Synthesis of CHA from MFI by three interzeolite transformation strategies and its Application in NH 3 -SCR reaction

Synthesis of CHA from MFI by three interzeolite transformation strategies and its Application in NH 3 -SCR reaction | 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 Synthesis of CHA from MFI by three interzeolite transformation strategies and its Application in NH 3 -SCR reaction Yufeng Liu, Yuping Li, Ze Chen, Fuchao Ji, Xiaohong Liang, Lina Han, and 1 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-5263931/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 17 Dec, 2024 Read the published version in Journal of Porous Materials → Version 1 posted 16 You are reading this latest preprint version Abstract CHA Zeolites are currently considered as the most effective catalysts to meet the increasingly stringent emission requirements of diesel vehicles. Herein, the synthesis of SSZ-13 zeolites(CHA topology) using ZSM-5 (MFI topology) with various SiO 2 /Al 2 O 3 ratios as parent zeolites were investigated in the presence of N,N,N, trimethtyl-1-adamantammonium hydroxide (TMAdaOH). The crystallization processes of three different strategies, that is, high silica ZSM-5 with additional Al source(HSZ + Al), completely zeolite to zeolite(CZTZ) transformation and low silica ZSM-5 with additional Si source(LSZ + Si) were compared. The results show that pure SSZ-13 zeolites with high crystallinity can be synthesized at 160°C for only 6 h by CZTZ strategy. While for the HSZ + Al and LSZ + Si synthesis systems, the complete transformation from MFI to CHA can even be shortened to 4.5 h at 160°C, suggesting the promoting effect of additional Al- or Si- source for MFI-CHA transformation. The rapid MFI-CHA transformation may be related to fast disintegration of parent ZSM-5 under the promotion of TMAdaOH template. Meanwhile, the five-membered rings predominating in the MFI framework rapidly disassembled and rearranged into favorable double six-membered ring and CHA cage composite building units, thus facilitate the rapid formation the CHA framework. Additionally, the resultant samples, after Cu 2+ exchange, showed superior catalytic activity and hydrothermal stability for the selective catalytic reduction of NO x with NH 3 . The operation temperature window (NO x conversion > 90%) of HSZ-4.5 h, CZTZ-6.0 h and LSZ-4.5 h samples were all about 200 ~ 500°C. Among three samples, the HSZ-4.5 h presents best low-temperature catalytic activity, while CZTZ-6.0 h and LSZ-4.5 h samples show more superior hydrothermal stability. SSZ-13 zeolite Interzeolite transformation ZSM-5 NH3-SCR of NOx Diesel exhaust Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 1. Introduction Zeolites, a family of crystalline microporous aluminosilicate materials, have been widely applied in catalyst, adsorption, and ion-exchange applications[ 1 , 2 ]. This variety of applications is due to their uniform pore structure, high specific surface area, suitable acidity, special shape selectivity, and brilliant thermal/hydrothermal stability[ 3 – 5 ]. Among them, SSZ-13, a typical CHA zeolite, is composed of 4 and 6 membered rings organized in double six-membered rings (D6Rs) composite building units (CBUs) and large ellipsoidal CHA cages (6.7*10Å) with pore openings of 3.8*3.8 Å. This unique pore system confers it excellent properties in catalysis such as NO x abatement, methanol-to-olefins (MTO) and ethylene-to-propylene (ETP) reaction[ 6 – 9 ]. Generally, zeolites are synthesized under conventional hydrothermal conditions, which taking amorphous aluminosilicate gel as raw materials[ 10 , 11 ]. Over the last decade, the strategy called interzeolite conversion(IZC) has attracted considerable attention for zeolite synthesis, which uses easily available or inexpensive crystallized zeolites as silica/alumina or alumina source to synthesize the target zeolite. Compared with conventional hydrothermal synthesis, the IZC method achieves various specific merits, such as rapid crystallization[ 12 – 14 ], high solid yield[ 15 , 16 ], specific Al distribution[ 17 ], unusual framework composition[ 18 ], and small crystal size[ 19 , 20 ]. It is widely accepted that the successful interzeolite transformation is preferably achieved from those parent zeolites containing common composite building units(CBUs), with less dense framework density(FD), and larger pore size. Up to now, a variety of zeolites has been used as parent zeolite to synthesize SSZ-13 by IZC method, including LEV[ 12 ], MFI[ 15 ], BEA[ 16 ], GIS[ 21 ], LTL[ 22 , 23 ], FAU[ 24 ], LTA[ 25 ], and FER[ 26 ]. Among them, FAU, LEV and LTL zeolite could be efficiently converted into SSZ-13, which were attributed to that the starting zeolite contains the common CBUs with the target zeolite, namely D6Rs. However, the other 5 zeolites listed(GIS(8-membered rings(8MRs) pore, FD = 16.4 T/1000 Å 3 ), BEA(12MRs pore, FD = 15.3 T/1000 Å 3 ), MFI(10MRs pore, FD = 18.4 T/1000 Å 3 ), FER(10MRs pore, FD = 17.6 T/1000 Å 3 ), and LTA(8MRs pore, FD = 14.2T/1000 Å 3 ), with no common CBUs (D6Rs) with CHA(8MRs pore, FD = 15.1 T/1000 Å 3 ), can also be successfully converted to SSZ-13. Additionally, compared to the CHA zeolite, these starting zeolites had higher FD except for LTA, verifies that framework density (FD) actually had only a weak effect on successful IZC. As for the effect of pore size, these starting zeolites have larger (FAU, LTL, BEA, LTA, MFI and FER) or smaller (LEV and GIS) pore sizes than that of CHA structure. Therefore, the interzeolite transformation mechanism is not yet fully elucidated, especially when the transformation occurs between two zeolites without similar structure features. ZSM-5 zeolite (10MRs pore, FD = 18.4 T/1000 Å 3 ) with MFI topology, which does not contain D6Rs units but a mass of single five-membered rings (S5Rs), as well as a small amount of single four-membered rings (S4Rs) and six-membered rings (S6Rs). For MFI-CHA transformation, it is unfavorable from the perspective of both thermodynamics (higher FD of starting zeolite than that of target one) and dynamics (without common D6R CBUs). At present, there are only a few reports on the successful transformation from ZSM-5 to SSZ-13[ 27 , 28 ]. Moreover, in these existing reported synthesis of SSZ-13 from ZSM-5, ZSM-5 is usually used as sole Si-/Al- source[ 28 ] or as an Al-source combined with additional silica sources[ 29 ]. As we know, the successful complete transformation of the starting zeolite is highly dependent on its SAR. Moreover, the addition of extra Si- or Al- source can not only broaden the SAR range of the initial zeolite required for the synthesis of the product zeolite, but also modulate the crystallization process, the morphology and size, and the distribution of the Al atom of the product zeolite. Herein, we adopt a new interzeolite conversion strategy based on a combination of a high-silica ZSM-5 and an additional Al- source (denoted as HSZ + Al) to synthesize SSZ-13 zeolite. Meanwhile, for comparation, the other ZSM-5 with medium and low SARs were also selected to prepare SSZ-13 by the methods of completely zeolite to zeolite (CZTZ) and low-silica ZSM-5 with a combination of additional Si-source (LSZ + Si), respectively. The crystallization processes of the CHA zeolite from HSZ + Al, CZTZ and LSZ + Si methods were monitored and analyzed by various characterization techniques. Finally, the catalytic performances of the CHA zeolites synthesized from these three experimental strategies after copper ion exchange in NH 3 -SCR reaction of NO x were investigated. 2. Experimental 2.1 Materials The reagents used in this study are as follows: sodium hydroxide(NaOH, AR, 96 wt%) were purchased from Tianjin Kemiou Chemical Reagent Co., Ltd, ammonium chloride (NH 4 Cl, AR, 99.5 wt%) and aluminium sulfate octadecahydrate (Al 2 (SO 4 ) 3 ·18H 2 O, AR, 99 wt%) were purchased from Tianjin wind boat chemical reagent technology Co., Ltd. N, N, N-trimethyladamantammonium hydroxide (25 wt% TMAdaOH in water) were provided by Dayou chemical co., LTD. Guangzhou. Fumed silica (92 wt% SiO 2 ) were obtained from Qingdao Ocean Chemical Factory Co. ZSM-5 zeolites (SAR = 24,38 and 120) were either obtained from commercial suppliers (Nankai University Catalyst Co Ltd) or prepared in-house. Copper nitrate trihydrate (Cu(NO 3 ) 2 ·3H 2 O, AR 99 wt%) were provided by Shanghai McLean Biochemical Technology Co., Ltd. All chemicals were used without further purification. 2.2 Preparation of SSZ-13 zeolite from ZSM-5 Experiments of the synthesis of SSZ-13 zeolites were carried out by three experimental schemes, namely using a combination of ZSM-5 with high SAR and aluminium sulfate octadecahydrate as Si- and Al- sources (HSZ + Al), using ZSM-5 with medium SAR as the sole source of Si and Al (complete zeolite to zeolite transformation) and using a combination of low silica ZSM-5 and fumed silica as Al- and Si-sources(LSZ + Si), respectively(Table 1 ). It needs to be mentioned that the SSZ-13 zeolites were all synthesized with an initial molar composition of 1SiO 2 : 0.0263Al 2 O 3 : 0.1Na 2 O : 0.2TMAdaOH : 15H 2 O. (1) HSZ + Al approach In a typical synthesis, aluminium sulfate octadecahydrate,NaOH, TMAdaOH and deionized water was mixed to form a clear solution. Then, ZSM-5 (SAR = 120) zeolite was added in the above mixture under stirring for 1 h. (2) CZTZ approach In a typical synthesis, NaOH, TMAdaOH and deionized water was mixed to form a clear solution. Then ZSM-5(SAR = 38) zeolite was added in the above mixture under stirring for 1 h. (3) LSZ + Si approach In a typical synthesis, NaOH, TMAdaOH and deionized water was mixed to form a clear solution. Then, fumed silica was slowly added in the above solution keeping with vigorous stirring for 1 h. With a further addition of ZSM-5(SAR = 24) zeolite under stirring for 1 h. Subsequently, in all cases, SSZ-13 (2 wt% of the silica) was added as a seed crystal and the mixture was stirred for 1 h. Finally, the resulting gel was transferred into stainless steel autoclave with a 100 mL Teflon liner. After crystallization at 160°C for 1.5 ~ 48 h, solid products were collected by centrifugation, washed thoroughly with distilled water until a near neutral pH was achieved, and then dried overnight at 80°C. The as-synthesized SSZ-13 sample was calcined to remove the OSDA at 550°C for 8 h and obtain the calcined SSZ-13 sample. Table 1 Starting materials prepared using different combinations of silica༆alumina sources Starting materials (abbreviation) Silica source Alumina source Parent zeolites High-silica ZSM-5 + alumina (HSZ + Al) —— Al 2 (SO 4 ) 3 · 18H 2 O ZSM-5 (SiO 2 /Al 2 O 3 = 120) High-silica ZSM-5 (CZTZ) —— —— ZSM-5 (SiO 2 /Al 2 O 3 = 38) Low-silica ZSM-5 + silica (LSZ + Si) Fumed silica —— ZSM-5 (SiO 2 /Al 2 O 3 = 24) 2.3 Preparation of Cu-SSZ-13 zeolite The NH 4 -form SSZ-13 sample was obtained by ion-exchange of the calcined sample with NH 4 Cl solution (1.0 M, liquid/solid = 20) at 80°C, each time is 3 h for a total of two times. Then, H-form SSZ-13 sample was acquired by NH 4 -form SSZ-13 calcination at 500°C for 4 h. The Cu-form sample was prepared by ion exchange of the H-form sample two times with Cu(NO 3 ) 2 solution (0.1 M, liquid/solid = 100) at 80°C, and each time is 3 h, followed by filtration, washing and drying at 80°C. 2.4 Samples Characterization Powder X-ray diffraction (XRD) patterns of the samples were recorded on a MiniFlex 600 X-ray diffractometer(Japan, Rigaku) using Cu Kα radiation at 40 kV and 15 mA. The relative crystallinity of each sample was determined by calculating the ratio of the total area of five major diffraction peaks in the obtained sample at 2θ = 9.6, 16.2, 20.8, 24.9 and 26.2° to that of the SSZ-13 seed zeolite (100% crystallinity). The TENSOR 27 Fourier-transform infrared spectrometer produced by BRUKER Company was used for measurement of FTIR spectra of the samples by the conventional KBr(spectroscopy grade) pellet technique. The crystal morphology of the samples was observed by a JEOL/JSM-6700F scanning electron microscopy (SEM). Energy dispersive spectroscopy (EDS) element analysis was performed operated at 10 kV. Thermal analysis was performed using Rigaku Thermo Plus Evo TG8120. Approximately 10 mg of the sample was introduced in an alumina crucible and loaded in the analyzer chamber. The samples were heated from room temperature to 800°C with a heating rate of 10°C·min − 1 under an air flow of 30 mL·min − 1 . Textural properties of the samples were measured by N 2 adsorption at 77 K on a Micrometrics ASAP 2020 system. Prior to the experiment, the samples were degassed at 200°C for 8 h, and then adsorbed N 2 at -196°C. The specific surface area of the sample was calculated based on the BET equation, and the micropore volume and surface area were determined using the t-plot method. The acidity of the samples was measured using an NH 3 temperature-programmed desorption instrument (NH 3 -TPD, Micrometrics AutoChem II 2920 chemisorption analyzer) equipped with a thermal conductivity detector (TCD). 0.1 g sample was pretreated at 550°C for 30 min and then cooled to 100°C in Ar. Subsequently, the sample adsorbed NH 3 for 0.5 h under the mixed gas of 10% NH 3 /Ar. After purging in Ar for 0.5 h at 100°C to remove the weakly adsorbed NH 3 . The measurement of the desorbed NH 3 was performed from 100 to 650°C at a rate of 10°C·min − 1 in Ar flow (30 mL·min − 1 ). H 2 Temperature-programmed reduction (H 2 -TPR) was also performed on the AUTO-CHEM-II-2920 with a thermal conductivity detector (TCD). 0.1 g sample was pretreated in a 5% O 2 /He flow at 300°C for 30 min, then heated from room temperature to 800°C at 10°C·min − 1 in the mixed gas of 10 vol% H 2 /Ar (40 mL·min − 1 ). The hydrogen consumption was measured quantitatively by TCD. The element composition(SAR) was determined by inductively coupled plasma optical emission spectrometry (ICP-OES) (Agilent, 720). The 27 Al and 29 Si MAS NMR spectra were measured on a Bruker Avance III 600 spectrometer at 156.4 and 99.3 MHz, respectively. 27 Al NMR spectra were recorded under a spinning rate of 20 KHz, and the reference chemical shift was Al(NO 3 ) 3 aqueous solution. The 29 Si MAS NMR spectra were recorded at a spinning rate of 5 kHz, and the reference chemical shift was tetramethylsilane (TMS). The Si/Al ratio of the samples were calculated from 29 Si MAS NMR spectra using Eq. ( 1 )[ 30 , 31 ]: $$\:\frac{\text{S}\text{i}}{\text{A}\text{l}}=\frac{\sum\:_{n=0}^{4}{I}_{\text{S}\text{i}\left(n\text{A}\text{l}\right)}}{\sum\:_{n=0}^{4}0.25n{I}_{\text{s}\text{i}\left(n\text{A}\text{l}\right)}}$$ 1 where n is the number of Al neighbors, \(\:{I}_{\text{s}\text{i}\left(\text{n}\text{A}\text{l}\right)}\) is the intensity of peak n . 2.5 Catalytic test The NH 3 -SCR reaction was performed in a fixed-bed quartz reactor. The catalysts with particle size of 40–60 mesh were placed in the tube reactor. The total flow rate was held at 200 mL·min − 1 , with gas composition of 0.05%NO, 10% O 2 , 0.05%NH 3 and Ar as balance gas. 0.1 g zeolite samples were used for the tests, with gas hourly space velocity of 80000 h − 1 . A Fourier transform infrared spectrometer (Bruker) was chosen to detect the concentration of NO, N 2 O and NH 3 . To investigate the hydrothermal stability, the samples were hydrothermally treated at 750°C for 16 h in flowing air containing 10% H 2 O. 3. Results and discussion 3.1 SSZ-13 zeolite synthesis using various combinations of silica/alumina sources (A) HSZ + Al, (B) CZTZ, (C) LSZ + Si Figure 1 shows the hydrothermal conversion process of three synthesis strategies monitored by XRD. All XRD patterns were measured after 1.5 ~ 48 h hydrothermal crystallization. Apparently, with the extension of crystallization time, typical diffraction peaks of starting MFI gradually decrease, while the diffraction peaks of target CHA structure increase. The diffraction peaks corresponding to MFI zeolite disappeared completely after hydrothermal treatment for 3.5 h (HSZ + Al, Fig. 1 a), 4.5 h (CZTZ, Fig. 1 b) and 3 h (LSZ + Si, Fig. 1 c), respectively. After 2.5,3, or 1.5 h of hydrothermal treatment, the diffraction peaks corresponding to CHA zeolite were initially observed in HSZ + Al, CZTZ and LSZ + Si samples, respectively, implying that the nucleation of CHA zeolite occurred during the first 3 h of treatment. The highly crystalline CHA zeolites with no impurity were obtained only after 4.5, 6, or 4.5 h, indicating rapid transformation of ZSM-5 regardless of their initial SARs. Further extending the crystallization time to 48 h, there are no significant changes in the relative crystallinity of all obtained samples from three strategies. It was also noted that trace competitive phases MOR appear in CZTZ samples when crystallized less than 6 h, while quartz phases appear in HSZ + Al and LSZ + Si samples after long-time crystallization for 24 ~ 48 h. different starting materials at various crystallization time Combined with the corresponding crystallization curves and solid yields(Fig. 2 ), it can also be seen that the crystallization rates of HSZ + Al and LSZ + Si synthesis systems are faster than that of CZTZ system. Further extending the crystallization time to 48 h, the relative crystallinities of samples are still maintained above 90%, which suggest full crystallization of SSZ-13. Additionally, the solid yields of the obtained samples increase with the crystallization time at early stage, and then stabilizes at ~ 85% for HSZ + Al, ~ 71% for CZTZ and ~ 65% for LSZ + Si, respectively(inset of Fig. 2 ). To sum up, SSZ-13 zeolites can be synthesized rapidly by interzeolite transformation of ZSM-5 with various SARs through three experimental schemes, and additional Al- or Si- source accelerated dissolution of starting ZSM-5 and crystallization of target SSZ-13 zeolite. (A) HSZ + Al, (B) CZTZ, (C) LSZ + Si Furthermore, the framework/ring vibrations in zeolites samples obtained from three experimental schemes at the different transformation stages were monitored by FT-IR measurements (Fig. 3 ), in order to offer an insight into the evolution of the short-range order in solid samples during the MFI-CHA transformation process. In the starting ZSM-5 zeolites, the adsorption bands at 800 and 450 cm − 1 were assigned to the symmetric stretching and bending vibration mode of T–O–T in the framework structure, respectively[ 32 – 34 ], and the peaks at 550 and 626 cm − 1 were ascribed to the vibration of isolated and condensed five-membered rings, respectively [ 35 , 36 ]. As for the samples obtained at various crystallization time, the bands centered at 420 and 460 cm -1 are related to T-O bending vibration of CHA zeolites[ 37 ], the peaks at 796 cm -1 were assigned to the T-O-T symmetric stretching vibration in CHA cages[ 38 , 39 ]. Additionally, the vibrational peaks at 639 and 537 cm -1 were ascribed to the double six-member rings(D6Rs) and single six-member rings(S6Rs) in the SSZ-13 framework[ 39 ]. As the crystallization process proceeds, the peaks at 550 and 626 cm − 1 weakened gradually and finally disappeared at 3.5 h (HSZ + Al), 4.5 h(CZTZ), and 3 h (LSZ + Si), respectively, indicating the disintegration of 5Rs in the ZSM-5 framework. Meanwhile, the bands at 800 and 450 cm -1 gradually shifted to 796 and 460 cm -1 , respectively, and the peaks at 420, 537, 639 and 676 cm -1 of CHA gradually appeared and increased with time until SSZ-13 fully crystallize at 4.5 h(HSZ + Al), 6 h(CZTZ) and 4.5 h (LSZ + Si), respectively. Subsequently, there was almost no significant change over time. This is consistent with the aforementioned XRD results. Therefore, it seems that the MFI-CHA transformation is triggered by disintegration of S5Rs in MFI and simultaneous generation of S4Rs and S6Rs, which were further rearranged into D6Rs and CHA cages(composite building units of CHA zeolites) and then serve as a kinetic mediator for nucleating the CHA structure[ 40 ]. To comprehend the evolution of parent ZSM-5 zeolites with and without combination of Si- or Al- source during the rapid transformation, morphological changes of obtained samples during the crystallization process were analyzed. Figure 4 displays the SEM images of the samples obtained from three experimental schemes at various crystallization time. For HSZ + Al system, it was observed that the high silica ZSM-5 (SAR = 120) crystals exhibited the aggregates of ellipsoidal particles with the size of 200 ~ 400 nm (Fig. 4A1). After crystallization for 1.5 h, some ZSM-5 crystals showed obvious fracture and damage (Fig. 4A2), while at this time the SSZ-13 crystals could not be found. When the crystallization time was 2.5 h, a large amount of ZSM-5 zeolites were dispersed and depolymerized into fragments, accompanied by appearance of SSZ-13 cubic crystals with a size of 300 ~ 500 nm (indicated by red arrows in Fig. 4A3). After 4.5 h of crystallization, SSZ-13 cubic crystals grew to 700 nm and showed layered cubic morphology, while ZSM-5 zeolite and other amorphous substances completely disappeared (Fig. 4A4). When the crystallization time was further extended to 48 h, the layered cubic morphology (~ 700 nm) of the sample did not change significantly, but some quartz phase impurities could be observed (indicated by yellow arrows in Fig. 4A5). Regarding the CZTZ system, the parent ZSM-5(SAR = 38) displayed typical hexagonal prismatic morphology with a size of about 3 ~ 4 µm (Fig. 4B1). After crystallization for 1.5 h, it was seen that ZSM-5 crystals were cracked and damaged obviously under the action of alkaline solution, and the surface also became rough (Fig. 4B2). When the crystallization time is 3 h (Fig. 4B3), numerous SSZ-13 cubic crystals about 400 nm appeared at the crack and defect site on the surface of ZSM-5, suggesting that nucleation could occur on the available MFI surface. When the crystallization time is 6 h, ZSM-5 zeolites were completely transformed into SSZ-13 cubic crystals with a size of 600 ~ 900 nm (Fig. 4B4). Notably, in addition to well-developed cubic crystals, some complex intergrowths and interpolations between two or more cubic crystals were also observed. This may be related to the fact that dissolved MFI fragments are not easily assembled into crystals with perfect morphologies. Extending the crystallization time to 48 h, the sizes of the SSZ-13 zeolites were slightly increased to 700 ~ 1000 nm (Fig. 4B5). In the case of LSZ + Si system, the parent ZSM-5(SAR = 24) also exhibits typical hexagonal prismatic crystals with a size of 3 ~ 4 µm (Fig. 4C1). After crystallization for 1.5 h (Fig. 4C2), SSZ-13 cubic crystals with a size of approximately 200 nm have appeared on the surface of ZSM-5, corresponding to the weak XRD signal of CHA (Fig. 1 b). When the crystallization time was extended to 2.5 h, the majority of ZSM-5 zeolites have been transformed into cubic SSZ-13 crystals with a size of 100 ~ 300 nm, and only a small quantity of residual ZSM-5 fragments remained (indicated by red arrows in Fig. 4C3). It is noteworthy that the starting ZSM-5 zeolites have a similar size compared to CZTZ scheme, while the starting ZSM-5 with lower SAR in LSZ + Si system dissolved more rapidly in the alkaline solution. After 4.5 h of crystallization, the complete transformation of MFI-CHA was already achieved, and the average size of SSZ-13 cubic crystals increased to ~ 400 nm (Fig. 4C4). When the crystallization time is further extended to 48 h, the cube morphology of some crystals became less regular, and accompanied by a small amount of quartz phase impurities (indicated by yellow arrows in Fig. 4C5). Based on the above results, it is inferred that the additional Al- or Si- source have a significant effect on the properties of the synthesis gel and thus on the crystallization kinetics. Figure 5 shows the TG-DTG curves of the samples obtained from three experimental schemes. It was seen that all TG curves of fully crystallized samples exhibited three weight loss steps. The first stage between room temperature and 300°C is attributed to physically adsorbed water inside zeolites. The second weight loss occurring at 300 ~ 500°C was assigned to the combustion of TMAdaOH, indicating that TMAdaOH was incorporated into the SSZ-13 structure. The third stage of weight loss occurs above 500°C, which is related to the removal of organic remnants. The amount of weight loss of fully crystallized samples in 300 ~ 700°C range is about 21 ~ 22 wt%, indicating that a large amount of TMAdaOH were occluded in the product zeolite. Additionally, it was noted that an additional weak peak near 350°C appeared in the DTG curves of samples obtained from three synthetic systems at the initial crystallization stage (before 2.5 h, 3 h and 1.5 h, respectively) (Fig. 5 ), at which time ZSM-5 was not completely transformation. Considering that no organic template should remain on the outer surface of the sample after repeated washing, suggesting that TMAdaOH may be infiltrated or inserted into the micro-cracks of ZSM-5 crystals caused by the initial dissolution. This may promote the rapid disintegration of parent ZSM-5 zeolite. 3.2 Mechanism of the interzeolite conversion from MFI to CHA According to the above results, it is apparent that highly crystalline SSZ-13 with submicron dimensions can be synthesized rapidly within 6 h at 160°C via interzeolite transformation from ZSM-5 zeolites with various SAR (24 ~ 120), although the MFI-CHA transformation is unfavorable from both thermodynamic (adverse FD gradient) and kinetic (no common D6Rs CBU) perspectives. There are two aspects possible reasons for the successful and rapid transformation of MFI to CHA. On the one hand, combined with aforementioned SEM observation (Fig. 4 ) that the initially formed SSZ-13 cubic crystals grew at the crack or defect site on the surface of remnant ZSM-5, and the phenomenon that TMAdaOH presented in incompletely dissolved ZSM-5 at the initial stage (Fig. 5 ). It was suggested that TMAdaOH may first be inserted into the micro-cracks or small defects of ZSM-5 crystals formed by the degradation in the early stage of hydrothermal transformation. This may have acted as a wedge, thus promoted the disintegration of the parent ZSM-5 zeolite. On the other hand, with the rapid degradation of starting ZSM-5, the S5Rs predominating in the MFI framework were disassembled, while rapidly producing S4Rs and S6Rs building units, which facilitate the assembly of D6Rs and CHA cages. These CBUs act as a kinetic mediator to promote the rapid crystallization of product SSZ-13 zeolite. In addition, compared with CZTZ synthesis system, the crystallization rates of SSZ-13 synthesized by HSZ + Al and LSZ + Si system were faster, and the pure SSZ-13 with high crystallinity and small size can be obtained in only 4.5 h at 160°C. This is mainly due to the fact that the SBUs produced by the early dissolution of MFI combines with additional Al- or Si- source to rapidly form a larger amount of crystal nuclei under the assistance of the TMAdaOH and seed. Simultaneously, with the rapid consumption of these structural units, the dissolution of the starting ZSM-5 zeolite will be further accelerated. Meanwhile, the rapid formation of a large number of crystal nuclei also leads to smaller SSZ-13 product crystals, which are in good agreement with SEM observation (Fig. 4 ). Based on the above analysis, the interzeolite transformation process of MFI-CHA from three strategies was proposed and illustrated in Fig. 6 . 3.3 Physicochemical properties Further, three fully crystallized SSZ-13 samples prepared from various experimental schemes, HSZ-4.5 h, ESZ-6.0 h and LSZ-4.5 h were selected to conduct N 2 adsorption-desorption, NH 3 -TPD, 29 Si/ 27 Al-MAS NMR and H 2 -TPR measurement for a detail investigation of their texture properties, acidity properties, chemical states of Si- and Al- species, and the status and dispersion of Cu species after Cu 2+ exchange, respectively. Figure 7 illustrates the N 2 adsorption-desorption isotherms of three SSZ-13 samples, which exhibit type-I isotherms characteristic of microporous solids along with a capillary condensation step above a relative pressure of 0.9 due to the intercrystal voids arising from the stacking of nanocrystals. Their textual properties and SARs are listed in Table 2 . Clearly, the specific surface area and the total pore volume of the three SSZ-13 samples are all above 700 m 2 ·g − 1 and 0.29 cm 3 ·g − 1 , respectively, which further verify the high crystallinity of these samples and successful interzeolite conversion. Among them, the SSZ-13 synthesized by LSZ + Si strategy has the largest specific surface area (800 m 2 ·g − 1 ), the total pore volume (0.36 cm 3 ·g − 1 ) and mesopore volume (0.05 cm 3 ·g − 1 ), which should be related to the smaller size of the resultant sample due to the promoting effect of additional Si source on the conversion of parent MFI zeolite. Besides, the SARs of three SSZ-13 samples measured by ICP are 25.8, 29.5 and 35.1, respectively. The difference in SARs of SSZ-13 samples may be due to the various disintegration rate and degree caused by the different SARs and particle sizes of parent zeolites at the initial stage, as well as the different reactivity of the additional Si- or Al- source. Among them, the SAR of LSZ-4.5 h sample was the highest, which may be related to that the Al source was entirely from ZSM-5 with low SAR, and there were fewer Al species and more silicon species available in the nucleation stage. Table 2 Textural properties and compositions(SAR) of HSZ-4.5 h, CZTZ-6.0 h and LSZ-4.5 h samples Samples S BET (m 2 ·g − 1 ) S micro (m 2 ·g − 1) S ext (m 2 ·g − 1 ) V tot (cm 3 ·g − 1 ) V micro (cm 3 ·g − 1 ) V meso (cm 3 ·g − 1 ) SAR a SAR b HSZ-4.5 h 737 711 26 0.30 0.28 0.02 25.8 26.4 CZTZ-6.0 h 707 679 18 0.29 0.27 0.02 29.5 27.3 LSZ-4.5 h 800 779 21 0.36 0.31 0.05 35.1 37.4 a SiO 2 /Al 2 O 3 ratio, determined by ICP. b SiO 2 /Al 2 O 3 ratio, determined by 29 Si MAS NMR spectra. The chemical states of the aluminum and silicon in the obtained HSZ-4.5 h, CZTZ-6 h, LSZ-4.5 h samples were investigated by 27 Al and 29 Si MAS NMR, as illustrated in Fig. 8 A and B, respectively. According to Fig. 8 A, only the resonances around 58 ppm assigned to tetrahedrally coordinated framework Al species were observed for all three samples[ 41 , 42 ], while a resonance corresponding to that of octahedrally coordinated Al species, namely an extra-framework aluminum species, was not detected around 0 ppm. This means that all Al species are well incorporated into the zeolitic frameworks of three samples. Moreover, a faint signal appearing around − 20 ppm is due to a spinning-side band[ 43 ]. In addition, the 29 Si MAS NMR spectra of all three samples showed three similar resonance peaks (Fig. 8 B). The resonances at -108 ~ -111, -103 ~ -106 and − 98 ~ -101 ppm are attributed to Si(4Si, 0Al), Si(3Si,1Al)、 Si(2Si, 2Al) or Si(3Si, OH) structures, respectively[ 44 , 45 ]. The peak area percentages of these resonances are obtained from the deconvolution of the 29 Si MAS NMR spectra was shown in Fig. 8 C. It was found that although they all contain three similar resonances at almost the same chemical shift, there are some differences in the relative proportion of each peak area in total peak area, indicating the slightly different distribution of Si and Al of three samples. Moreover, when the resonance at -98 ~ -101 ppm was assigned to Si(3Si, OH) atom arising from the defect groups [ 44 ], the framework SiO 2 /Al 2 O 3 ratios of the three samples calculated based on the areas of these resonances using Eq. 1 are in good agreement with the data from ICP analysis (Table 2 ). The acidity of three samples are measured by temperature-programmed desorption of ammonia (NH 3 -TPD) technique. The NH 3 -TPD profiles and corresponding acidity data are shown in Fig. 9 and Table S2, respectively. Obviously, there are two well resolved peaks in the desorption temperature range of all three samples. The low-temperature desorption peaks at 173 ~ 179°C correspond to desorption of NH 3 from weak Lewis acid sites, while the high temperature desorption peaks located at 456 ~ 470°C are assigned to strong Brønsted acid sites[ 36 ]. Among them, the CZTZ-6 h sample possesses the largest total acid and strong acid amount, while those of the LSZ-4.5 h sample with the highest SAR were the lowest. In addition, compared to HSZ-4.5 h, the high temperature NH 3 -desorption peaks of CZTZ-6 h and LSZ-4.5 h slightly shift to high and low temperature, respectively. This is indicative of the higher acid strength of CZTZ-6 h and the lower one of LSZ-4.5 h[ 46 ]. H 2 -TPR measurements were carried out to determine the distribution of Cu species in these samples, and the results are shown in Fig. S1 . It illustrates that the reduction peaks below 500°C can be attributed to different types of Cu species(Fig. S1 A), where the peaks at ~ 215 and 340°C are ascribed to the reduction of Cu 2+ to Cu + in the 8MRs (Cu(OH) + -Z species balanced by one framework charge) and in D6Rs (Cu 2+ -2Z species balanced by two framework charges), respectively. For the NH 3 -SCR reaction, it is demonstrated that these two copper species in Cu-CHA are the active sites[ 47 , 48 ]. Moreover, the peak at ~ 470°C is assigned to the reduction of Cu + ions to Cu 0 , and this peak is strongest in HSZ-4.5 h sample. It is thought that this kind of Cu + ion is also coming from D6Rs unit[ 49 ].Additionally, broad peaks at temperatures above 550°C are associated with the reduction of highly stable Cu + to Cu 0 [ 50 – 52 ]. The different relative proportions(Fig. S1 B) and reduction temperatures of various copper species in the three samples indicate that the synthesis strategies have a certain effect on the copper distribution and reduction of the samples. 3.4 Catalytic performances of samples The catalytic performances of three Cu-SSZ-13 samples in NH 3 -SCR reaction before and after hydrothermal aging treatments were evaluated, and the results are given in Fig. 10 . All fresh samples exhibit high NO conversions (above 90%) over a wide temperature range of 190 ~ 490°C for HSZ-4.5 h, 200 ~ 500°C for CZTZ-6 h, and 210 ~ 510°C for LSZ-4.5 h, respectively, evidencing the superior catalytic activity of three SSZ-13 samples synthesized by three synthesis schemes. Additionally, it was found that the low temperature ( CZTZ-6 h > LSZ-4.5 h. The best low temperature activity of HSZ-4.5 h in NH 3 -SCR performance may be related to more amount of Cu + as revealed by the H 2 -TPR result(Fig. S1 ). This is due to that, in addition to Cu 2+ active species, Cu + sites solvated by NH 3 have also been proposed as SCR active sites below 200°C[ 53 ], which is conducive to the reaction between adsorbed NH 3 substances and NO molecules at low temperatures. Given that the high-temperature hydrothermal stability of Cu-SSZ-13 is vital for its practical application, the NH 3 -SCR catalytic properties of hydrothermally aged Cu-SSZ-13 samples are also investigated. For Cu-CZTZ-6 h and Cu-LSZ-4.5 h samples, the NO conversions still remain higher than 90% in the range of 200 ~ 480°C after hydrothermal treatment at 750°C for 16 h, suggesting their excellent hydrothermal stability. While for Cu-HSZ-4.5 h sample, the NO x conversion decreased significantly, but also remained above 80% in the wide range of 240 ~ 600°C after the same treatment. The relatively inferior hydrothermal stability of Cu-HSZ-4.5 h may be related to its relatively low SAR, less Cu 2+ -2Z active site, and NH 3 desolvation from Cu + -complexes at higher temperature[ 53 ]. 4. Conclusions In summary, the synthesis of SSZ-13 with ZSM-5 as the starting zeolite was investigated by three transformation strategies, namely HSZ + Al, CZTZ and LSZ + Si. Based on these three strategies, highly crystalline SSZ-13 zeolites with submicron sizes were successfully prepared within 6 h at 160°C. Besides, it is revealed that HSZ + Al and LSZ + Si schemes exhibit faster crystallization rates and distinct crystal size compared with CZTZ, suggesting that additional Al- or Si- source can not only regulate the SAR of initial gel, but also modify the kinetics of nucleation and crystallization during the MFI-CHA transformation process. In addition, a plausible mechanism for the highly efficient transformation from MFI to CHA was discussed. Under the action of alkaline solution and promotion of TMAdaOH, 5Rs in ZSM-5 framework was rapidly deconstructed and converted into S4Rs and S6Rs, which is rapidly assembled into D6Rs and CHA cages, thus further forming CHA framework. Significantly, the properties of the locally ordered aluminosilicate species formed in the gel are associated with the starting material and ultimately play a role in the kinetic nucleation and crystallization process. The resultant HSZ-4.5 h, CZTZ-6 h and LSZ-4.5 h samples, after Cu 2+ exchange, show good catalytic activity (the NO conversion remained over 90% at a temperature window of 200 ~ 500°C) and hydrothermal stability. Declarations CRediT authorship contribution statement Yufeng Liu: Investigation, Validation, Writing - original draft. Yuping Li: Conceptualization, Methodology, Validation, Writing - review & editing. Ze Chen: Investigation, Validation, Writing - original draft. Fuchao Ji : Data curation，Formal analysis. Lina Han: Resources, Funding acquisition. Xiaohong Liang: Writing – review & editing. Peide Han: Supervision. Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. Author Contribution Y L: Investigation, Validation, Writing - original draft. Y L Conceptualization, Methodology, Validation, Writing - review & editing. Z C: Investigation, Validation, Writing - original draft. F J: Data curation Formal analysis. L H: Resources, Funding acquisition. X L: Writing – review & editing. P H: Supervision. Acknowledgements This work was supported by the National Natural Science Foundation of China (No.21978195) and Central Guided Local Science and Technology Development Fund Project(No. YDZJSX20231A012) Data availability Data will be made available on request. References S. Mintova, M. Jaber, V. 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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-5263931","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":367185300,"identity":"7fe4aab5-0590-482a-ab7c-beea93dcc28b","order_by":0,"name":"Yufeng Liu","email":"","orcid":"","institution":"Taiyuan University of Technology","correspondingAuthor":false,"prefix":"","firstName":"Yufeng","middleName":"","lastName":"Liu","suffix":""},{"id":367185304,"identity":"af9aeece-98fb-4a63-bbad-a0a93dedf893","order_by":1,"name":"Yuping Li","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA00lEQVRIiWNgGAWjYBACPmYQacDAwA8VYGwgpIUNpkWyDUgfIEoLjGFwjGgt7Dxm0gUFd+w23+8xk/7AYCO74QDzswf4HQbUMsPgWfK2YzxmEgcY0ow3HGAzNyCohcfgcLIZRMvhxA0HeNgkiNJi3AbW8p94LXYGbGAtB4jRwlZsPcPgcILEsbRiizMGycYzD7OZ4dXCz3944+2CP4ft+ZsPb7xRUWEn23e8+RleLQwMHAag2ExsADLAccrAjF89ELA/AKmxBzEIqh0Fo2AUjIKRCQDwekApQPny1QAAAABJRU5ErkJggg==","orcid":"","institution":"Taiyuan University of Technology","correspondingAuthor":true,"prefix":"","firstName":"Yuping","middleName":"","lastName":"Li","suffix":""},{"id":367185305,"identity":"cea521c6-c8b9-4ea7-9818-2d55f84868a1","order_by":2,"name":"Ze Chen","email":"","orcid":"","institution":"Taiyuan University of Technology","correspondingAuthor":false,"prefix":"","firstName":"Ze","middleName":"","lastName":"Chen","suffix":""},{"id":367185306,"identity":"3fa21700-f77d-4657-a819-abc2fed8ab48","order_by":3,"name":"Fuchao Ji","email":"","orcid":"","institution":"Taiyuan University of Technology","correspondingAuthor":false,"prefix":"","firstName":"Fuchao","middleName":"","lastName":"Ji","suffix":""},{"id":367185307,"identity":"18633502-3fc3-465e-93e7-aec90ceb5c10","order_by":4,"name":"Xiaohong Liang","email":"","orcid":"","institution":"Taiyuan University of Technology","correspondingAuthor":false,"prefix":"","firstName":"Xiaohong","middleName":"","lastName":"Liang","suffix":""},{"id":367185308,"identity":"915bf8bb-ef9d-4b66-aef0-d97b1650f584","order_by":5,"name":"Lina Han","email":"","orcid":"","institution":"Taiyuan University of Technology","correspondingAuthor":false,"prefix":"","firstName":"Lina","middleName":"","lastName":"Han","suffix":""},{"id":367185309,"identity":"f632a116-46a3-4015-97bf-4433d5b7be31","order_by":6,"name":"Peide Han","email":"","orcid":"","institution":"Taiyuan University of Technology","correspondingAuthor":false,"prefix":"","firstName":"Peide","middleName":"","lastName":"Han","suffix":""}],"badges":[],"createdAt":"2024-10-14 23:53:05","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-5263931/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-5263931/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1007/s10934-024-01730-5","type":"published","date":"2024-12-17T15:58:38+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":67147563,"identity":"b43c0c0c-f159-4175-ac8f-4162c80985d9","added_by":"auto","created_at":"2024-10-21 15:51:58","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":54552,"visible":true,"origin":"","legend":"\u003cp\u003eXRD patterns of samples prepared at various crystallization time.\u003c/p\u003e\n\u003cp\u003e(A) HSZ+Al, (B) CZTZ, (C) LSZ+Si\u003c/p\u003e","description":"","filename":"floatimage1.png","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/19eead402583f8fd5dd38437.png"},{"id":67146242,"identity":"9db6ac0f-4eda-4b4f-98f7-16f9158dc7f6","added_by":"auto","created_at":"2024-10-21 15:35:57","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":33452,"visible":true,"origin":"","legend":"\u003cp\u003eRelative crystallinity of SSZ-13 and solid yields(inset) obtained from different starting materials at various crystallization time\u003c/p\u003e","description":"","filename":"floatimage2.png","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/f6645fce9305923bab650c18.png"},{"id":67146244,"identity":"0f96abe9-d8dd-4ef5-b0f3-279cc1fa923f","added_by":"auto","created_at":"2024-10-21 15:35:58","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":67167,"visible":true,"origin":"","legend":"\u003cp\u003eFT-IR spectra of samples prepared at various crystallization time.\u003c/p\u003e\n\u003cp\u003e(A) HSZ+Al, (B) CZTZ, \u0026nbsp;(C) LSZ+Si\u003c/p\u003e","description":"","filename":"floatimage3.png","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/430937dbad1522cbada58da8.png"},{"id":67147260,"identity":"e3be20ea-299f-4e05-af37-5551a0d77897","added_by":"auto","created_at":"2024-10-21 15:43:58","extension":"jpeg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":138039,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of samples obtained by a different combination of a starting ZSM-5 zeolite and aluminum＆silica sources at various crystallization time.(A1 to A5) HSZ+Al: ZSM-5(SAR=120),1.5 h, 2.5 h, 4.5 h, 48 h; (B1 to B5) CZTZ: ZSM-5(SAR=38), 1.5 h, 3 h, 6 h, 48 h; (C1 to C5) LSZ+Si: ZSM-5 (SAR=24), 1.5 h, 2.5 h, 4.5 h, 48 h.\u003c/p\u003e","description":"","filename":"floatimage4.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/8906ea642e390b296a48ef10.jpeg"},{"id":67146243,"identity":"e56c966d-09bd-402c-8074-f4e3f47c0952","added_by":"auto","created_at":"2024-10-21 15:35:58","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":49762,"visible":true,"origin":"","legend":"\u003cp\u003eTGA (solid lines) and corresponding DTG profiles (dotted lines) of SSZ-13 samples obtained at various crystallization time. (A)HSZ+Al, (B)CZTZ, (C)LSZ+Si\u003c/p\u003e","description":"","filename":"floatimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/24aa23cfeb43a77fb122a347.png"},{"id":67146251,"identity":"cf1a425d-ec79-4186-9ee3-410a73d36d45","added_by":"auto","created_at":"2024-10-21 15:35:58","extension":"jpeg","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":112929,"visible":true,"origin":"","legend":"\u003cp\u003eSchematic diagram of proposed process for the synthesis of SSZ-13 via interzeolite transformation from a starting ZSM-5 withvarious SARs by a combination of Al- or Si- source.\u003c/p\u003e","description":"","filename":"floatimage6.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/734e1c843c0c0eea05d261bb.jpeg"},{"id":67147257,"identity":"fdb0408a-6f7c-45ac-9727-8380445c3865","added_by":"auto","created_at":"2024-10-21 15:43:58","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":19175,"visible":true,"origin":"","legend":"\u003cp\u003eN\u003csub\u003e2\u003c/sub\u003e adsorption-desorption isotherms of HSZ-4.5 h, CZTZ-6.0 h and LSZ-4.5 h samples.\u003c/p\u003e","description":"","filename":"floatimage7.png","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/52f63f52d94e8dc624526232.png"},{"id":67147564,"identity":"840194f3-727b-4a31-b6a5-039c48826074","added_by":"auto","created_at":"2024-10-21 15:51:58","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":45617,"visible":true,"origin":"","legend":"\u003cp\u003e\u003csup\u003e27\u003c/sup\u003eAl(A) and\u003csup\u003e 29\u003c/sup\u003eSi(B) MAS NMR spectra of samples and spectra fitting results(C) of \u003csup\u003e29\u003c/sup\u003eSi MAS NMR.\u003c/p\u003e","description":"","filename":"floatimage8.png","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/cb0f6c6fb0eb7fd00cbdf1c9.png"},{"id":67146246,"identity":"964bbcb5-aa99-4d88-84e2-d67a1dcb5f23","added_by":"auto","created_at":"2024-10-21 15:35:58","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":17643,"visible":true,"origin":"","legend":"\u003cp\u003eNH\u003csub\u003e3\u003c/sub\u003e-TPD profiles of SSZ-13 samples obtained under three various conditions.\u003c/p\u003e","description":"","filename":"floatimage9.png","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/6dfdf6b1b438380f6219aaeb.png"},{"id":67146249,"identity":"58bef38a-82a1-4f29-8246-2b987580a6d1","added_by":"auto","created_at":"2024-10-21 15:35:58","extension":"png","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":27295,"visible":true,"origin":"","legend":"\u003cp\u003eNO conversion as a function of temperature over Cu-HSZ-4.5 h, Cu-CZTZ-6 h and Cu-LSZ-4.5 h samples before (solid line) and after (dotted line) hydrothermal aging.\u003c/p\u003e","description":"","filename":"floatimage10.png","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/69abeec630997f32fda442bc.png"},{"id":72202730,"identity":"5f6c995b-78e5-44e2-b3b6-c0373a97d7ff","added_by":"auto","created_at":"2024-12-23 16:15:46","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1324113,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/d376e32a-72bb-4230-a9cf-980e5f92a941.pdf"},{"id":67147261,"identity":"4ebef86e-d6d7-423d-ae8e-8e0725741de1","added_by":"auto","created_at":"2024-10-21 15:43:58","extension":"docx","order_by":2,"title":"","display":"","copyAsset":false,"role":"supplement","size":306901,"visible":true,"origin":"","legend":"","description":"","filename":"SupportingInformation20240929.docx","url":"https://assets-eu.researchsquare.com/files/rs-5263931/v1/80786d813e31715dc5c2efb7.docx"}],"financialInterests":"No competing interests reported.","formattedTitle":"Synthesis of CHA from MFI by three interzeolite transformation strategies and its Application in NH 3 -SCR reaction","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eZeolites, a family of crystalline microporous aluminosilicate materials, have been widely applied in catalyst, adsorption, and ion-exchange applications[\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. This variety of applications is due to their uniform pore structure, high specific surface area, suitable acidity, special shape selectivity, and brilliant thermal/hydrothermal stability[\u003cspan additionalcitationids=\"CR4\" citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]. Among them, SSZ-13, a typical CHA zeolite, is composed of 4 and 6 membered rings organized in double six-membered rings (D6Rs) composite building units (CBUs) and large ellipsoidal CHA cages (6.7*10\u0026Aring;) with pore openings of 3.8*3.8 \u0026Aring;. This unique pore system confers it excellent properties in catalysis such as NO\u003cem\u003ex\u003c/em\u003e abatement, methanol-to-olefins (MTO) and ethylene-to-propylene (ETP) reaction[\u003cspan additionalcitationids=\"CR7 CR8\" citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eGenerally, zeolites are synthesized under conventional hydrothermal conditions, which taking amorphous aluminosilicate gel as raw materials[\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e, \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e]. Over the last decade, the strategy called interzeolite conversion(IZC) has attracted considerable attention for zeolite synthesis, which uses easily available or inexpensive crystallized zeolites as silica/alumina or alumina source to synthesize the target zeolite. Compared with conventional hydrothermal synthesis, the IZC method achieves various specific merits, such as rapid crystallization[\u003cspan additionalcitationids=\"CR13\" citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e], high solid yield[\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e, \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e], specific Al distribution[\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e], unusual framework composition[\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e], and small crystal size[\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e, \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e]. It is widely accepted that the successful interzeolite transformation is preferably achieved from those parent zeolites containing common composite building units(CBUs), with less dense framework density(FD), and larger pore size. Up to now, a variety of zeolites has been used as parent zeolite to synthesize SSZ-13 by IZC method, including LEV[\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e], MFI[\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e], BEA[\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e], GIS[\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e], LTL[\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e, \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e], FAU[\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e], LTA[\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e], and FER[\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. Among them, FAU, LEV and LTL zeolite could be efficiently converted into SSZ-13, which were attributed to that the starting zeolite contains the common CBUs with the target zeolite, namely D6Rs. However, the other 5 zeolites listed(GIS(8-membered rings(8MRs) pore, FD\u0026thinsp;=\u0026thinsp;16.4 T/1000 \u0026Aring;\u003csup\u003e3\u003c/sup\u003e), BEA(12MRs pore, FD\u0026thinsp;=\u0026thinsp;15.3 T/1000 \u0026Aring;\u003csup\u003e3\u003c/sup\u003e), MFI(10MRs pore, FD\u0026thinsp;=\u0026thinsp;18.4 T/1000 \u0026Aring;\u003csup\u003e3\u003c/sup\u003e), FER(10MRs pore, FD\u0026thinsp;=\u0026thinsp;17.6 T/1000 \u0026Aring;\u003csup\u003e3\u003c/sup\u003e), and LTA(8MRs pore, FD\u0026thinsp;=\u0026thinsp;14.2T/1000 \u0026Aring;\u003csup\u003e3\u003c/sup\u003e), with no common CBUs (D6Rs) with CHA(8MRs pore, FD\u0026thinsp;=\u0026thinsp;15.1 T/1000 \u0026Aring;\u003csup\u003e3\u003c/sup\u003e), can also be successfully converted to SSZ-13. Additionally, compared to the CHA zeolite, these starting zeolites had higher FD except for LTA, verifies that framework density (FD) actually had only a weak effect on successful IZC. As for the effect of pore size, these starting zeolites have larger (FAU, LTL, BEA, LTA, MFI and FER) or smaller (LEV and GIS) pore sizes than that of CHA structure. Therefore, the interzeolite transformation mechanism is not yet fully elucidated, especially when the transformation occurs between two zeolites without similar structure features.\u003c/p\u003e \u003cp\u003eZSM-5 zeolite (10MRs pore, FD\u0026thinsp;=\u0026thinsp;18.4 T/1000 \u0026Aring;\u003csup\u003e3\u003c/sup\u003e) with MFI topology, which does not contain D6Rs units but a mass of single five-membered rings (S5Rs), as well as a small amount of single four-membered rings (S4Rs) and six-membered rings (S6Rs). For MFI-CHA transformation, it is unfavorable from the perspective of both thermodynamics (higher FD of starting zeolite than that of target one) and dynamics (without common D6R CBUs). At present, there are only a few reports on the successful transformation from ZSM-5 to SSZ-13[\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e, \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. Moreover, in these existing reported synthesis of SSZ-13 from ZSM-5, ZSM-5 is usually used as sole Si-/Al- source[\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e] or as an Al-source combined with additional silica sources[\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. As we know, the successful complete transformation of the starting zeolite is highly dependent on its SAR. Moreover, the addition of extra Si- or Al- source can not only broaden the SAR range of the initial zeolite required for the synthesis of the product zeolite, but also modulate the crystallization process, the morphology and size, and the distribution of the Al atom of the product zeolite.\u003c/p\u003e \u003cp\u003eHerein, we adopt a new interzeolite conversion strategy based on a combination of a high-silica ZSM-5 and an additional Al- source (denoted as HSZ\u0026thinsp;+\u0026thinsp;Al) to synthesize SSZ-13 zeolite. Meanwhile, for comparation, the other ZSM-5 with medium and low SARs were also selected to prepare SSZ-13 by the methods of completely zeolite to zeolite (CZTZ) and low-silica ZSM-5 with a combination of additional Si-source (LSZ\u0026thinsp;+\u0026thinsp;Si), respectively. The crystallization processes of the CHA zeolite from HSZ\u0026thinsp;+\u0026thinsp;Al, CZTZ and LSZ\u0026thinsp;+\u0026thinsp;Si methods were monitored and analyzed by various characterization techniques. Finally, the catalytic performances of the CHA zeolites synthesized from these three experimental strategies after copper ion exchange in NH\u003csub\u003e3\u003c/sub\u003e-SCR reaction of NO\u003cem\u003ex\u003c/em\u003e were investigated.\u003c/p\u003e"},{"header":"2. Experimental","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1 Materials\u003c/h2\u003e \u003cp\u003eThe reagents used in this study are as follows: sodium hydroxide(NaOH, AR, 96 wt%) were purchased from Tianjin Kemiou Chemical Reagent Co., Ltd, ammonium chloride (NH\u003csub\u003e4\u003c/sub\u003eCl, AR, 99.5 wt%) and aluminium sulfate octadecahydrate (Al\u003csub\u003e2\u003c/sub\u003e(SO\u003csub\u003e4\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e\u0026middot;18H\u003csub\u003e2\u003c/sub\u003eO, AR, 99 wt%) were purchased from Tianjin wind boat chemical reagent technology Co., Ltd. N, N, N-trimethyladamantammonium hydroxide (25 wt% TMAdaOH in water) were provided by Dayou chemical co., LTD. Guangzhou. Fumed silica (92 wt% SiO\u003csub\u003e2\u003c/sub\u003e) were obtained from Qingdao Ocean Chemical Factory Co. ZSM-5 zeolites (SAR\u0026thinsp;=\u0026thinsp;24,38 and 120) were either obtained from commercial suppliers (Nankai University Catalyst Co Ltd) or prepared in-house. Copper nitrate trihydrate (Cu(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e2\u003c/sub\u003e\u0026middot;3H\u003csub\u003e2\u003c/sub\u003eO, AR 99 wt%) were provided by Shanghai McLean Biochemical Technology Co., Ltd. All chemicals were used without further purification.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2 Preparation of SSZ-13 zeolite from ZSM-5\u003c/h2\u003e \u003cp\u003eExperiments of the synthesis of SSZ-13 zeolites were carried out by three experimental schemes, namely using a combination of ZSM-5 with high SAR and aluminium sulfate octadecahydrate as Si- and Al- sources (HSZ\u0026thinsp;+\u0026thinsp;Al), using ZSM-5 with medium SAR as the sole source of Si and Al (complete zeolite to zeolite transformation) and using a combination of low silica ZSM-5 and fumed silica as Al- and Si-sources(LSZ\u0026thinsp;+\u0026thinsp;Si), respectively(Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). It needs to be mentioned that the SSZ-13 zeolites were all synthesized with an initial molar composition of 1SiO\u003csub\u003e2\u003c/sub\u003e : 0.0263Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e : 0.1Na\u003csub\u003e2\u003c/sub\u003eO : 0.2TMAdaOH : 15H\u003csub\u003e2\u003c/sub\u003eO.\u003c/p\u003e \u003cp\u003e(1) HSZ\u0026thinsp;+\u0026thinsp;Al approach\u003c/p\u003e \u003cp\u003eIn a typical synthesis, aluminium sulfate octadecahydrate,NaOH, TMAdaOH and deionized water was mixed to form a clear solution. Then, ZSM-5 (SAR\u0026thinsp;=\u0026thinsp;120) zeolite was added in the above mixture under stirring for 1 h.\u003c/p\u003e \u003cp\u003e(2) CZTZ approach\u003c/p\u003e \u003cp\u003eIn a typical synthesis, NaOH, TMAdaOH and deionized water was mixed to form a clear solution. Then ZSM-5(SAR\u0026thinsp;=\u0026thinsp;38) zeolite was added in the above mixture under stirring for 1 h.\u003c/p\u003e \u003cp\u003e(3) LSZ\u0026thinsp;+\u0026thinsp;Si approach\u003c/p\u003e \u003cp\u003eIn a typical synthesis, NaOH, TMAdaOH and deionized water was mixed to form a clear solution. Then, fumed silica was slowly added in the above solution keeping with vigorous stirring for 1 h. With a further addition of ZSM-5(SAR\u0026thinsp;=\u0026thinsp;24) zeolite under stirring for 1 h.\u003c/p\u003e \u003cp\u003eSubsequently, in all cases, SSZ-13 (2 wt% of the silica) was added as a seed crystal and the mixture was stirred for 1 h. Finally, the resulting gel was transferred into stainless steel autoclave with a 100 mL Teflon liner. After crystallization at 160\u0026deg;C for 1.5\u0026thinsp;~\u0026thinsp;48 h, solid products were collected by centrifugation, washed thoroughly with distilled water until a near neutral pH was achieved, and then dried overnight at 80\u0026deg;C. The as-synthesized SSZ-13 sample was calcined to remove the OSDA at 550\u0026deg;C for 8 h and obtain the calcined SSZ-13 sample.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eStarting materials prepared using different combinations of silica༆alumina sources\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"4\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eStarting materials (abbreviation)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eSilica source\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eAlumina source\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eParent zeolites\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eHigh-silica ZSM-5\u0026thinsp;+\u0026thinsp;alumina (HSZ\u0026thinsp;+\u0026thinsp;Al)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u0026mdash;\u0026mdash;\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eAl\u003csub\u003e2\u003c/sub\u003e(SO\u003csub\u003e4\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e\u003cb\u003e\u0026middot;\u003c/b\u003e18H\u003csub\u003e2\u003c/sub\u003eO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eZSM-5\u003c/p\u003e \u003cp\u003e(SiO\u003csub\u003e2\u003c/sub\u003e/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e\u0026thinsp;=\u0026thinsp;120)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eHigh-silica ZSM-5\u003c/p\u003e \u003cp\u003e(CZTZ)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u0026mdash;\u0026mdash;\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u0026mdash;\u0026mdash;\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eZSM-5\u003c/p\u003e \u003cp\u003e(SiO\u003csub\u003e2\u003c/sub\u003e/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e\u0026thinsp;=\u0026thinsp;38)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eLow-silica ZSM-5\u0026thinsp;+\u0026thinsp;silica\u003c/p\u003e \u003cp\u003e(LSZ\u0026thinsp;+\u0026thinsp;Si)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eFumed silica\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u0026mdash;\u0026mdash;\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eZSM-5 (SiO\u003csub\u003e2\u003c/sub\u003e/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e\u0026thinsp;=\u0026thinsp;24)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3 Preparation of Cu-SSZ-13 zeolite\u003c/h2\u003e \u003cp\u003eThe NH\u003csub\u003e4\u003c/sub\u003e-form SSZ-13 sample was obtained by ion-exchange of the calcined sample with NH\u003csub\u003e4\u003c/sub\u003eCl solution (1.0 M, liquid/solid\u0026thinsp;=\u0026thinsp;20) at 80\u0026deg;C, each time is 3 h for a total of two times. Then, H-form SSZ-13 sample was acquired by NH\u003csub\u003e4\u003c/sub\u003e-form SSZ-13 calcination at 500\u0026deg;C for 4 h. The Cu-form sample was prepared by ion exchange of the H-form sample two times with Cu(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e2\u003c/sub\u003e solution (0.1 M, liquid/solid\u0026thinsp;=\u0026thinsp;100) at 80\u0026deg;C, and each time is 3 h, followed by filtration, washing and drying at 80\u0026deg;C.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e2.4 Samples Characterization\u003c/h2\u003e \u003cp\u003ePowder X-ray diffraction (XRD) patterns of the samples were recorded on a MiniFlex 600 X-ray diffractometer(Japan, Rigaku) using Cu Kα radiation at 40 kV and 15 mA. The relative crystallinity of each sample was determined by calculating the ratio of the total area of five major diffraction peaks in the obtained sample at 2θ\u0026thinsp;=\u0026thinsp;9.6, 16.2, 20.8, 24.9 and 26.2\u0026deg; to that of the SSZ-13 seed zeolite (100% crystallinity). The TENSOR 27 Fourier-transform infrared spectrometer produced by BRUKER Company was used for measurement of FTIR spectra of the samples by the conventional KBr(spectroscopy grade) pellet technique. The crystal morphology of the samples was observed by a JEOL/JSM-6700F scanning electron microscopy (SEM). Energy dispersive spectroscopy (EDS) element analysis was performed operated at 10 kV. Thermal analysis was performed using Rigaku Thermo Plus Evo TG8120. Approximately 10 mg of the sample was introduced in an alumina crucible and loaded in the analyzer chamber. The samples were heated from room temperature to 800\u0026deg;C with a heating rate of 10\u0026deg;C\u0026middot;min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e under an air flow of 30 mL\u0026middot;min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. Textural properties of the samples were measured by N\u003csub\u003e2\u003c/sub\u003e adsorption at 77 K on a Micrometrics ASAP 2020 system. Prior to the experiment, the samples were degassed at 200\u0026deg;C for 8 h, and then adsorbed N\u003csub\u003e2\u003c/sub\u003e at -196\u0026deg;C. The specific surface area of the sample was calculated based on the BET equation, and the micropore volume and surface area were determined using the t-plot method. The acidity of the samples was measured using an NH\u003csub\u003e3\u003c/sub\u003e temperature-programmed desorption instrument (NH\u003csub\u003e3\u003c/sub\u003e-TPD, Micrometrics AutoChem II 2920 chemisorption analyzer) equipped with a thermal conductivity detector (TCD). 0.1 g sample was pretreated at 550\u0026deg;C for 30 min and then cooled to 100\u0026deg;C in Ar. Subsequently, the sample adsorbed NH\u003csub\u003e3\u003c/sub\u003e for 0.5 h under the mixed gas of 10% NH\u003csub\u003e3\u003c/sub\u003e/Ar. After purging in Ar for 0.5 h at 100\u0026deg;C to remove the weakly adsorbed NH\u003csub\u003e3\u003c/sub\u003e. The measurement of the desorbed NH\u003csub\u003e3\u003c/sub\u003e was performed from 100 to 650\u0026deg;C at a rate of 10\u0026deg;C\u0026middot;min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e in Ar flow (30 mL\u0026middot;min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e). H\u003csub\u003e2\u003c/sub\u003e Temperature-programmed reduction (H\u003csub\u003e2\u003c/sub\u003e-TPR) was also performed on the AUTO-CHEM-II-2920 with a thermal conductivity detector (TCD). 0.1 g sample was pretreated in a 5% O\u003csub\u003e2\u003c/sub\u003e/He flow at 300\u0026deg;C for 30 min, then heated from room temperature to 800\u0026deg;C at 10\u0026deg;C\u0026middot;min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e in the mixed gas of 10 vol% H\u003csub\u003e2\u003c/sub\u003e/Ar (40 mL\u0026middot;min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e). The hydrogen consumption was measured quantitatively by TCD. The element composition(SAR) was determined by inductively coupled plasma optical emission spectrometry (ICP-OES) (Agilent, 720). The \u003csup\u003e27\u003c/sup\u003eAl and \u003csup\u003e29\u003c/sup\u003eSi MAS NMR spectra were measured on a Bruker Avance III 600 spectrometer at 156.4 and 99.3 MHz, respectively. \u003csup\u003e27\u003c/sup\u003eAl NMR spectra were recorded under a spinning rate of 20 KHz, and the reference chemical shift was Al(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e aqueous solution. The \u003csup\u003e29\u003c/sup\u003eSi MAS NMR spectra were recorded at a spinning rate of 5 kHz, and the reference chemical shift was tetramethylsilane (TMS).\u003c/p\u003e \u003cp\u003eThe Si/Al ratio of the samples were calculated from \u003csup\u003e29\u003c/sup\u003eSi MAS NMR spectra using Eq.\u0026nbsp;(\u003cspan refid=\"Equ1\" class=\"InternalRef\"\u003e1\u003c/span\u003e)[\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e, \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e]:\u003cdiv id=\"Equ1\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ1\" name=\"EquationSource\"\u003e\n$$\\:\\frac{\\text{S}\\text{i}}{\\text{A}\\text{l}}=\\frac{\\sum\\:_{n=0}^{4}{I}_{\\text{S}\\text{i}\\left(n\\text{A}\\text{l}\\right)}}{\\sum\\:_{n=0}^{4}0.25n{I}_{\\text{s}\\text{i}\\left(n\\text{A}\\text{l}\\right)}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e1\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003ewhere \u003cem\u003en\u003c/em\u003e is the number of Al neighbors, \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:{I}_{\\text{s}\\text{i}\\left(\\text{n}\\text{A}\\text{l}\\right)}\\)\u003c/span\u003e\u003c/span\u003e is the intensity of peak \u003cem\u003en\u003c/em\u003e.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003e2.5 Catalytic test\u003c/h2\u003e \u003cp\u003eThe NH\u003csub\u003e3\u003c/sub\u003e-SCR reaction was performed in a fixed-bed quartz reactor. The catalysts with particle size of 40\u0026ndash;60 mesh were placed in the tube reactor. The total flow rate was held at 200 mL\u0026middot;min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, with gas composition of 0.05%NO, 10% O\u003csub\u003e2\u003c/sub\u003e, 0.05%NH\u003csub\u003e3\u003c/sub\u003e and Ar as balance gas. 0.1 g zeolite samples were used for the tests, with gas hourly space velocity of 80000 h\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. A Fourier transform infrared spectrometer (Bruker) was chosen to detect the concentration of NO, N\u003csub\u003e2\u003c/sub\u003eO and NH\u003csub\u003e3\u003c/sub\u003e. To investigate the hydrothermal stability, the samples were hydrothermally treated at 750\u0026deg;C for 16 h in flowing air containing 10% H\u003csub\u003e2\u003c/sub\u003eO.\u003c/p\u003e \u003c/div\u003e"},{"header":"3. Results and discussion","content":"\u003cdiv id=\"Sec9\" class=\"Section2\"\u003e \u003ch2\u003e3.1 SSZ-13 zeolite synthesis using various combinations of silica/alumina sources\u003c/h2\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e(A) HSZ\u0026thinsp;+\u0026thinsp;Al, (B) CZTZ, (C) LSZ\u0026thinsp;+\u0026thinsp;Si\u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e shows the hydrothermal conversion process of three synthesis strategies monitored by XRD. All XRD patterns were measured after 1.5\u0026thinsp;~\u0026thinsp;48 h hydrothermal crystallization. Apparently, with the extension of crystallization time, typical diffraction peaks of starting MFI gradually decrease, while the diffraction peaks of target CHA structure increase. The diffraction peaks corresponding to MFI zeolite disappeared completely after hydrothermal treatment for 3.5 h (HSZ\u0026thinsp;+\u0026thinsp;Al, Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ea), 4.5 h (CZTZ, Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eb) and 3 h (LSZ\u0026thinsp;+\u0026thinsp;Si, Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ec), respectively. After 2.5,3, or 1.5 h of hydrothermal treatment, the diffraction peaks corresponding to CHA zeolite were initially observed in HSZ\u0026thinsp;+\u0026thinsp;Al, CZTZ and LSZ\u0026thinsp;+\u0026thinsp;Si samples, respectively, implying that the nucleation of CHA zeolite occurred during the first 3 h of treatment. The highly crystalline CHA zeolites with no impurity were obtained only after 4.5, 6, or 4.5 h, indicating rapid transformation of ZSM-5 regardless of their initial SARs. Further extending the crystallization time to 48 h, there are no significant changes in the relative crystallinity of all obtained samples from three strategies. It was also noted that trace competitive phases MOR appear in CZTZ samples when crystallized less than 6 h, while quartz phases appear in HSZ\u0026thinsp;+\u0026thinsp;Al and LSZ\u0026thinsp;+\u0026thinsp;Si samples after long-time crystallization for 24\u0026thinsp;~\u0026thinsp;48 h.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003edifferent starting materials at various crystallization time\u003c/p\u003e \u003cp\u003eCombined with the corresponding crystallization curves and solid yields(Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e), it can also be seen that the crystallization rates of HSZ\u0026thinsp;+\u0026thinsp;Al and LSZ\u0026thinsp;+\u0026thinsp;Si synthesis systems are faster than that of CZTZ system. Further extending the crystallization time to 48 h, the relative crystallinities of samples are still maintained above 90%, which suggest full crystallization of SSZ-13. Additionally, the solid yields of the obtained samples increase with the crystallization time at early stage, and then stabilizes at ~\u0026thinsp;85% for HSZ\u0026thinsp;+\u0026thinsp;Al, ~\u0026thinsp;71% for CZTZ and ~\u0026thinsp;65% for LSZ\u0026thinsp;+\u0026thinsp;Si, respectively(inset of Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e). To sum up, SSZ-13 zeolites can be synthesized rapidly by interzeolite transformation of ZSM-5 with various SARs through three experimental schemes, and additional Al- or Si- source accelerated dissolution of starting ZSM-5 and crystallization of target SSZ-13 zeolite.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e(A) HSZ\u0026thinsp;+\u0026thinsp;Al, (B) CZTZ, (C) LSZ\u0026thinsp;+\u0026thinsp;Si\u003c/p\u003e \u003cp\u003eFurthermore, the framework/ring vibrations in zeolites samples obtained from three experimental schemes at the different transformation stages were monitored by FT-IR measurements (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e), in order to offer an insight into the evolution of the short-range order in solid samples during the MFI-CHA transformation process. In the starting ZSM-5 zeolites, the adsorption bands at 800 and 450 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e were assigned to the symmetric stretching and bending vibration mode of T\u0026ndash;O\u0026ndash;T in the framework structure, respectively[\u003cspan additionalcitationids=\"CR33\" citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e], and the peaks at 550 and 626 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e were ascribed to the vibration of isolated and condensed five-membered rings, respectively [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e, \u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e]. As for the samples obtained at various crystallization time, the bands centered at 420 and 460 cm\u003csup\u003e-1\u003c/sup\u003e are related to T-O bending vibration of CHA zeolites[\u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e], the peaks at 796 cm\u003csup\u003e-1\u003c/sup\u003e were assigned to the T-O-T symmetric stretching vibration in CHA cages[\u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e, \u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e]. Additionally, the vibrational peaks at 639 and 537 cm\u003csup\u003e-1\u003c/sup\u003e were ascribed to the double six-member rings(D6Rs) and single six-member rings(S6Rs) in the SSZ-13 framework[\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e]. As the crystallization process proceeds, the peaks at 550 and 626 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e weakened gradually and finally disappeared at 3.5 h (HSZ\u0026thinsp;+\u0026thinsp;Al), 4.5 h(CZTZ), and 3 h (LSZ\u0026thinsp;+\u0026thinsp;Si), respectively, indicating the disintegration of 5Rs in the ZSM-5 framework. Meanwhile, the bands at 800 and 450 cm\u003csup\u003e-1\u003c/sup\u003e gradually shifted to 796 and 460 cm\u003csup\u003e-1\u003c/sup\u003e, respectively, and the peaks at 420, 537, 639 and 676 cm\u003csup\u003e-1\u003c/sup\u003e of CHA gradually appeared and increased with time until SSZ-13 fully crystallize at 4.5 h(HSZ\u0026thinsp;+\u0026thinsp;Al), 6 h(CZTZ) and 4.5 h (LSZ\u0026thinsp;+\u0026thinsp;Si), respectively. Subsequently, there was almost no significant change over time. This is consistent with the aforementioned XRD results. Therefore, it seems that the MFI-CHA transformation is triggered by disintegration of S5Rs in MFI and simultaneous generation of S4Rs and S6Rs, which were further rearranged into D6Rs and CHA cages(composite building units of CHA zeolites) and then serve as a kinetic mediator for nucleating the CHA structure[\u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e40\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eTo comprehend the evolution of parent ZSM-5 zeolites with and without combination of Si- or Al- source during the rapid transformation, morphological changes of obtained samples during the crystallization process were analyzed. Figure\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e displays the SEM images of the samples obtained from three experimental schemes at various crystallization time.\u003c/p\u003e \u003cp\u003eFor HSZ\u0026thinsp;+\u0026thinsp;Al system, it was observed that the high silica ZSM-5 (SAR\u0026thinsp;=\u0026thinsp;120) crystals exhibited the aggregates of ellipsoidal particles with the size of 200\u0026thinsp;~\u0026thinsp;400 nm (Fig.\u0026nbsp;4A1). After crystallization for 1.5 h, some ZSM-5 crystals showed obvious fracture and damage (Fig.\u0026nbsp;4A2), while at this time the SSZ-13 crystals could not be found. When the crystallization time was 2.5 h, a large amount of ZSM-5 zeolites were dispersed and depolymerized into fragments, accompanied by appearance of SSZ-13 cubic crystals with a size of 300\u0026thinsp;~\u0026thinsp;500 nm (indicated by red arrows in Fig.\u0026nbsp;4A3). After 4.5 h of crystallization, SSZ-13 cubic crystals grew to 700 nm and showed layered cubic morphology, while ZSM-5 zeolite and other amorphous substances completely disappeared (Fig.\u0026nbsp;4A4). When the crystallization time was further extended to 48 h, the layered cubic morphology (~\u0026thinsp;700 nm) of the sample did not change significantly, but some quartz phase impurities could be observed (indicated by yellow arrows in Fig.\u0026nbsp;4A5).\u003c/p\u003e \u003cp\u003eRegarding the CZTZ system, the parent ZSM-5(SAR\u0026thinsp;=\u0026thinsp;38) displayed typical hexagonal prismatic morphology with a size of about 3\u0026thinsp;~\u0026thinsp;4 \u0026micro;m (Fig.\u0026nbsp;4B1). After crystallization for 1.5 h, it was seen that ZSM-5 crystals were cracked and damaged obviously under the action of alkaline solution, and the surface also became rough (Fig.\u0026nbsp;4B2). When the crystallization time is 3 h (Fig.\u0026nbsp;4B3), numerous SSZ-13 cubic crystals about 400 nm appeared at the crack and defect site on the surface of ZSM-5, suggesting that nucleation could occur on the available MFI surface. When the crystallization time is 6 h, ZSM-5 zeolites were completely transformed into SSZ-13 cubic crystals with a size of 600\u0026thinsp;~\u0026thinsp;900 nm (Fig.\u0026nbsp;4B4). Notably, in addition to well-developed cubic crystals, some complex intergrowths and interpolations between two or more cubic crystals were also observed. This may be related to the fact that dissolved MFI fragments are not easily assembled into crystals with perfect morphologies. Extending the crystallization time to 48 h, the sizes of the SSZ-13 zeolites were slightly increased to 700\u0026thinsp;~\u0026thinsp;1000 nm (Fig.\u0026nbsp;4B5).\u003c/p\u003e \u003cp\u003eIn the case of LSZ\u0026thinsp;+\u0026thinsp;Si system, the parent ZSM-5(SAR\u0026thinsp;=\u0026thinsp;24) also exhibits typical hexagonal prismatic crystals with a size of 3\u0026thinsp;~\u0026thinsp;4 \u0026micro;m (Fig.\u0026nbsp;4C1). After crystallization for 1.5 h (Fig.\u0026nbsp;4C2), SSZ-13 cubic crystals with a size of approximately 200 nm have appeared on the surface of ZSM-5, corresponding to the weak XRD signal of CHA (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eb). When the crystallization time was extended to 2.5 h, the majority of ZSM-5 zeolites have been transformed into cubic SSZ-13 crystals with a size of 100\u0026thinsp;~\u0026thinsp;300 nm, and only a small quantity of residual ZSM-5 fragments remained (indicated by red arrows in Fig.\u0026nbsp;4C3). It is noteworthy that the starting ZSM-5 zeolites have a similar size compared to CZTZ scheme, while the starting ZSM-5 with lower SAR in LSZ\u0026thinsp;+\u0026thinsp;Si system dissolved more rapidly in the alkaline solution. After 4.5 h of crystallization, the complete transformation of MFI-CHA was already achieved, and the average size of SSZ-13 cubic crystals increased to ~\u0026thinsp;400 nm (Fig.\u0026nbsp;4C4). When the crystallization time is further extended to 48 h, the cube morphology of some crystals became less regular, and accompanied by a small amount of quartz phase impurities (indicated by yellow arrows in Fig.\u0026nbsp;4C5).\u003c/p\u003e \u003cp\u003eBased on the above results, it is inferred that the additional Al- or Si- source have a significant effect on the properties of the synthesis gel and thus on the crystallization kinetics.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e shows the TG-DTG curves of the samples obtained from three experimental schemes. It was seen that all TG curves of fully crystallized samples exhibited three weight loss steps. The first stage between room temperature and 300\u0026deg;C is attributed to physically adsorbed water inside zeolites. The second weight loss occurring at 300\u0026thinsp;~\u0026thinsp;500\u0026deg;C was assigned to the combustion of TMAdaOH, indicating that TMAdaOH was incorporated into the SSZ-13 structure. The third stage of weight loss occurs above 500\u0026deg;C, which is related to the removal of organic remnants. The amount of weight loss of fully crystallized samples in 300\u0026thinsp;~\u0026thinsp;700\u0026deg;C range is about 21\u0026thinsp;~\u0026thinsp;22 wt%, indicating that a large amount of TMAdaOH were occluded in the product zeolite. Additionally, it was noted that an additional weak peak near 350\u0026deg;C appeared in the DTG curves of samples obtained from three synthetic systems at the initial crystallization stage (before 2.5 h, 3 h and 1.5 h, respectively) (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e), at which time ZSM-5 was not completely transformation. Considering that no organic template should remain on the outer surface of the sample after repeated washing, suggesting that TMAdaOH may be infiltrated or inserted into the micro-cracks of ZSM-5 crystals caused by the initial dissolution. This may promote the rapid disintegration of parent ZSM-5 zeolite.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec10\" class=\"Section2\"\u003e \u003ch2\u003e3.2 Mechanism of the interzeolite conversion from MFI to CHA\u003c/h2\u003e \u003cp\u003eAccording to the above results, it is apparent that highly crystalline SSZ-13 with submicron dimensions can be synthesized rapidly within 6 h at 160\u0026deg;C via interzeolite transformation from ZSM-5 zeolites with various SAR (24\u0026thinsp;~\u0026thinsp;120), although the MFI-CHA transformation is unfavorable from both thermodynamic (adverse FD gradient) and kinetic (no common D6Rs CBU) perspectives. There are two aspects possible reasons for the successful and rapid transformation of MFI to CHA. On the one hand, combined with aforementioned SEM observation (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e) that the initially formed SSZ-13 cubic crystals grew at the crack or defect site on the surface of remnant ZSM-5, and the phenomenon that TMAdaOH presented in incompletely dissolved ZSM-5 at the initial stage (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e). It was suggested that TMAdaOH may first be inserted into the micro-cracks or small defects of ZSM-5 crystals formed by the degradation in the early stage of hydrothermal transformation. This may have acted as a wedge, thus promoted the disintegration of the parent ZSM-5 zeolite. On the other hand, with the rapid degradation of starting ZSM-5, the S5Rs predominating in the MFI framework were disassembled, while rapidly producing S4Rs and S6Rs building units, which facilitate the assembly of D6Rs and CHA cages. These CBUs act as a kinetic mediator to promote the rapid crystallization of product SSZ-13 zeolite.\u003c/p\u003e \u003cp\u003eIn addition, compared with CZTZ synthesis system, the crystallization rates of SSZ-13 synthesized by HSZ\u0026thinsp;+\u0026thinsp;Al and LSZ\u0026thinsp;+\u0026thinsp;Si system were faster, and the pure SSZ-13 with high crystallinity and small size can be obtained in only 4.5 h at 160\u0026deg;C. This is mainly due to the fact that the SBUs produced by the early dissolution of MFI combines with additional Al- or Si- source to rapidly form a larger amount of crystal nuclei under the assistance of the TMAdaOH and seed. Simultaneously, with the rapid consumption of these structural units, the dissolution of the starting ZSM-5 zeolite will be further accelerated. Meanwhile, the rapid formation of a large number of crystal nuclei also leads to smaller SSZ-13 product crystals, which are in good agreement with SEM observation (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e). Based on the above analysis, the interzeolite transformation process of MFI-CHA from three strategies was proposed and illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec11\" class=\"Section2\"\u003e \u003ch2\u003e3.3 Physicochemical properties\u003c/h2\u003e \u003cp\u003eFurther, three fully crystallized SSZ-13 samples prepared from various experimental schemes, HSZ-4.5 h, ESZ-6.0 h and LSZ-4.5 h were selected to conduct N\u003csub\u003e2\u003c/sub\u003e adsorption-desorption, NH\u003csub\u003e3\u003c/sub\u003e-TPD, \u003csup\u003e29\u003c/sup\u003eSi/\u003csup\u003e27\u003c/sup\u003eAl-MAS NMR and H\u003csub\u003e2\u003c/sub\u003e-TPR measurement for a detail investigation of their texture properties, acidity properties, chemical states of Si- and Al- species, and the status and dispersion of Cu species after Cu\u003csup\u003e2+\u003c/sup\u003e exchange, respectively.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e illustrates the N\u003csub\u003e2\u003c/sub\u003e adsorption-desorption isotherms of three SSZ-13 samples, which exhibit type-I isotherms characteristic of microporous solids along with a capillary condensation step above a relative pressure of 0.9 due to the intercrystal voids arising from the stacking of nanocrystals. Their textual properties and SARs are listed in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e. Clearly, the specific surface area and the total pore volume of the three SSZ-13 samples are all above 700 m\u003csup\u003e2\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e and 0.29 cm\u003csup\u003e3\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, respectively, which further verify the high crystallinity of these samples and successful interzeolite conversion. Among them, the SSZ-13 synthesized by LSZ\u0026thinsp;+\u0026thinsp;Si strategy has the largest specific surface area (800 m\u003csup\u003e2\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), the total pore volume (0.36 cm\u003csup\u003e3\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) and mesopore volume (0.05 cm\u003csup\u003e3\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), which should be related to the smaller size of the resultant sample due to the promoting effect of additional Si source on the conversion of parent MFI zeolite. Besides, the SARs of three SSZ-13 samples measured by ICP are 25.8, 29.5 and 35.1, respectively. The difference in SARs of SSZ-13 samples may be due to the various disintegration rate and degree caused by the different SARs and particle sizes of parent zeolites at the initial stage, as well as the different reactivity of the additional Si- or Al- source. Among them, the SAR of LSZ-4.5 h sample was the highest, which may be related to that the Al source was entirely from ZSM-5 with low SAR, and there were fewer Al species and more silicon species available in the nucleation stage.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab2\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eTextural properties and compositions(SAR) of HSZ-4.5 h, CZTZ-6.0 h and LSZ-4.5 h samples\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"9\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c8\" colnum=\"8\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c9\" colnum=\"9\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSamples\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cem\u003eS\u003c/em\u003e\u003csub\u003eBET\u003c/sub\u003e\u003c/p\u003e \u003cp\u003e(m\u003csup\u003e2\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u003cem\u003eS\u003c/em\u003e\u003csub\u003emicro\u003c/sub\u003e\u003c/p\u003e \u003cp\u003e(m\u003csup\u003e2\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1)\u003c/sup\u003e\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cem\u003eS\u003c/em\u003e\u003csub\u003eext\u003c/sub\u003e\u003c/p\u003e \u003cp\u003e(m\u003csup\u003e2\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003e\u003cem\u003eV\u003c/em\u003e\u003csub\u003etot\u003c/sub\u003e\u003c/p\u003e \u003cp\u003e(cm\u003csup\u003e3\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u003cem\u003eV\u003c/em\u003e\u003csub\u003emicro\u003c/sub\u003e\u003c/p\u003e \u003cp\u003e(cm\u003csup\u003e3\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cem\u003eV\u003c/em\u003e\u003csub\u003emeso\u003c/sub\u003e\u003c/p\u003e \u003cp\u003e(cm\u003csup\u003e3\u003c/sup\u003e\u0026middot;g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c8\"\u003e \u003cp\u003eSAR\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c9\"\u003e \u003cp\u003eSAR\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eHSZ-4.5 h\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e737\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e711\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e26\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e0.30\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e0.28\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\"\u003e \u003cp\u003e0.02\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c8\"\u003e \u003cp\u003e25.8\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e \u003cp\u003e26.4\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eCZTZ-6.0 h\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e707\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e679\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e18\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e0.29\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e0.27\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\"\u003e \u003cp\u003e0.02\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c8\"\u003e \u003cp\u003e29.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e \u003cp\u003e27.3\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eLSZ-4.5 h\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e800\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e779\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e21\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c5\"\u003e \u003cp\u003e0.36\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e0.31\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c7\"\u003e \u003cp\u003e0.05\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c8\"\u003e \u003cp\u003e35.1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e \u003cp\u003e37.4\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003e \u003csup\u003ea\u003c/sup\u003e SiO\u003csub\u003e2\u003c/sub\u003e/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e ratio, determined by ICP. \u003csup\u003eb\u003c/sup\u003e SiO\u003csub\u003e2\u003c/sub\u003e/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e ratio, determined by \u003csup\u003e29\u003c/sup\u003eSi MAS NMR spectra.\u003c/p\u003e \u003cp\u003eThe chemical states of the aluminum and silicon in the obtained HSZ-4.5 h, CZTZ-6 h, LSZ-4.5 h samples were investigated by \u003csup\u003e27\u003c/sup\u003eAl and \u003csup\u003e29\u003c/sup\u003eSi MAS NMR, as illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003eA and B, respectively. According to Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003eA, only the resonances around 58 ppm assigned to tetrahedrally coordinated framework Al species were observed for all three samples[\u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e41\u003c/span\u003e, \u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e], while a resonance corresponding to that of octahedrally coordinated Al species, namely an extra-framework aluminum species, was not detected around 0 ppm. This means that all Al species are well incorporated into the zeolitic frameworks of three samples. Moreover, a faint signal appearing around \u0026minus;\u0026thinsp;20 ppm is due to a spinning-side band[\u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e]. In addition, the \u003csup\u003e29\u003c/sup\u003eSi MAS NMR spectra of all three samples showed three similar resonance peaks (Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003eB). The resonances at -108 ~ -111, -103 ~ -106 and \u0026minus;\u0026thinsp;98 ~ -101 ppm are attributed to Si(4Si, 0Al), Si(3Si,1Al)、 Si(2Si, 2Al) or Si(3Si, OH) structures, respectively[\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e44\u003c/span\u003e, \u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e]. The peak area percentages of these resonances are obtained from the deconvolution of the \u003csup\u003e29\u003c/sup\u003eSi MAS NMR spectra was shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003eC. It was found that although they all contain three similar resonances at almost the same chemical shift, there are some differences in the relative proportion of each peak area in total peak area, indicating the slightly different distribution of Si and Al of three samples. Moreover, when the resonance at -98 ~ -101 ppm was assigned to Si(3Si, OH) atom arising from the defect groups [\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e44\u003c/span\u003e], the framework SiO\u003csub\u003e2\u003c/sub\u003e/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e ratios of the three samples calculated based on the areas of these resonances using Eq.\u0026nbsp;\u003cspan refid=\"Equ1\" class=\"InternalRef\"\u003e1\u003c/span\u003e are in good agreement with the data from ICP analysis (Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe acidity of three samples are measured by temperature-programmed desorption of ammonia (NH\u003csub\u003e3\u003c/sub\u003e-TPD) technique. The NH\u003csub\u003e3\u003c/sub\u003e-TPD profiles and corresponding acidity data are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003e and Table S2, respectively. Obviously, there are two well resolved peaks in the desorption temperature range of all three samples. The low-temperature desorption peaks at 173\u0026thinsp;~\u0026thinsp;179\u0026deg;C correspond to desorption of NH\u003csub\u003e3\u003c/sub\u003e from weak Lewis acid sites, while the high temperature desorption peaks located at 456\u0026thinsp;~\u0026thinsp;470\u0026deg;C are assigned to strong Br\u0026oslash;nsted acid sites[\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e]. Among them, the CZTZ-6 h sample possesses the largest total acid and strong acid amount, while those of the LSZ-4.5 h sample with the highest SAR were the lowest. In addition, compared to HSZ-4.5 h, the high temperature NH\u003csub\u003e3\u003c/sub\u003e-desorption peaks of CZTZ-6 h and LSZ-4.5 h slightly shift to high and low temperature, respectively. This is indicative of the higher acid strength of CZTZ-6 h and the lower one of LSZ-4.5 h[\u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e46\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eH\u003csub\u003e2\u003c/sub\u003e-TPR measurements were carried out to determine the distribution of Cu species in these samples, and the results are shown in Fig. \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003e. It illustrates that the reduction peaks below 500\u0026deg;C can be attributed to different types of Cu species(Fig. \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003eA), where the peaks at ~\u0026thinsp;215 and 340\u0026deg;C are ascribed to the reduction of Cu\u003csup\u003e2+\u003c/sup\u003e to Cu\u003csup\u003e+\u003c/sup\u003e in the 8MRs (Cu(OH)\u003csup\u003e+\u003c/sup\u003e-Z species balanced by one framework charge) and in D6Rs (Cu\u003csup\u003e2+\u003c/sup\u003e-2Z species balanced by two framework charges), respectively. For the NH\u003csub\u003e3\u003c/sub\u003e-SCR reaction, it is demonstrated that these two copper species in Cu-CHA are the active sites[\u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e47\u003c/span\u003e, \u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e48\u003c/span\u003e]. Moreover, the peak at ~\u0026thinsp;470\u0026deg;C is assigned to the reduction of Cu\u003csup\u003e+\u003c/sup\u003e ions to Cu\u003csup\u003e0\u003c/sup\u003e, and this peak is strongest in HSZ-4.5 h sample. It is thought that this kind of Cu\u003csup\u003e+\u003c/sup\u003e ion is also coming from D6Rs unit[\u003cspan citationid=\"CR49\" class=\"CitationRef\"\u003e49\u003c/span\u003e].Additionally, broad peaks at temperatures above 550\u0026deg;C are associated with the reduction of highly stable Cu\u003csup\u003e+\u003c/sup\u003e to Cu\u003csup\u003e0\u003c/sup\u003e[\u003cspan additionalcitationids=\"CR51\" citationid=\"CR50\" class=\"CitationRef\"\u003e50\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e52\u003c/span\u003e]. The different relative proportions(Fig. \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003eB) and reduction temperatures of various copper species in the three samples indicate that the synthesis strategies have a certain effect on the copper distribution and reduction of the samples.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec12\" class=\"Section2\"\u003e \u003ch2\u003e3.4 Catalytic performances of samples\u003c/h2\u003e \u003cp\u003eThe catalytic performances of three Cu-SSZ-13 samples in NH\u003csub\u003e3\u003c/sub\u003e-SCR reaction before and after hydrothermal aging treatments were evaluated, and the results are given in Fig.\u0026nbsp;\u003cspan refid=\"Fig10\" class=\"InternalRef\"\u003e10\u003c/span\u003e. All fresh samples exhibit high NO conversions (above 90%) over a wide temperature range of 190\u0026thinsp;~\u0026thinsp;490\u0026deg;C for HSZ-4.5 h, 200\u0026thinsp;~\u0026thinsp;500\u0026deg;C for CZTZ-6 h, and 210\u0026thinsp;~\u0026thinsp;510\u0026deg;C for LSZ-4.5 h, respectively, evidencing the superior catalytic activity of three SSZ-13 samples synthesized by three synthesis schemes. Additionally, it was found that the low temperature (\u0026lt;\u0026thinsp;220\u0026deg;C) activity of the three samples in the order of HSZ-4.5 h\u0026thinsp;\u0026gt;\u0026thinsp;CZTZ-6 h\u0026thinsp;\u0026gt;\u0026thinsp;LSZ-4.5 h. The best low temperature activity of HSZ-4.5 h in NH\u003csub\u003e3\u003c/sub\u003e-SCR performance may be related to more amount of Cu\u003csup\u003e+\u003c/sup\u003e as revealed by the H\u003csub\u003e2\u003c/sub\u003e-TPR result(Fig. \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003e). This is due to that, in addition to Cu\u003csup\u003e2+\u003c/sup\u003e active species, Cu\u003csup\u003e+\u003c/sup\u003e sites solvated by NH\u003csub\u003e3\u003c/sub\u003e have also been proposed as SCR active sites below 200\u0026deg;C[\u003cspan citationid=\"CR53\" class=\"CitationRef\"\u003e53\u003c/span\u003e], which is conducive to the reaction between adsorbed NH\u003csub\u003e3\u003c/sub\u003e substances and NO molecules at low temperatures.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eGiven that the high-temperature hydrothermal stability of Cu-SSZ-13 is vital for its practical application, the NH\u003csub\u003e3\u003c/sub\u003e-SCR catalytic properties of hydrothermally aged Cu-SSZ-13 samples are also investigated. For Cu-CZTZ-6 h and Cu-LSZ-4.5 h samples, the NO conversions still remain higher than 90% in the range of 200\u0026thinsp;~\u0026thinsp;480\u0026deg;C after hydrothermal treatment at 750\u0026deg;C for 16 h, suggesting their excellent hydrothermal stability. While for Cu-HSZ-4.5 h sample, the NO\u003cem\u003ex\u003c/em\u003e conversion decreased significantly, but also remained above 80% in the wide range of 240\u0026thinsp;~\u0026thinsp;600\u0026deg;C after the same treatment. The relatively inferior hydrothermal stability of Cu-HSZ-4.5 h may be related to its relatively low SAR, less Cu\u003csup\u003e2+\u003c/sup\u003e-2Z active site, and NH\u003csub\u003e3\u003c/sub\u003e desolvation from Cu\u003csup\u003e+\u003c/sup\u003e-complexes at higher temperature[\u003cspan citationid=\"CR53\" class=\"CitationRef\"\u003e53\u003c/span\u003e].\u003c/p\u003e \u003c/div\u003e"},{"header":"4. Conclusions","content":"\u003cp\u003eIn summary, the synthesis of SSZ-13 with ZSM-5 as the starting zeolite was investigated by three transformation strategies, namely HSZ\u0026thinsp;+\u0026thinsp;Al, CZTZ and LSZ\u0026thinsp;+\u0026thinsp;Si. Based on these three strategies, highly crystalline SSZ-13 zeolites with submicron sizes were successfully prepared within 6 h at 160\u0026deg;C. Besides, it is revealed that HSZ\u0026thinsp;+\u0026thinsp;Al and LSZ\u0026thinsp;+\u0026thinsp;Si schemes exhibit faster crystallization rates and distinct crystal size compared with CZTZ, suggesting that additional Al- or Si- source can not only regulate the SAR of initial gel, but also modify the kinetics of nucleation and crystallization during the MFI-CHA transformation process. In addition, a plausible mechanism for the highly efficient transformation from MFI to CHA was discussed. Under the action of alkaline solution and promotion of TMAdaOH, 5Rs in ZSM-5 framework was rapidly deconstructed and converted into S4Rs and S6Rs, which is rapidly assembled into D6Rs and CHA cages, thus further forming CHA framework. Significantly, the properties of the locally ordered aluminosilicate species formed in the gel are associated with the starting material and ultimately play a role in the kinetic nucleation and crystallization process. The resultant HSZ-4.5 h, CZTZ-6 h and LSZ-4.5 h samples, after Cu\u003csup\u003e2+\u003c/sup\u003e exchange, show good catalytic activity (the NO conversion remained over 90% at a temperature window of 200\u0026thinsp;~\u0026thinsp;500\u0026deg;C) and hydrothermal stability.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eCRediT authorship contribution statement\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eYufeng Liu:\u003c/strong\u003e Investigation, Validation, Writing - original draft.\u0026nbsp;\u003cstrong\u003eYuping Li:\u003c/strong\u003e Conceptualization, Methodology, Validation, Writing - review \u0026amp; editing. \u003cstrong\u003eZe Chen:\u0026nbsp;\u003c/strong\u003eInvestigation, Validation, Writing - original draft. \u003cstrong\u003eFuchao Ji\u003c/strong\u003e: Data curation，Formal analysis. \u003cstrong\u003eLina Han:\u003c/strong\u003e Resources, Funding acquisition.\u003cstrong\u003e\u0026nbsp;Xiaohong Liang:\u003c/strong\u003e Writing \u0026ndash; review \u0026amp; editing. \u003cstrong\u003ePeide Han:\u0026nbsp;\u003c/strong\u003eSupervision.\u003c/p\u003e\u003cp\u003e \u003ch2\u003eDeclaration of Competing Interest\u003c/h2\u003e \u003cp\u003eThe authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.\u003c/p\u003e \u003c/p\u003e\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eY L: Investigation, Validation, Writing - original draft. Y L Conceptualization, Methodology, Validation, Writing - review \u0026amp; editing. Z C: Investigation, Validation, Writing - original draft. F J: Data curation Formal analysis. L H: Resources, Funding acquisition. X L: Writing \u0026ndash; review \u0026amp; editing. P H: Supervision.\u003c/p\u003e\u003ch2\u003eAcknowledgements\u003c/h2\u003e \u003cp\u003eThis work was supported by the National Natural Science Foundation of China (No.21978195) and Central Guided Local Science and Technology Development Fund Project(No. YDZJSX20231A012)\u003c/p\u003e\u003ch2\u003eData availability\u003c/h2\u003e \u003cp\u003eData will be made available on request.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eS. Mintova, M. Jaber, V. Valtchev, Nanosized microporous crystals: emerging applications. Chem. Soc. 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Soc. \u003cb\u003e138\u003c/b\u003e(37), 12025\u0026ndash;12028 (2016). \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003e.https://doi.org/10.1021/jacs.6b06809\u003c/span\u003e\u003cspan address=\".10.1021/jacs.6b06809\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"journal-of-porous-materials","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"jopo","sideBox":"Learn more about [Journal of Porous Materials](http://link.springer.com/journal/10934)","snPcode":"10934","submissionUrl":"https://submission.nature.com/new-submission/10934/3","title":"Journal of Porous Materials","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"SSZ-13 zeolite, Interzeolite transformation, ZSM-5, NH3-SCR of NOx, Diesel exhaust","lastPublishedDoi":"10.21203/rs.3.rs-5263931/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-5263931/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eCHA Zeolites are currently considered as the most effective catalysts to meet the increasingly stringent emission requirements of diesel vehicles. Herein, the synthesis of SSZ-13 zeolites(CHA topology) using ZSM-5 (MFI topology) with various SiO\u003csub\u003e2\u003c/sub\u003e/Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e ratios as parent zeolites were investigated in the presence of N,N,N, trimethtyl-1-adamantammonium hydroxide (TMAdaOH). The crystallization processes of three different strategies, that is, high silica ZSM-5 with additional Al source(HSZ\u0026thinsp;+\u0026thinsp;Al), completely zeolite to zeolite(CZTZ) transformation and low silica ZSM-5 with additional Si source(LSZ\u0026thinsp;+\u0026thinsp;Si) were compared. The results show that pure SSZ-13 zeolites with high crystallinity can be synthesized at 160\u0026deg;C for only 6 h by CZTZ strategy. While for the HSZ\u0026thinsp;+\u0026thinsp;Al and LSZ\u0026thinsp;+\u0026thinsp;Si synthesis systems, the complete transformation from MFI to CHA can even be shortened to 4.5 h at 160\u0026deg;C, suggesting the promoting effect of additional Al- or Si- source for MFI-CHA transformation. The rapid MFI-CHA transformation may be related to fast disintegration of parent ZSM-5 under the promotion of TMAdaOH template. Meanwhile, the five-membered rings predominating in the MFI framework rapidly disassembled and rearranged into favorable double six-membered ring and CHA cage composite building units, thus facilitate the rapid formation the CHA framework. Additionally, the resultant samples, after Cu\u003csup\u003e2+\u003c/sup\u003e exchange, showed superior catalytic activity and hydrothermal stability for the selective catalytic reduction of NO\u003cem\u003ex\u003c/em\u003e with NH\u003csub\u003e3\u003c/sub\u003e. The operation temperature window (NO\u003cem\u003ex\u003c/em\u003e conversion\u0026thinsp;\u0026gt;\u0026thinsp;90%) of HSZ-4.5 h, CZTZ-6.0 h and LSZ-4.5 h samples were all about 200\u0026thinsp;~\u0026thinsp;500\u0026deg;C. Among three samples, the HSZ-4.5 h presents best low-temperature catalytic activity, while CZTZ-6.0 h and LSZ-4.5 h samples show more superior hydrothermal stability.\u003c/p\u003e","manuscriptTitle":"Synthesis of CHA from MFI by three interzeolite transformation strategies and its Application in NH 3 -SCR reaction","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-10-21 15:35:53","doi":"10.21203/rs.3.rs-5263931/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2024-11-22T02:21:43+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-11-21T23:40:58+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"260168987014771691137512423635001524210","date":"2024-11-06T01:02:31+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-11-05T13:25:48+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"171210367152603904972594709618509389118","date":"2024-11-02T16:13:49+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"137830317869193467714037857817012094237","date":"2024-11-02T01:54:09+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"330864089667446791823617579167697345435","date":"2024-11-01T13:04:46+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"137771596930194653266744702065035947294","date":"2024-11-01T12:59:43+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-11-01T04:56:51+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"286370860619976600336171308062502775311","date":"2024-11-01T04:26:42+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"249567469250481771854321177690055422734","date":"2024-11-01T02:48:30+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"222797579077114625288645403340050295991","date":"2024-11-01T01:10:47+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2024-11-01T00:44:20+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2024-10-17T10:07:26+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2024-10-17T10:04:48+00:00","index":"","fulltext":""},{"type":"submitted","content":"Journal of Porous Materials","date":"2024-10-14T23:38:58+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"journal-of-porous-materials","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"jopo","sideBox":"Learn more about [Journal of Porous Materials](http://link.springer.com/journal/10934)","snPcode":"10934","submissionUrl":"https://submission.nature.com/new-submission/10934/3","title":"Journal of Porous Materials","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"ddf0bb19-2435-410d-a0a1-f85fdf429474","owner":[],"postedDate":"October 21st, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2024-12-23T16:09:10+00:00","versionOfRecord":{"articleIdentity":"rs-5263931","link":"https://doi.org/10.1007/s10934-024-01730-5","journal":{"identity":"journal-of-porous-materials","isVorOnly":false,"title":"Journal of Porous Materials"},"publishedOn":"2024-12-17 15:58:38","publishedOnDateReadable":"December 17th, 2024"},"versionCreatedAt":"2024-10-21 15:35:53","video":"","vorDoi":"10.1007/s10934-024-01730-5","vorDoiUrl":"https://doi.org/10.1007/s10934-024-01730-5","workflowStages":[]},"version":"v1","identity":"rs-5263931","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-5263931","identity":"rs-5263931","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}