reactions at elevated temperatures, such as the decomposition of sugars in the straw powder, resulting in the formation of byproducts and reduced overall conversion efficiency\u003csup\u003e26\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eFig. 5b illustrates the combined effects of reaction time and solid-to-liquid ratio on NCC conversion efficiency. The efficiency increased as reaction time and solid-to-liquid ratio rose, peaking at a ratio of approximately 30\u0026ndash;35 and a reaction time of 12\u0026ndash;13 hours. At short reaction times (\u0026lt;12 hours) or lower ratios (\u0026lt;20), insufficient solvent and incomplete reactions resulted in lower efficiency. Conversely, excessive reaction times (\u0026gt;12 hours) or high ratios (\u0026gt;35) suppressed further improvements in conversion efficiency. Prolonged reaction times increased the likelihood of side reactions, while excessive solvent diluted the reactant concentration, thus hindering the reaction \u003csup\u003e27\u003c/sup\u003e. The optimal conditions were identified as a reaction time of 12\u0026ndash;13 hours and a solid-to-liquid ratio of 30~35, yielding a peak NCC conversion efficiency of 71~72 %.\u003c/p\u003e\n\u003cp\u003eAs shown in Fig. 5c, the impact of solid-to-liquid ratio and reaction temperature on NCC conversion efficiency was also highly significant. At low ratios (\u0026lt;20), insufficient contact between the reactants and solvent limited the reaction. When the ratio reached 30, the reaction system achieved an ideal balance of solvent and solid, allowing for full diffusion and efficient reaction, which resulted in the highest conversion efficiency. At higher ratios (\u0026gt;35), however, excessive solvent diluted the reactant concentration, reducing reaction efficiency and lowering the conversion rate \u003csup\u003e28\u003c/sup\u003e. Similarly, reaction temperature followed a similar trend. At lower temperatures (\u0026lt;90\u0026deg;C), the reaction rate was too slow, and activation energy was insufficient, restricting NCC formation. The efficiency increased with temperature, peaking at around 102 \u0026deg;C. Beyond this, higher temperatures (\u0026gt;114\u0026deg;C) led to degradation of the target product or intensified side reactions \u003csup\u003e29\u003c/sup\u003e, Similarly, reaction temperature followed a similar trend. At lower temperatures (\u0026lt;90 \u0026deg;C), the reaction rate was too slow and activation energy was insufficient, restricting NCC formation. The efficiency increased with temperature, peaking at around 102\u0026deg;C. Beyond this, higher temperatures (\u0026gt;114 \u0026deg;C) led to degradation of the target product or intensified side reactions.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.Comparative Work of Conversion Efficiency of Wheat Straw and Cellulose to NCC Using DES, Ionic Liquid, Cellulase, and TEMPO Treatments\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.1Conversion Efficiency of Different Treatments\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe conversion efficiency of different agents in producing NCC from wheat straw powder is shown in Fig. 6. The results reveal significant differences, which are closely related to the reaction mechanisms of each agent and the raw material properties. DES demonstrated the highest conversion efficiency at 72.3 %, attributed to its ability to dissolve cellulose and partially remove non-cellulosic components, thereby significantly increasing cellulose exposure\u003csup\u003e30\u003c/sup\u003e，In comparison, the [DMIM][DMP] improved reaction activity by disrupting the hydrogen bonding network of cellulose \u003csup\u003e31\u003c/sup\u003e, achieving a conversion efficiency of 67.0 %. Cellulase directly degraded cellulose into NCC by hydrolyzing \u0026beta;-1,4-glycosidic bonds1 \u003csup\u003e32\u003c/sup\u003e，but due to the complex matrix of wheat straw powder, its conversion efficiency was limited to 54.0 %. TEMPO oxidant selectively oxidized the C6 hydroxyl groups to carboxyl groups \u003csup\u003e33\u003c/sup\u003e，but its conversion efficiency was also hindered by lignin and hemicellulose, resulting in a conversion efficiency of 56.7 %. Overall, DES emerged as the most promising treatment method for producing NCC from wheat straw powder due to its higher conversion efficiency and broader applicability.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.2 FTIR Analysis of NCC Produced by Different Treatments\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe FTIR spectra (Fig. 7) of NCC prepared from wheat straw powder and MCC revealed significant differences and trends in chemical structure and derivatization. Untreated wheat straw (Fig. 7a) showed broad \u0026ndash;OH absorption bands (~3400 cm\u003csup\u003e⁻\u0026sup1;\u003c/sup\u003e), strong C=O absorption peaks (~1730 cm\u003csup\u003e⁻\u0026sup1;\u003c/sup\u003e), and aromatic C=C peaks (~1600 cm\u003csup\u003e⁻\u0026sup1;\u003c/sup\u003e), indicative of abundant lignin and hemicellulose. MCC (Fig. 7b), being more purified, exhibited a narrower \u0026ndash;OH band, weaker C=O peaks, and stronger C\u0026ndash;O\u0026ndash;C absorption bands near 1100 cm\u003csup\u003e⁻\u0026sup1;\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eDES-treated wheat straw powder (Fig. 7c) displayed nearly complete disappearance of lignin and hemicellulose peaks, along with a pronounced enhancement of C\u0026ndash;O\u0026ndash;C absorption bands. This change indicates that DES effectively removed non-cellulosic components from wheat straw, significantly increasing cellulose purity and crystallinity \u003csup\u003e34\u003c/sup\u003e.treatment (Fig. 7d) also resulted in enhanced C\u0026ndash;O\u0026ndash;C absorption, but since cellulase mainly hydrolyzes \u0026beta;-1,4-glycosidic bonds, it caused minimal changes to the chemical structure, and the C=O absorption bands remained relatively unchanged. This method maintained the fundamental cellulose framework while improving crystallinity\u003csup\u003e18\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eTEMPO oxidation (Fig. 7e) demonstrated pronounced derivatization effects. The carboxyl absorption peak (~1730 cm\u003csup\u003e⁻\u0026sup1;\u003c/sup\u003e) was significantly enhanced, while the \u0026ndash;OH absorption band (~3400 cm\u003csup\u003e⁻\u0026sup1;\u003c/sup\u003e) was relatively reduced, indicating that TEMPO selectively oxidized C6 hydroxyl groups into carboxyl groups and increased functionalization levels \u003csup\u003e35\u003c/sup\u003e.\u0026nbsp;[DMIM][DMP] treatment (Fig. 7f) mainly disrupted intra- and intermolecular hydrogen bonding within cellulose, promoting physical reorganization and crystallization. The FTIR spectra showed a weakening of \u0026ndash;OH absorption and an enhancement of C\u0026ndash;O\u0026ndash;C bands, while the C=O peaks remained stable, suggesting no significant chemical derivatization\u003csup\u003e36\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eIn summary, producing NCC from wheat straw powder requires efficient impurity removal to eliminate lignin and hemicellulose. DES effectively enhances crystallinity and purity, cellulase treatment is mild and retains the native properties of cellulose while improving crystallinity, TEMPO oxidation greatly increases carboxylation levels, and [DMIM][DMP] excels in physical reorganization and crystallization. DES stands out for its excellent impurity removal capability and improvement of cellulose crystallinity, making it a promising method for producing NCC from wheat straw powder.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.3 XRD Analysis of NCC Crystallinity\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eXRD patterns (Fig. 8A) reveal clear differences in the crystallinity improvement and structural changes of NCC prepared from wheat straw powder after different treatments. Untreated wheat straw powder (Fig. 8a) displayed broad and weak diffraction peaks (2\u0026theta; = 15.1\u0026deg; and 22\u0026deg;), indicating low crystallinity due to the presence of amorphous lignin and hemicellulose \u003csup\u003e37\u003c/sup\u003e. MCC (Fig. 8b), which inherently has higher crystallinity, showed sharp diffraction peaks at 2\u0026theta; = 22.5\u0026deg;, reflecting minimal amorphous content.\u003c/p\u003e\n\u003cp\u003eAmong the treatments, DES (Fig. 8f) showed the most significant improvement in crystallinity. The diffraction peak at 2\u0026theta; = 22.5\u0026deg; was sharp and intense, suggesting that DES efficiently removed amorphous components (e.g., lignin, hemicellulose) through strong hydrogen bonding and acid-base interactions, thereby greatly enhancing crystallinity \u003csup\u003e38\u003c/sup\u003e [DMIM][DMP] treatment (Fig. 8d) also demonstrated a notable increase in crystallinity by breaking cellulose hydrogen bonds and promoting molecular rearrangement, as evidenced by stronger diffraction peaks and reduced amorphous content\u0026nbsp;\u003csup\u003e39\u003c/sup\u003e.\u0026nbsp;TEMPO oxidation (Fig. 8c), focusing on chemical derivatization, selectively oxidized cellulose\u0026rsquo;s C6 hydroxyl groups into carboxyl groups, conferring new functional groups\u0026nbsp;\u003csup\u003e40\u003c/sup\u003e.However, its effect on enhancing crystallinity was relatively limited. Cellulase treatment (Fig. 8e) increased crystallinity to a lesser extent, as it hydrolyzed \u0026beta;-1,4-glycosidic bonds\u003csup\u003e41\u003c/sup\u003e, partially removing amorphous regions. However, its milder action left some amorphous components intact, resulting in lower crystallinity improvement compared to DES and [DMIM][DMP].\u003c/p\u003e\n\u003cp\u003eIn conclusion, due to its low initial crystallinity and high amorphous content, wheat straw powder has significant potential for modification. DES and [DMIM][DMP] were the most effective treatments for achieving high-quality crystalline cellulose. TEMPO oxidation is better suited for applications requiring high functionalization, while cellulase treatment is ideal for preserving the inherent characteristics of cellulose. Considering the desired performance and processing requirements, DES treatment offers the greatest improvement in crystallinity and optimal crystalline structure when producing NCC from wheat straw powder.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e2.4\u0026nbsp;\u003c/strong\u003e\u003cstrong\u003eSEM Analysis of NCC Morphology and Crystallinity\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eHigh impurity content in wheat straw powder significantly affected the ability of different agents to modify morphology and enhance crystallinity (Fig. 9 Table 4) (the details are shown in Supplementary information 3、4). TEMPO oxidation selectively introduced carboxyl groups by oxidizing C6 hydroxyl groups in cellulose, adding functionalized modifications. However, it showed limited effectiveness in optimizing morphology and controlling size. The NCC produced from wheat straw powder (Fig. 9a) had particle sizes of 93.4\u0026ndash;54.4 nm, with larger and unevenly distributed particles, indicating that the high impurity content interfered with TEMPO\u0026rsquo;s ability to modify cellulose fiber morphology.\u003c/p\u003e\n\u003cp\u003e[DMIM][DMP] treatment disrupted hydrogen bonds within cellulose and promoted molecular rearrangement, improving crystallinity and some degree of morphological regularity \u003csup\u003e42\u003c/sup\u003e. The NCC produced from wheat straw powder (Fig. 9c) exhibited particle sizes of 92.1\u0026ndash;44.7 nm, with improved crystallinity, though the morphology remained irregular, and agglomeration was evident. This suggests that ionic liquids have limited tolerance to high impurity levels.\u003c/p\u003e\n\u003cp\u003eCellulase treatment, being a mild modification method, preserved the original characteristics of cellulose and increased crystallinity but showed weaker effects on morphology and size optimization. The NCC produced from wheat straw powder (Fig. 9e) had particle sizes of 82.8\u0026ndash;47.5 nm, with significant agglomeration. The enzymatic hydrolysis was insufficient to completely remove lignin and hemicellulose, making it difficult to obtain regular NCC morphology.\u003c/p\u003e\n\u003cp\u003eDES treatment dissolved lignin, hemicellulose, and other non-cellulosic components, breaking cellulose hydrogen bonds and significantly enhancing crystallinity and morphology \u003csup\u003e43\u003c/sup\u003e The NCC produced from wheat straw powder (Fig. 9g) had particle sizes of 98.8\u0026ndash;52.2 nm. While still irregular in shape, it showed notable improvement compared to the raw material. This highlights DES\u0026rsquo;s excellent ability to remove non-cellulosic components and enhance cellulose crystallinity and morphology \u003csup\u003e44\u003c/sup\u003e.\u003c/p\u003e\n\u003cp\u003eOverall, for wheat straw powder with high impurity content, DES and [DMIM][DMP] both performed well in removing non-cellulosic components and improving crystallinity, with DES demonstrating greater advantages. DES not only achieved higher crystallinity but also partially improved cellulose morphology. [DMIM][DMP], while also promoting crystallization, showed slightly lower tolerance to high impurity levels. TEMPO oxidation effectively increased functionalization levels but had limited control over morphology and size. Cellulase treatment was suitable for mild modifications that preserved the native cellulose properties, though its morphological optimization was less effective than DES and [DMIM][DMP] treatments. Ultimately, the choice of treatment agent should consider multiple performance criteria, including functionalization, crystallinity, and morphology. DES\u0026rsquo;s excellent impurity removal and crystallinity enhancement capabilities make it a superior choice for processing high-impurity wheat straw powder.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e3.\u003c/strong\u003e\u003cstrong\u003e\u0026nbsp;Recyclable Process Design and Environmental Evaluation of NCC Production\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eIn this work, the production processes of NCC were evaluated by comparing two primary indicators: economic efficiency and environmental feasibility\u0026nbsp;(the details are shown in Supplementary information 5). Initially, four methods\u0026mdash;DES, [DMIM][DMP], Cellulase, and TEMPO\u0026mdash;were examined regarding their respective requirements for straw, chemical reagents, and electricity in the production of one ton of NCC (Table 5). The results indicated that DES demonstrates a pronounced economic advantage, whereas [DMIM][DMP]\u0026mdash;due to the high cost of ionic liquids\u0026mdash;fails to achieve significant economic returns in large-scale production. By comparison, the Cellulase approach entails relatively lower chemical reagent expenses, while the TEMPO oxidation route incurs considerable costs owing to the use of expensive oxidizing agents.\u003c/p\u003e\n\u003cp\u003eBeyond economic considerations, this work also assessed the four methods from the perspectives of Energy Consumption (ECS), Carbon Footprint (CF), Solvent Recovery (SR), and Wastewater Treatment (WWT) (Fig.10). The findings show that both Cellulase and DES perform well in terms of energy consumption and wastewater management, thereby exhibiting favorable environmental compatibility. In contrast, [DMIM][DMP] exhibits notable environmental challenges arising from the complexity of synthesizing, recovering, and disposing of ionic liquids, while TEMPO oxidation faces similar issues due to its reliance on oxidizing agents and the associated by-product handling, thus necessitating thorough evaluation of its environmental impact in practical applications.\u003c/p\u003e\n\u003cp\u003eTaking both economic and environmental factors into account, DES stands out as the most viable option, offering low production costs and strong environmental performance, thereby making it particularly suitable for industrial-scale manufacturing and sustainable development. Nevertheless, the Cellulase, TEMPO, and [DMIM][DMP] processes retain their unique value for producing high-quality or functionalized cellulose products, although their potentially high costs and environmental implications call for more prudent consideration when selecting an appropriate process route.\u003c/p\u003e"},{"header":"Conclusion","content":"\u003cp\u003eThis study systematically addresses the technical, economic, and environmental challenges in producing CNC from straw by comparing four methods: CA\u0026ndash;EG DES, the [DMIM][DMP], cellulase hydrolysis, and TEMPO oxidation. Each method\u0026rsquo;s conversion efficiency, structural characterization, and economic and environmental feasibility were evaluated. Results indicate that the CA\u0026ndash;EG DES process exhibits pronounced advantages in terms of yield, cost-effectiveness, and environmental compatibility, highlighting its potential for large-scale industrial deployment in line with sustainable development goals. Under optimized temperature, reaction duration, and solid\u0026ndash;liquid ratio conditions, CA\u0026ndash;EG DES effectively removes non-cellulosic components, thereby increasing the yield and crystallinity of CNC while reducing energy consumption and environmental burden. These findings align with the recent trend of \u0026ldquo;green solvents\u0026rdquo; in the production of cellulose-based nanomaterials. By contrast, although ionic liquids significantly enhance cellulose crystallinity, their high cost and difficult solvent recovery hinder extensive industrial application. Meanwhile, cellulase treatment preserves cellulose integrity under mild conditions but exhibits lower efficiency in multi-component straw systems and requires high substrate purity and enzyme activity. TEMPO oxidation enables selective oxidation and functionalization yet encounters notable challenges in cost and wastewater treatment. From a comprehensive process, economic, and environmental perspective, the CA\u0026ndash;EG DES method clearly stands out due to its lower raw material and energy requirements, readily recyclable solvent, mild reaction parameters, and reduced wastewater treatment needs. Future work can focus on tailoring CA\u0026ndash;EG DES formulations for various types of lignocellulosic feedstocks, while further technological improvements\u0026mdash;such as lowering solvent viscosity and energy demands, enhancing recovery rates, and accommodating diverse biomass sources\u0026mdash;could foster a more efficient, greener CNC production framework. This strategy ultimately supports the high-value-added utilization of agricultural straw and other renewable biomasses, laying a foundation for the development of novel bio-based materials.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eFunding\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eWe wish to express our thanks for the support from the Postgraduate Research \u0026amp; Practice Innovation Program of Jiangsu Province (KYCX25_4409), the Zhenjiang Carbon Peaking \u0026amp; Neutrality Project (No. CN2022001) and Jiangsu Overseas Research \u0026amp; Training Program for University Prominent Young \u0026amp; Middle-aged Teachers and Presidents.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor Contributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eNiuniu Deng Conceptualization; Data curation; Formal analysis; Writing – original draft. Qiang Li: Methodology; Supervision; Writing- Reviewing and Editing; Project administration. Wenjie Wang: Investigation; Visualization. Gengsheng Ji: Partial data collection.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConflict of Interest\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors have declared no conflict of interest.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n \u003cli\u003eChen, S.\u003cem\u003e\u0026nbsp;et al.\u003c/em\u003e Disassembly of lignocellulose into cellulose, hemicellulose, and lignin for preparation of porous carbon materials with enhanced performances. \u003cem\u003eJ. Hazard. 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Crops Prod.\u003c/em\u003e \u003cstrong\u003e223\u003c/strong\u003e, 120173 (2025). https://doi.org:10.1016/j.indcrop.2024.120173\u003c/li\u003e\n\u003c/ol\u003e"},{"header":"Tables","content":"\u003cp\u003eTable 1: response surface experimental factor levels\u003c/p\u003e\n\u003ctable border=\"1\" cellspacing=\"0\" cellpadding=\"0\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"2\" valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003eFactor\u003c/p\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd colspan=\"3\" valign=\"top\" style=\"width: 415px;\"\u003e\n \u003cp\u003eCoding level\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003eA\u0026nbsp;Time（h）\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e12\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e24\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003eB\u0026nbsp;Temperature（\u0026deg;C）\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e90\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e100\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e120\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003eC\u0026nbsp;Solid-liquid ratio（g/ml）\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e1:20\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e1:30\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd valign=\"top\" style=\"width: 138px;\"\u003e\n \u003cp\u003e1:40\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n\u003c/table\u003e\n\u003cp\u003eTable 2 box Behnken test design and results\u003c/p\u003e\n\u003cdiv align=\"center\"\u003e\n \u003ctable border=\"1\" cellspacing=\"0\" cellpadding=\"0\" width=\"100%\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd rowspan=\"2\" style=\"width: 20px;\"\u003e\n \u003cp\u003eTest No\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd colspan=\"3\" style=\"width: 60px;\"\u003e\n \u003cp\u003eFactor\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd rowspan=\"2\" style=\"width: 19px;\"\u003e\n \u003cp\u003eNC conversion%\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003ea\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eb\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003ec\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e65\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e62.7\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e68.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e71.6\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e64.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e66.8\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e72\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e70.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e64.8\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e10\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e62.8\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e11\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e62.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e12\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e66\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e13\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e60.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e14\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e72.3\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e15\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e-1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e71.8\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e16\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e64\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e17\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 19px;\"\u003e\n \u003cp\u003e63.7\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n\u003c/div\u003e\n\u003cp\u003eNote: \u0026quot;*\u0026quot; has significant difference (p\u0026lt;0.05), The difference of \u0026quot;* *\u0026quot; was extremely significant (p\u0026lt;0.01)\u003c/p\u003e\n\u003cp\u003eTable 3 Variance Analysis of regression model\u003cbr\u003e\u0026nbsp;\u003c/p\u003e\n\u003ctable border=\"1\" cellspacing=\"0\" cellpadding=\"0\" width=\"100%\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eSource\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003eSum of Squares\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003edf\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003eMean Square\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003eF-value\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003ep-value\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eModel\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e238.98\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e26.55\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e28.48\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0001\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e**\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eA\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e0.007\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.007\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0075\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.9333\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eB\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e0.0206\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0206\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0221\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.8861\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eC\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e0.0091\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0091\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0098\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.924\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eAB\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e4.97\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e4.97\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e5.33\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0544\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eAC\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e0.0582\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0582\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0624\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.81\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eBC\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e5.82\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e5.82\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e6.25\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.041\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e*\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eA\u0026sup2;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e12.86\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e12.86\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e13.79\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0075\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e**\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eB\u0026sup2;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e42.84\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e42.84\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e45.95\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.0003\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e**\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eC\u0026sup2;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e148.96\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e148.96\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e159.76\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e\u0026lt; 0.0001\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e**\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eResidual\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e6.53\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.9324\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eLack of Fit\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e3.88\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e1.29\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e1.95\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.2631\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003enot significant\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003ePure Error\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e2.65\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e0.662\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003eCor Total\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 14px;\"\u003e\n \u003cp\u003e245.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 6px;\"\u003e\n \u003cp\u003e16\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 12px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 20px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n\u003c/table\u003e\n\u003cp\u003eTable 4: size comparison under SEM of NCC prepared by straw powder treated with different reagents\u003c/p\u003e\n\u003ctable border=\"1\" cellspacing=\"0\" cellpadding=\"0\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 111px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 111px;\"\u003e\n \u003cp\u003eTEMPO\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 111px;\"\u003e\n \u003cp\u003e[DMIM][DMP]\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 111px;\"\u003e\n \u003cp\u003ecellulase\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 111px;\"\u003e\n \u003cp\u003eDES\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 111px;\"\u003e\n \u003cp\u003eSize of NCC (Length- width)/nm\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 111px;\"\u003e\n \u003cp\u003e93.4-54.4\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 111px;\"\u003e\n \u003cp\u003e92.1-44.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 111px;\"\u003e\n \u003cp\u003e82.8-47.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 111px;\"\u003e\n \u003cp\u003e98.8-52.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n\u003c/table\u003e\n\u003cp\u003eTable 5: Comparison of Material Requirements and Cost Estimates for Producing 1 Ton of NCC Across Four Treatment Methods\u003c/p\u003e\n\u003cdiv align=\"Left\"\u003e\n \u003ctable border=\"0\" cellspacing=\"0\" cellpadding=\"0\" width=\"661\"\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 69px;\"\u003e\n \u003cp\u003e\u0026nbsp;\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003eStraw dosage(t)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 113px;\"\u003e\n \u003cp\u003eStraw（CNY）\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 109px;\"\u003e\n \u003cp\u003eChemical (CNY)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003eElectricity (CNY)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 104px;\"\u003e\n \u003cp\u003eAll-in cost（CNY）\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 104px;\"\u003e\n \u003cp\u003eAll-in cost（USD）\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 69px;\"\u003e\n \u003cp\u003eDES\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e1.38\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 113px;\"\u003e\n \u003cp\u003e61.16\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 109px;\"\u003e\n \u003cp\u003e7356.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e1067.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 104px;\"\u003e\n \u003cp\u003e\u0026yen;8485.46/t\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 104px;\"\u003e\n \u003cp\u003e$1164.96\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 69px;\"\u003e\n \u003cp\u003e[DMIM][DMP]\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e1.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 113px;\"\u003e\n \u003cp\u003e66\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 109px;\"\u003e\n \u003cp\u003e157300\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e1577\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 104px;\"\u003e\n \u003cp\u003e\u0026yen;158943/t\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 104px;\"\u003e\n \u003cp\u003e$21823.6\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 69px;\"\u003e\n \u003cp\u003eCellulase\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e1.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 113px;\"\u003e\n \u003cp\u003e83.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 109px;\"\u003e\n \u003cp\u003e31588.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e1171.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 104px;\"\u003e\n \u003cp\u003e\u0026yen;32760.4/t\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 104px;\"\u003e\n \u003cp\u003e$4498.16\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd style=\"width: 69px;\"\u003e\n \u003cp\u003eTEMPO\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 87px;\"\u003e\n \u003cp\u003e1.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 113px;\"\u003e\n \u003cp\u003e79.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 109px;\"\u003e\n \u003cp\u003e72630\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 77px;\"\u003e\n \u003cp\u003e1328\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 104px;\"\u003e\n \u003cp\u003e\u0026yen;74037.2/t\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd style=\"width: 104px;\"\u003e\n \u003cp\u003e$10165.67\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n\u003c/div\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Agricultural Straw, Biomass-Derived, Deep Eutectic Solvent (DES), High Solvent Recovery, Cellulose Nanocrystal, Sustainable materials","lastPublishedDoi":"10.21203/rs.3.rs-7700269/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-7700269/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eAgricultural residues represent a valuable renewable resource for producing sustainable functional materials. Here, we report a biomass-derived DES (Deep Eutectic Solvent) system, composed of CA\u0026ndash;EG (Citric acid and Ethylene glycol) DES, for the selective extraction of CNC (Cellulose Nanocrystal) from agricultural straw. Operating under mild conditions, the DES efficiently disrupts the lignocellulosic network, yielding CNC with high crystallinity (72.3%) and uniform nanoscale morphology. The process achieves over 85% solvent recovery, significantly reducing chemical input and waste generation, and offers clear advantages in conversion efficiency, operational simplicity, and environmental compatibility compared to other green strategies such as [DMIM][DMP] (1,3-Dimethylimidazolium dimethyl phosphate), enzymatic hydrolysis, and TEMPO oxidation. Comprehensive structural characterization confirmed the high-quality CNC obtained, while techno-economic evaluation demonstrated the cost-effectiveness and industrial scalability of the process. This work provides an integrated, resource-efficient, and environmentally benign platform for transforming agricultural waste into high-value nanomaterials, contributing to circular material systems and the advancement of sustainable manufacturing.\u003c/p\u003e","manuscriptTitle":"Green and Scalable Production of Nanocrystalline Cellulose Driven by a Biomass-Derived Deep Eutectic Solvent","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2026-01-30 12:57:30","doi":"10.21203/rs.3.rs-7700269/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"8a152a02-a4c2-49eb-81cb-500ef74c11b8","owner":[],"postedDate":"January 30th, 2026","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2026-03-05T23:24:02+00:00","versionOfRecord":[],"versionCreatedAt":"2026-01-30 12:57:30","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-7700269","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-7700269","identity":"rs-7700269","version":["v1"]},"buildId":"XKTyCvWXoU3ODBz1xrDgd","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}