Preparation of High Temperature Vulcanized Fluorosilicone Rubber by Hydrosilylation Addition Reaction

Preparation of High Temperature Vulcanized Fluorosilicone Rubber by Hydrosilylation Addition 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 Preparation of High Temperature Vulcanized Fluorosilicone Rubber by Hydrosilylation Addition Reaction Lele Huang, Mingying Wang, Yuqiang Zhang, Shen Diao This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-4218684/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 18 Jun, 2024 Read the published version in Silicon → Version 1 posted 7 You are reading this latest preprint version Abstract Fluorsilicone rubber as a new type of special functional rubber has attracted attention, which combines the advantages of the organic silicone materials and the organic fluorine materials. Herein, we reported fluorosilicone rubber vulcanized at high temperature by the hydrosilylation addition reaction. The silicone oil containing hydrogen in the pendant group and the perfluorocyclobutyl aryl ether (PFCBAE) group in the backbone (S-H-Oil-PFCBAE) was prepared by the hydrolytic polycondensation and ring opening reaction of silane with PFCBAE (M 4 ), octamethylcyclotetrasiloxane (D 4 ), and tetramethylcyclotetrasiloxane (D 4 H ) by the traditional catalysis of concentrated sulfuric acid. And S-H-Oil-PFCBAE was used as the crosslinker to vulcanize fluorosilicone rubber. The mechanical property, the thermal stability, the hydrophobicity, and the solvent resistance of vulcanizates were studied in detail. The result showed that S-H-Oil-PFCBAE could improve the comprehensive performances of fluorosilicone rubber. fluorosilicone rubber perfluorocyclobutyl hydrosilylation addition reaction Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 1. Introduction Fluorosilicone material which is a combination of Si-C bonds with the high bonding energy and C-F bonds which can play the role of shielding C-C bonds shows excellent performances. As the most significant product of the fluorosilicone material, fluorosilicone rubber was first launched in the 1950s (the commercial brand Silastic LS-53, Dow Corning). And then, fluorosilicone rubber has been widely applied in a variety of fields, including aerospace, automobiles, electronics, medicine and so on for the outstanding performances such as thermostable and cold resistance, environmental aging resistance, oil resistance and chemical corrosion resistance. The researchers have carried out many significative studies on the preparations and properties of fluorinesilicone rubber. Cui [ 1 ] successfully synthesized polyfluorosiloxane (just polymer not rubber) with different contents (12, 22, 29, and 38 mol%) of trifluoropropyl groups (-CH 2 CH 2 CF 3 ) and the test results showed that the higher contents of -CH 2 CH 2 CF 3 group, the better solvent resistance and the lower the thermal stability of polyfluorosiloxane. Indelekha [ 2 , 3 ] prepared fluorosilicone rubber (also -CH 2 CH 2 CF 3 group) cured in the hydrosilation system. And the vulcanizate exhibited not only excellent hydrophobicity and lipophobicity but also the acid resistance. Fei [ 4 ] synthesized fluorosilicone rubber (-CH 2 CH 2 CF 3 group). And the phenyl group was also introduced into the side chain. It was found that the phenyl group could improve the thermal stability and damping performance of the rubber. Xu used nano materials (including nano cerium dioxide [ 5 ] , multi-walled carbon nanotube [ 6 ] and boron particle [ 7 ] ) as the fillers to prepare fluorosilicone rubber (-CH 2 CH 2 CF 3 group). The nano materials can increase the thermal decomposition temperature of the rubber. Xu [ 8 ] used the vinyl fluorosilicone resin (-CH 2 CH 2 CF 3 group) containing imide which improves the thermal stability of the rubber as the crosslinker for fluorosilicone rubber. So [ 9 ] used the vinyl-functionalized POSS as the crosslinker to prepare fluorosilicone rubber (-CH 2 CH 2 CF 3 group), which also improves the thermal stability of the rubber. Tan [ 10 – 12 ] used the nano-particles (the multiwalled carbon nanotubes (MWCNT), modified SiO 2 /MWCNT, and the graphene nanoplatelets/barium titanate hybrid nanoparticles) as the fillers to prepared fluorosilicone rubber (-CH 2 CH 2 CF 3 group). Besides the mechanical and the thermal properties, the dielectric property was also systematically investigated. Although the research on fluorosilicone rubber has made some great progress, it can be found that the fluorine group of fluorosilicone rubber is generally -CH 2 CH 2 CF 3 group. However, the -CH 2 CH 2 CF 3 group usually has bed effect on the performances of fluorosilicone rubber, particularly the thermal stability. As a result, it is needed to develop the methods to improve the thermal stability of fluorosilicone rubber. Generally, it is essential to develop some new types of fluorine structure to enrich the types of fluorosilicone rubber and investigate the effect of novel fluorine structure on the properties of the materials. In our previous work [ 13 – 15 ] , we reported two kinds of fluorosilicone rubber containing perfluorocyclobutyl aryl ether (PFCBAE) group. Fluorosilicone rubber containing PFCBAE was first vulcanized by the thermal cyclization reaction of trifluoroethylene aryl ether (TFVE) which was also a new vulcanization method. But we found the stability of TFVE was not very good, which lead to the low content of PFCBAE structure and the extreme reaction conditions. Further, we synthesized a vinyl silicone oil with PFCBAE group in the backbone which was so-called the centralized crosslinker for fluorosilicone rubber. As we all know, vulcanization is a critical process in rubber processing, and the comprehensive properties of rubber can be significantly improved through the vulcanization. The vulcanization of fluorosilicone rubber is the same as that of traditional silicone rubber. The high temperature vulcanization of fluorosilicone rubber is mainly accomplished by the traditional peroxide reaction which is suitable for vulcanization of most rubbers and the hydrosilylation addition reaction which is a special reaction in organosilicone chemistry. In the present work, we prepare fluorosilicone rubber containing PFCBAE group by hydrosilylation addition reaction. Hydrogen containing silicone oil containing PFCBAE group (S-H-Oil-PFCBAE) is firstly synthesized. And then S-H-Oil-PFCBAE is used as the crosslinker to prepare the fluorosilicone rubber. The overall process is shown in Fig. 1 . The synthesis of S-H-Oil-PFCBAE and the influences of S-H-Oil-PFCBAE on fluorosilicone rubber are investigated in this work. 2. Experimental 2.1 Materials Silane with PFCBAE (M 4 ) was synthesized in our lab according to the literature [ 15 ] . Octamethylcyclotetrasiloxane (D 4 ) was purchased from Guangzhou Skycent Chemicals Co., Ltd. Tetramethylcyclotetrasiloxane (D 4 H ) was purchased from Jiande Juhe New Materials Co., Ltd. Hexamethyldisiloxane (MM) was purchased from Shanghai Gaoming Chemicals Co., Ltd. Base gum (110-2S, methylvinyl polysiloxane) was obtained by Dongjue Silicone Group Co., Limited. CAB-O-SIL-TS530 Fumed Silica was purchased from Cabot Corporation. Karstedt catalyst was synthesized in our lab according to the literature [ 16 ] . 2.2 Synthesis of S-H-Oil-PFCBAE According to the composition of S-H-Oil-PFCBAE listed in Table 1, D 4 , D 4 H , M 4 , and MM were mixed into the three-necked flask and were stirred vigorously at room temperature. And then concentrated sulfuric acid (4% weight of monomer) was added. The mixture was kept on stirring vigorously for 0.5 h and then 0.1g H 2 O was added and kept for 6 h. Another 0.1 g H 2 O and 20 mL toluene were added for 1 h. Then the mixture was washed with deionized H 2 O to the neutral and dried by Na 2 SO 4 . And the mixture was filtered. Finally, a yellow oily liquid was obtained after evaporating. The synthesis route was shown in Fig. 2 . Table 1 The composition of S 1 to S 5 Sample PFCBAE* D 4 (g) D 4 H (g) M 4 (g) MM(g) S 1 0 12.88 18 0 0.85 S 2 1 11.06 20.73 2.76 0.95 S 3 3 2.41 7.75 2.76 0.33 S 4 5 0.89 4.98 2.76 0.25 S 5 6.7 0 4.14 2.76 0.19 * mol content % 2.3 Preparation of fluorosilicone rubber Table 2 The composition of P 1 to P5* Sample Base gum Fumed silica Karstedt catalyst S-H-Oil-PFCBAE P 1 100 60 0.5 S 1 P 2 100 60 0.5 S 2 P 3 100 60 0.5 S 3 P 4 100 60 0.5 S 4 P 5 100 60 0.5 S 5 * All components are by weight as phr. The dosage of S-H-Oil-PFCBAE is 5 phr. The base gum was milled on a two-roll mill for 5–10 min. The fumed silica was added in batches for 30–40 min. The rubber was kept on milling for another 10 min after uniformly mixed. Then the rubber was kept in an air-dry oven at 160 o C for 1 h. The rubber was cooled to room temperature and remilled. Then S-H-Oil-PFCBAE (S 1 , S 2 , S 3 , S 4 , S 5 ) were added in batches for 5 min. After uniformly mixed, Karstedt catalyst was added. The rubber was vulcanized in the mold at 160 o C under a pressure of 15 MPa for 10 min and then postcured at 160 o C for 2 h under ambient pressure to obtain the final vulcanizates. The composition of fluorosilicone rubber is listed in Table 2 . 2.4 Characterization and measurements FTIR spectra were measured by IR spectrometer (Shimadzu IRAffinity-1S). 1 H NMR and 19 F NMR spectra were measured by NMR instrument (JEOL 400YH, CDCl 3 ). Molecular weights were determined by GPC (Waters 1515). DSC was measured by Netzsch Instrument (DSC 200F3). TGA was measured by TG 209F3 instrument under nitrogen. The tensile testing (ASTM D 412 method and ISO 527) and the tear testing (QB/T 1130–1991) were carried out by an electronic universal testing machine (UTM4103). Hardness (ASTM D 2240 method) was measured by durometer (Shore A). Water contact angle was determined by contact angle measuring instrument (JC2000C). Water absorption (GB/T 1034–2008) and solvent absorption (GB/T 1690–2010) were assessed at room temperature. 3. Results and discussion 3.1 Structure of S-H-Oil-PFCBAE Usually, polysiloxane is synthesized by the hydrolysis reaction of silicone or ring opening polymerization of cyclosiloxanes. In this work we synthesized S-H-Oil-PFCBAE by combining the two methods (Fig. 2 ). FTIR, 1 H NMR and 19 F NMR spectrum of S 4 were shown in Fig. 3 . Mn and the mol content of PFCBAE were shown in Table 3 . All the results illustrated the successful synthesis of S-H-Oil-PFCBAE. IR: 2176 cm − 1 (Si-H); 1587, 1500, 1406 cm − 1 (arC-C), 1025, 1080 cm − 1 (Si-O-Si). 1 H NMR: 7.10–7.60 (Ar), 4.60–4.70 (Si-H), 0.0-0.5 (Si-CH 3 ). 19 F NMR: -126~-132. Table 3 Mn and PDI of S 1 to S 5 PFCBAE content (x mol %) Mn (g/mol) PDI Theoretical Experiment* S 1 0 0 6086 1.55 S 2 1 0.9 5066 1.65 S 3 3 2.9 5177 1.68 S 4 5 4.8 5351 1.70 S 5 6.7 6.5 5221 1.71 * Determined by 1 H NMR 3.2 Properties of S-H-Oil-PFCBAE Table 4 The thermal properties of S 1 to S 5 * T g ( o C) T 5 ( o C) T 10 ( o C) T q ( o C) S 1 -119.2 220.3 269.2 475.2 S 2 -117.9 226.8 274.3 479.2 S 3 -117.8 230.9 280.1 479.9 S 4 -117.2 232.3 282.9 482.3 S 5 -117.0 231.8 281.6 480.2 * T g , the glass transition temperature; T 5 , the 5% weight loss temperature; T 10 , the 10% weight loss temperature; T q , the temperature at maximum weight loss rate S-H-Oil-PFCBAE was a new silicone oil, which had the PFCBAE group in the backbone and the hydrogen group in the pendant group. The thermal properties were investigated by DSC and TGA. The data were shown in Table 4 . T g of S-H-Oil-PFCBAE (S 2 , S 3 , S 4 , S 5 ) was similar to that of the reported polydimethylsiloxane(-125 to -100°C). [26, 27] However, T g of S-H-Oil-PFCBAE (S 2 , S 3 , S 4 , S 5 ) was a little higher than that of S 1 which was synthesized by the same method without the PFCBAE group in the backbone. The result illustrated that PFCBAE group in the backbone restricted the movement of the polymer chains. And it can also be found that the thermal stability of S-H-Oil-PFCBAE was superior to that of S 1 . In addition, with the increase of PFCBAE, the thermal stability showed an increasing trend, which implied that the introduce of PCFBAE could improve the thermal stability of S-H-Oil-PFCBAE. The irregular trend can attribute to the molecular weight. Besides the structure of the polymer, the length of the polymer also has an important effect on its properties. Moreover, the solubility behaviour of S-H-Oil-PFCBAE was listed in Table 5 . S-H-Oil-PFCBAE has a similar solubility compared to the hydrogen silicone oil (S 1 ), which is freely soluble in common solvents. Such a result implies that S-H-Oil-PFCBAE has an excellent solution processing performance, which probably has the potential application in the field of coating. Table 5 The solubility of S 1 to S 5 * 3.3 Vulcanization of fluorosilicone rubber Hydrosilylation reaction is a significant reaction in organosilicon chemistry, which utilizes an addition reaction between Si-H and Si-CH = CH 2 . The hydrosilylation reaction is also widely used as the vulcanization reaction at both high temperature and room temperature [ 17 – 22 ] . In the hydrosilylation vulcanization system, the hydrogen silicone oil that provides Si-H groups is the essential component as the crosslinker. In this work, S-H-Oil-PFCBAE which had both the PFCBAE group in the backbone and the hydrogen group in the pendant group was used as the crosslinker to achieve the vulcanization of fluorosilicone rubber (Fig. 1 ). 3.4 Mechanical properties of fluorosilicone rubber Table 6 The mechanical properties of P 1 to P 5 Sample Tensile strength (MPa) Tear strength (kN/m) Elongation at break (%) Hardness (ShA) P 1 9.42 44.59 804 69 P 2 9.86 29.96 844 70 P 3 10.10 30.98 729 71 P 4 10.94 28.70 854 71 P 5 10.95 28.57 900 71 As the most significant properties, the mechanical properties of the rubber reflect the comprehensive properties and are closely related to the other properties. And according to the mechanical properties, the potential application field of the rubber can be predicted. The influence factors of the mechanical properties of rubber are very complex, which is the comprehensive results of many factors such as the molecular structure of raw rubber, vulcanization state, reinforce effect, process condition and so on. The results of mechanical properties are showed in Table 6 . With the increase of PFCBAE, the tensile strength and the hardness increased, while the elongation at break and the tear strength decreased. The PFCBAE group which was a rigid structure increased the rigidity of the vulcanization system and reduced the toughness of the vulcanization system. The irregular trend with the increase of PFCBAE can be attributed to the effect of vulcanization state by the PFCBAE structure. 3.5 Thermal properties of fluorosilicone rubber The thermal properties of P 1 to P 5 were measured by DSC (Fig. 4 ) and TGA (Fig. 5 ). In Fig. 4 , the DSC traces of the samples containing PFCBAE (P 2 , P 3 , P 4 and P 5 ) were similar to that of the sample without PFCBAE (P 1 ). Such results illustrate that PFCBAE group has little effect on both the glass transition and the crystallization behavior of the vulcanizate. The influence of PFCBAE structure on the thermal stability of fluorosilicone rubber is complicated (Fig. 5 ). It should be considered the effects of both the PFCBAE structure and the chain length of S-H-Oil-PFCBAE. T 5 of all the samples was more than 400 o C, which illustrated that compared to -CH 2 CH 2 CF 3 structure PFCBAE structure did not damage the thermal stability of vulcanizate. In detail, T 5 of P 2 and P 3 was lower than that of P 1 , which can be attributed to the relatively short chain length of S-H-Oil-PFCBAE. In the thermal degradation process PFCBAE group could disrupt the ordering of molecular chain and restrict the backbite cyclization reaction. But the chain length of S 2 and S 3 was shorter than S 1 , which takes the dominate. Correspondingly, T 5 of P 4 and P 5 was higher than that of P 1 . It can be attributed to the relatively high content of PFCBAE, which takes the dominate. Interestingly, the residual char of P 2 , P 3 , P 4 and P 5 was higher than that of P 1 , which also improves that the PFCBAE group can generally restrict the thermal degradation process of fluorosilicone rubber. 3.6 Hydrophobic properties of fluorosilicone rubber The hydrophobicity of the vulcanizate was detected by the contact angle (Fig. 6) and the water absorption rate (Table 7 ). It was obviously found that with the increase of PFCBAE content from P 1 to P 5 , the contact angle of samples increased and the water absorption rate was decreased. All the results were simply attributed the hydrophobicity PFCBAE structure improved the hydrophobicity of silicone rubber. It was also noted that the water absorption rate of P 4 and P 5 was higher than that of P 2 and P 3 , which can be attributed to that the increase of PFCBAE content may affect the vulcanization system of the rubber. Table 7 The water absorption of P 1 to P 5 Sample P 1 P 2 P 3 P 4 P 5 Water absorption(%) 0.48 0.13 0.10 0.18 0.17 3.7 Solvent resistance of fluorosilicone rubber Table 8 The solvent absorption of P 1 to P 5 Sample Toluene Acetone THF P 1 120.1 20.1 153.8 P 2 112.7 12.8 145.2 P 3 117.8 13.7 145.9 P 4 116.9 14.5 146.6 P 5 118.9 14.3 147.1 The solvent resistance of P 1 to P 5 is shown in Table 8 . Toluene, acetone and THF were used to test the solvent resistance. Compared to the sample without PFCBAE (P 1 ), the samples with PFCBAE (P 2 , P 3 , P 4 , and P 5 ) have the lower absorption rate, which implies that the PFCBAE structure enhances the solvent resistance of rubber. However, there was an irregular rise of the mass change rate with the increase of PFCBAE. Similar to the mechanical properties and the hydrophobic properties, the vulcanization system was affected with the increase of PFCBAE group. And the solvent could permeate into the rubber. 4. Conclusions In summary, S-H-Oil-PFCBAE with the PFCBAE group in the backbone and the hydrogen group in the pendant group was first synthesized. And S-H-Oil-PFCBAE was used as the crosslinker to prepare a new kind of fluorosilicone rubber by the hydrosilylation addition reaction. We found that the PFCBAE structure could improve the tensile strength, the thermal stability, the hydrophobicity, and the solvent resistance of fluorosilicone rubber. Especially, compared to the traditional -CH 2 CH 2 CF 3 structure PFCBAE structure can improve the thermal stability of fluorosilicone rubber, which has a reference in enriching the types of fluorosilicone rubber and improving the performance of fluorosilicone rubber. But the PFCBAE group had some effect on the hydrosilylation vulcanization system. Declarations Ethics approval This study does not contain any human-related information and no animals were used. Consent to participate Consent was obtained from every researcher who participated in the experiment. Consent for publication All authors approved the version of the manuscript to be published. Availability of data and materials Research data are not shared. Competing interests The authors declare no conflict of interest. Funding and Acknowledgments This work was supported by the Natural Science Foundation of Shandong Province, China (ZR2023MB161), the National Natural Science Foundation of China (NSFC, No. 51603178), the open funds of the Shandong Key Laboratory of Advanced Organosilicon Materials and Technologies, the Foundation of Key Laboratory of Special Functional Aggregated Materials, Ministry of Education, P.R. China. Authors' contributions Shen Diao and Lele Huang wrote the main manuscript text. Lele Huang, Mingying Wang and Shen Diao did the experimental work. 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Hou, Enhanced ablation resistance of Divinyl-POSS modified additional liquid silicone rubber and its fiber reinforced composite, Polymer Composites, 2022, 43, 2896. https://doi.org/10.1002/pc.26585 Additional Declarations No competing interests reported. Cite Share Download PDF Status: Published Journal Publication published 18 Jun, 2024 Read the published version in Silicon → Version 1 posted Editorial decision: Revision requested 05 Jun, 2024 Reviews received at journal 05 Jun, 2024 Reviewers agreed at journal 05 Jun, 2024 Reviewers invited by journal 22 Apr, 2024 Submission checks completed at journal 22 Apr, 2024 Editor assigned by journal 22 Apr, 2024 First submitted to journal 04 Apr, 2024 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. 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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-4218684","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":295186375,"identity":"aed91524-8709-4386-8c27-b6e3df6e13a3","order_by":0,"name":"Lele Huang","email":"","orcid":"","institution":"Yantai University","correspondingAuthor":false,"prefix":"","firstName":"Lele","middleName":"","lastName":"Huang","suffix":""},{"id":295186377,"identity":"4e0a4dfe-9f41-48ab-b6a1-369601c22483","order_by":1,"name":"Mingying Wang","email":"","orcid":"","institution":"Yantai University","correspondingAuthor":false,"prefix":"","firstName":"Mingying","middleName":"","lastName":"Wang","suffix":""},{"id":295186378,"identity":"f6bb4bf4-88bd-4cb7-83f2-8fed7f68adaf","order_by":2,"name":"Yuqiang Zhang","email":"","orcid":"","institution":"Yantai University","correspondingAuthor":false,"prefix":"","firstName":"Yuqiang","middleName":"","lastName":"Zhang","suffix":""},{"id":295186380,"identity":"b36cc779-24a9-4c14-b163-e230d720939a","order_by":3,"name":"Shen Diao","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA3UlEQVRIiWNgGAWjYDCCw0DM2MDAIM/M//BBQkUNCVoM23mYDR6cOUaElgNQLQznedgkH7YwE9bBd5z54cOfO2zyGJt5j1UkNrAx8Ld3J+DVInmYzdiY90xaMTszX9qNxB0yDBJnzm7Aq8XgMIOZNGPb4cTGZgazG4ln2BgMJHIJaWH/Jvmz7X9iA1BvQWIbMzFaeMwkeNsOALXwmDEQpUXyME+xMW9bcuLGZrZkiYQzx3gI+oXv/PGND3+22SXO5z988OOPiho5/vZe/FowAA9pykfBKBgFo2AUYAUAZG9K1Asr4KwAAAAASUVORK5CYII=","orcid":"","institution":"Yantai University","correspondingAuthor":true,"prefix":"","firstName":"Shen","middleName":"","lastName":"Diao","suffix":""}],"badges":[],"createdAt":"2024-04-04 15:18:09","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-4218684/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-4218684/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1007/s12633-024-03066-w","type":"published","date":"2024-06-18T15:22:27+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":55384537,"identity":"053d9590-cade-4056-af96-2b1b1232493a","added_by":"auto","created_at":"2024-04-26 14:26:45","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":91232,"visible":true,"origin":"","legend":"\u003cp\u003ePreparation of fluorosilicone rubber\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-4218684/v1/dfb0118ec841be8ccda6a55d.png"},{"id":55384011,"identity":"936f13e8-1065-4a39-bcaa-cce4016a2ea9","added_by":"auto","created_at":"2024-04-26 14:18:45","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":13903,"visible":true,"origin":"","legend":"\u003cp\u003eThe synthesis of S-H-Oil-PFCBAE\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-4218684/v1/9d8cf1fa65a851cc22e89ac1.png"},{"id":55384006,"identity":"1ab0128a-ca98-46a7-8ac3-939475fdf079","added_by":"auto","created_at":"2024-04-26 14:18:45","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":24865,"visible":true,"origin":"","legend":"\u003cp\u003eFTIR and NMR spectrum of S\u003csub\u003e4 \u003c/sub\u003e(a: \u003csup\u003e1\u003c/sup\u003eH NMR, b: FTIR, c: \u003csup\u003e19\u003c/sup\u003eF NMR)\u003c/p\u003e","description":"","filename":"3.png","url":"https://assets-eu.researchsquare.com/files/rs-4218684/v1/beb516a5cbaeaa79a33db3c6.png"},{"id":55384008,"identity":"c9d9cb0c-dc74-4adf-a0d5-aa3d94092ab1","added_by":"auto","created_at":"2024-04-26 14:18:45","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":13236,"visible":true,"origin":"","legend":"\u003cp\u003eDSC traces of P\u003csub\u003e1\u003c/sub\u003e to P\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e","description":"","filename":"4.png","url":"https://assets-eu.researchsquare.com/files/rs-4218684/v1/94d8794d807d0eb126bcf437.png"},{"id":55384007,"identity":"9e643f10-b783-4541-a645-4a5a5ae0e654","added_by":"auto","created_at":"2024-04-26 14:18:45","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":10940,"visible":true,"origin":"","legend":"\u003cp\u003eTGA traces of P\u003csub\u003e1\u003c/sub\u003e to P\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e","description":"","filename":"5.png","url":"https://assets-eu.researchsquare.com/files/rs-4218684/v1/c4068f7ee0504bb83f41abcf.png"},{"id":55384009,"identity":"5fa7b667-09a6-4505-b75c-6e18dadc47a8","added_by":"auto","created_at":"2024-04-26 14:18:45","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":35372,"visible":true,"origin":"","legend":"\u003cp\u003eThe contact angels of P\u003csub\u003e1\u003c/sub\u003e to P\u003csub\u003e5\u003c/sub\u003e (a: P\u003csub\u003e1\u003c/sub\u003e; b: P\u003csub\u003e2\u003c/sub\u003e; c: P\u003csub\u003e3\u003c/sub\u003e; d: P\u003csub\u003e4\u003c/sub\u003e; e: P\u003csub\u003e5\u003c/sub\u003e)\u003c/p\u003e","description":"","filename":"6.png","url":"https://assets-eu.researchsquare.com/files/rs-4218684/v1/bd9b3abf439f3a75cb398fb1.png"},{"id":58823100,"identity":"196dcebf-2411-49a2-8dca-41600c33906f","added_by":"auto","created_at":"2024-06-21 16:53:10","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":889135,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-4218684/v1/9e2f4858-69a7-47a4-9b20-702b7528b221.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Preparation of High Temperature Vulcanized Fluorosilicone Rubber by Hydrosilylation Addition Reaction","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eFluorosilicone material which is a combination of Si-C bonds with the high bonding energy and C-F bonds which can play the role of shielding C-C bonds shows excellent performances. As the most significant product of the fluorosilicone material, fluorosilicone rubber was first launched in the 1950s (the commercial brand Silastic LS-53, Dow Corning). And then, fluorosilicone rubber has been widely applied in a variety of fields, including aerospace, automobiles, electronics, medicine and so on for the outstanding performances such as thermostable and cold resistance, environmental aging resistance, oil resistance and chemical corrosion resistance.\u003c/p\u003e \u003cp\u003eThe researchers have carried out many significative studies on the preparations and properties of fluorinesilicone rubber. Cui\u003csup\u003e[\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e]\u003c/sup\u003e successfully synthesized polyfluorosiloxane (just polymer not rubber) with different contents (12, 22, 29, and 38 mol%) of trifluoropropyl groups (-CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e) and the test results showed that the higher contents of -CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e group, the better solvent resistance and the lower the thermal stability of polyfluorosiloxane. Indelekha\u003csup\u003e[\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e, \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]\u003c/sup\u003e prepared fluorosilicone rubber (also -CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e group) cured in the hydrosilation system. And the vulcanizate exhibited not only excellent hydrophobicity and lipophobicity but also the acid resistance. Fei\u003csup\u003e[\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e]\u003c/sup\u003e synthesized fluorosilicone rubber (-CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e group). And the phenyl group was also introduced into the side chain. It was found that the phenyl group could improve the thermal stability and damping performance of the rubber. Xu used nano materials (including nano cerium dioxide\u003csup\u003e[\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]\u003c/sup\u003e, multi-walled carbon nanotube\u003csup\u003e[\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e]\u003c/sup\u003e and boron particle\u003csup\u003e[\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]\u003c/sup\u003e) as the fillers to prepare fluorosilicone rubber (-CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e group). The nano materials can increase the thermal decomposition temperature of the rubber. Xu\u003csup\u003e[\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]\u003c/sup\u003e used the vinyl fluorosilicone resin (-CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e group) containing imide which improves the thermal stability of the rubber as the crosslinker for fluorosilicone rubber. So\u003csup\u003e[\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e]\u003c/sup\u003e used the vinyl-functionalized POSS as the crosslinker to prepare fluorosilicone rubber (-CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e group), which also improves the thermal stability of the rubber. Tan \u003csup\u003e[\u003cspan additionalcitationids=\"CR11\" citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e]\u003c/sup\u003e used the nano-particles (the multiwalled carbon nanotubes (MWCNT), modified SiO\u003csub\u003e2\u003c/sub\u003e/MWCNT, and the graphene nanoplatelets/barium titanate hybrid nanoparticles) as the fillers to prepared fluorosilicone rubber (-CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e group). Besides the mechanical and the thermal properties, the dielectric property was also systematically investigated. Although the research on fluorosilicone rubber has made some great progress, it can be found that the fluorine group of fluorosilicone rubber is generally -CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e group. However, the -CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e group usually has bed effect on the performances of fluorosilicone rubber, particularly the thermal stability. As a result, it is needed to develop the methods to improve the thermal stability of fluorosilicone rubber. Generally, it is essential to develop some new types of fluorine structure to enrich the types of fluorosilicone rubber and investigate the effect of novel fluorine structure on the properties of the materials.\u003c/p\u003e \u003cp\u003eIn our previous work\u003csup\u003e[\u003cspan additionalcitationids=\"CR14\" citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]\u003c/sup\u003e, we reported two kinds of fluorosilicone rubber containing perfluorocyclobutyl aryl ether (PFCBAE) group. Fluorosilicone rubber containing PFCBAE was first vulcanized by the thermal cyclization reaction of trifluoroethylene aryl ether (TFVE) which was also a new vulcanization method. But we found the stability of TFVE was not very good, which lead to the low content of PFCBAE structure and the extreme reaction conditions. Further, we synthesized a vinyl silicone oil with PFCBAE group in the backbone which was so-called the centralized crosslinker for fluorosilicone rubber.\u003c/p\u003e \u003cp\u003eAs we all know, vulcanization is a critical process in rubber processing, and the comprehensive properties of rubber can be significantly improved through the vulcanization. The vulcanization of fluorosilicone rubber is the same as that of traditional silicone rubber. The high temperature vulcanization of fluorosilicone rubber is mainly accomplished by the traditional peroxide reaction which is suitable for vulcanization of most rubbers and the hydrosilylation addition reaction which is a special reaction in organosilicone chemistry. In the present work, we prepare fluorosilicone rubber containing PFCBAE group by hydrosilylation addition reaction. Hydrogen containing silicone oil containing PFCBAE group (S-H-Oil-PFCBAE) is firstly synthesized. And then S-H-Oil-PFCBAE is used as the crosslinker to prepare the fluorosilicone rubber. The overall process is shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. The synthesis of S-H-Oil-PFCBAE and the influences of S-H-Oil-PFCBAE on fluorosilicone rubber are investigated in this work.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e"},{"header":"2. Experimental","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1 Materials\u003c/h2\u003e \u003cp\u003eSilane with PFCBAE (M\u003csub\u003e4\u003c/sub\u003e) was synthesized in our lab according to the literature\u003csup\u003e[\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]\u003c/sup\u003e. Octamethylcyclotetrasiloxane (D\u003csub\u003e4\u003c/sub\u003e) was purchased from Guangzhou Skycent Chemicals Co., Ltd. Tetramethylcyclotetrasiloxane (D\u003csub\u003e4\u003c/sub\u003e\u003csup\u003eH\u003c/sup\u003e) was purchased from Jiande Juhe New Materials Co., Ltd. Hexamethyldisiloxane (MM) was purchased from Shanghai Gaoming Chemicals Co., Ltd. Base gum (110-2S, methylvinyl polysiloxane) was obtained by Dongjue Silicone Group Co., Limited. CAB-O-SIL-TS530 Fumed Silica was purchased from Cabot Corporation. Karstedt catalyst was synthesized in our lab according to the literature\u003csup\u003e[\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e]\u003c/sup\u003e.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2 Synthesis of S-H-Oil-PFCBAE\u003c/h2\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eAccording to the composition of S-H-Oil-PFCBAE listed in Table\u0026nbsp;1, D\u003csub\u003e4\u003c/sub\u003e, D\u003csub\u003e4\u003c/sub\u003e\u003csup\u003eH\u003c/sup\u003e, M\u003csub\u003e4\u003c/sub\u003e, and MM were mixed into the three-necked flask and were stirred vigorously at room temperature. And then concentrated sulfuric acid (4% weight of monomer) was added. The mixture was kept on stirring vigorously for 0.5 h and then 0.1g H\u003csub\u003e2\u003c/sub\u003eO was added and kept for 6 h. Another 0.1 g H\u003csub\u003e2\u003c/sub\u003eO and 20 mL toluene were added for 1 h. Then the mixture was washed with deionized H\u003csub\u003e2\u003c/sub\u003eO to the neutral and dried by Na\u003csub\u003e2\u003c/sub\u003eSO\u003csub\u003e4\u003c/sub\u003e. And the mixture was filtered. Finally, a yellow oily liquid was obtained after evaporating. The synthesis route was shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e.\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\u003eThe composition of S\u003csub\u003e1\u003c/sub\u003e to S\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"6\"\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 \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSample\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003ePFCBAE*\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eD\u003csub\u003e4\u003c/sub\u003e(g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eD\u003csub\u003e4\u003c/sub\u003e\u003csup\u003eH\u003c/sup\u003e(g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eM\u003csub\u003e4\u003c/sub\u003e(g)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c6\"\u003e \u003cp\u003eMM(g)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eS\u003csub\u003e1\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e0\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e12.88\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e18\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e0\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e0.85\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eS\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e11.06\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e20.73\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e2.76\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e0.95\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eS\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e2.41\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e7.75\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e2.76\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e0.33\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eS\u003csub\u003e4\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0.89\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e4.98\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e2.76\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e0.25\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eS\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e6.7\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e4.14\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e2.76\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c6\"\u003e \u003cp\u003e0.19\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003ctfoot\u003e \u003ctr\u003e\u003ctd colspan=\"6\"\u003e* mol content %\u003c/td\u003e\u003c/tr\u003e \u003c/tfoot\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3 Preparation of fluorosilicone rubber\u003c/h2\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\u003eThe composition of P\u003csub\u003e1\u003c/sub\u003e to P5*\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"5\"\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=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSample\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eBase gum\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eFumed silica\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eKarstedt catalyst\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS-H-Oil-PFCBAE\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP\u003csub\u003e1\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e100\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS\u003csub\u003e1\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e100\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e100\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP\u003csub\u003e4\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e100\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS\u003csub\u003e4\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e100\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e60\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0.5\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eS\u003csub\u003e5\u003c/sub\u003e\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* All components are by weight as phr. The dosage of S-H-Oil-PFCBAE is 5 phr.\u003c/p\u003e \u003cp\u003eThe base gum was milled on a two-roll mill for 5\u0026ndash;10 min. The fumed silica was added in batches for 30\u0026ndash;40 min. The rubber was kept on milling for another 10 min after uniformly mixed. Then the rubber was kept in an air-dry oven at 160 \u003csup\u003eo\u003c/sup\u003eC for 1 h. The rubber was cooled to room temperature and remilled. Then S-H-Oil-PFCBAE (S\u003csub\u003e1\u003c/sub\u003e, S\u003csub\u003e2\u003c/sub\u003e, S\u003csub\u003e3\u003c/sub\u003e, S\u003csub\u003e4\u003c/sub\u003e, S\u003csub\u003e5\u003c/sub\u003e) were added in batches for 5 min. After uniformly mixed, Karstedt catalyst was added. The rubber was vulcanized in the mold at 160 \u003csup\u003eo\u003c/sup\u003eC under a pressure of 15 MPa for 10 min and then postcured at 160 \u003csup\u003eo\u003c/sup\u003eC for 2 h under ambient pressure to obtain the final vulcanizates. The composition of fluorosilicone rubber is listed in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e2.4 Characterization and measurements\u003c/h2\u003e \u003cp\u003eFTIR spectra were measured by IR spectrometer (Shimadzu IRAffinity-1S). \u003csup\u003e1\u003c/sup\u003eH NMR and \u003csup\u003e19\u003c/sup\u003eF NMR spectra were measured by NMR instrument (JEOL 400YH, CDCl\u003csub\u003e3\u003c/sub\u003e). Molecular weights were determined by GPC (Waters 1515). DSC was measured by Netzsch Instrument (DSC 200F3). TGA was measured by TG 209F3 instrument under nitrogen. The tensile testing (ASTM D 412 method and ISO 527) and the tear testing (QB/T 1130\u0026ndash;1991) were carried out by an electronic universal testing machine (UTM4103). Hardness (ASTM D 2240 method) was measured by durometer (Shore A). Water contact angle was determined by contact angle measuring instrument (JC2000C). Water absorption (GB/T 1034\u0026ndash;2008) and solvent absorption (GB/T 1690\u0026ndash;2010) were assessed at room temperature.\u003c/p\u003e \u003c/div\u003e"},{"header":"3. Results and discussion","content":"\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e\n \u003ch2\u003e3.1 Structure of S-H-Oil-PFCBAE\u003c/h2\u003e\n \u003cp\u003eUsually, polysiloxane is synthesized by the hydrolysis reaction of silicone or ring opening polymerization of cyclosiloxanes. In this work we synthesized S-H-Oil-PFCBAE by combining the two methods (Fig. \u003cspan class=\"InternalRef\"\u003e2\u003c/span\u003e). FTIR, \u003csup\u003e1\u003c/sup\u003eH NMR and \u003csup\u003e19\u003c/sup\u003eF NMR spectrum of S\u003csub\u003e4\u003c/sub\u003e were shown in Fig. \u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003e. Mn and the mol content of PFCBAE were shown in Table \u003cspan class=\"InternalRef\"\u003e3\u003c/span\u003e. All the results illustrated the successful synthesis of S-H-Oil-PFCBAE.\u003c/p\u003e\n \u003cp\u003eIR: 2176 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e (Si-H); 1587, 1500, 1406 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e (arC-C), 1025, 1080 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e(Si-O-Si).\u003c/p\u003e\n \u003cp\u003e\u003csup\u003e1\u003c/sup\u003eH NMR: 7.10\u0026ndash;7.60 (Ar), 4.60\u0026ndash;4.70 (Si-H), 0.0-0.5 (Si-CH\u003csub\u003e3\u003c/sub\u003e).\u003c/p\u003e\n \u003cp\u003e\u003csup\u003e19\u003c/sup\u003eF NMR: -126~-132.\u003c/p\u003e\n \u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u003ctable id=\"Tab3\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 3\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003eMn and PDI of S\u003csub\u003e1\u003c/sub\u003e to S\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003ccolgroup cols=\"5\"\u003e\u003c/colgroup\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\" rowspan=\"2\"\u003e\u0026nbsp;\u003c/th\u003e\n \u003cth align=\"left\" colspan=\"2\"\u003e\n \u003cp\u003ePFCBAE content (x mol %)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\" rowspan=\"2\"\u003e\n \u003cp\u003eMn\u003c/p\u003e\n \u003cp\u003e(g/mol)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\" rowspan=\"2\"\u003e\n \u003cp\u003ePDI\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eTheoretical\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eExperiment*\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eS\u003csub\u003e1\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e6086\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.55\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eS\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e5066\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.65\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eS\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e2.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e5177\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.68\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eS\u003csub\u003e4\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e4.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e5351\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.70\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eS\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e6.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e6.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e5221\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e1.71\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003ctfoot\u003e\n \u003ctr\u003e\n \u003ctd colspan=\"5\"\u003e* Determined by \u003csup\u003e1\u003c/sup\u003eH NMR\u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tfoot\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec9\" class=\"Section2\"\u003e\n \u003ch2\u003e3.2 Properties of S-H-Oil-PFCBAE\u003c/h2\u003e\n \u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u003ctable id=\"Tab4\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 4\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003eThe thermal properties of S\u003csub\u003e1\u003c/sub\u003e to S\u003csub\u003e5\u003c/sub\u003e *\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003ccolgroup cols=\"5\"\u003e\u003c/colgroup\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\u0026nbsp;\u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eT\u003csub\u003eg\u003c/sub\u003e (\u003csup\u003eo\u003c/sup\u003eC)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eT\u003csub\u003e5\u003c/sub\u003e (\u003csup\u003eo\u003c/sup\u003eC)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eT\u003csub\u003e10\u003c/sub\u003e (\u003csup\u003eo\u003c/sup\u003eC)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eT\u003csub\u003eq\u003c/sub\u003e (\u003csup\u003eo\u003c/sup\u003eC)\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eS\u003csub\u003e1\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e-119.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e220.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e269.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e475.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eS\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e-117.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e226.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e274.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e479.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eS\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e-117.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e230.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e280.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e479.9\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eS\u003csub\u003e4\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e-117.2\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e232.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e282.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e482.3\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eS\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e-117.0\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e231.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e281.6\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e480.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003ctfoot\u003e\n \u003ctr\u003e\n \u003ctd colspan=\"5\"\u003e* T\u003csub\u003eg\u003c/sub\u003e, the glass transition temperature; T\u003csub\u003e5\u003c/sub\u003e, the 5% weight loss temperature; T\u003csub\u003e10\u003c/sub\u003e, the 10% weight loss temperature; T\u003csub\u003eq\u003c/sub\u003e, the temperature at maximum weight loss rate\u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tfoot\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n \u003cp\u003eS-H-Oil-PFCBAE was a new silicone oil, which had the PFCBAE group in the backbone and the hydrogen group in the pendant group. The thermal properties were investigated by DSC and TGA. The data were shown in Table \u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003e. T\u003csub\u003eg\u003c/sub\u003e of S-H-Oil-PFCBAE (S\u003csub\u003e2\u003c/sub\u003e, S\u003csub\u003e3\u003c/sub\u003e, S\u003csub\u003e4\u003c/sub\u003e, S\u003csub\u003e5\u003c/sub\u003e) was similar to that of the reported polydimethylsiloxane(-125 to -100\u0026deg;C).\u003csup\u003e[26, 27]\u003c/sup\u003e However, T\u003csub\u003eg\u003c/sub\u003e of S-H-Oil-PFCBAE (S\u003csub\u003e2\u003c/sub\u003e, S\u003csub\u003e3\u003c/sub\u003e, S\u003csub\u003e4\u003c/sub\u003e, S\u003csub\u003e5\u003c/sub\u003e) was a little higher than that of S\u003csub\u003e1\u003c/sub\u003e which was synthesized by the same method without the PFCBAE group in the backbone. The result illustrated that PFCBAE group in the backbone restricted the movement of the polymer chains. And it can also be found that the thermal stability of S-H-Oil-PFCBAE was superior to that of S\u003csub\u003e1\u003c/sub\u003e. In addition, with the increase of PFCBAE, the thermal stability showed an increasing trend, which implied that the introduce of PCFBAE could improve the thermal stability of S-H-Oil-PFCBAE. The irregular trend can attribute to the molecular weight. Besides the structure of the polymer, the length of the polymer also has an important effect on its properties.\u003c/p\u003e\n \u003cp\u003eMoreover, the solubility behaviour of S-H-Oil-PFCBAE was listed in Table \u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003e. S-H-Oil-PFCBAE has a similar solubility compared to the hydrogen silicone oil (S\u003csub\u003e1\u003c/sub\u003e), which is freely soluble in common solvents. Such a result implies that S-H-Oil-PFCBAE has an excellent solution processing performance, which probably has the potential application in the field of coating.\u003c/p\u003e\n \u003cp\u003eTable 5 The solubility of S\u003csub\u003e1\u003c/sub\u003e to S\u003csub\u003e5\u003c/sub\u003e *\u003c/p\u003e\n \u003cp\u003e\u003cimg 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\"\u003e\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec10\" class=\"Section2\"\u003e\n \u003ch2\u003e3.3 Vulcanization of fluorosilicone rubber\u003c/h2\u003e\n \u003cp\u003eHydrosilylation reaction is a significant reaction in organosilicon chemistry, which utilizes an addition reaction between Si-H and Si-CH\u0026thinsp;\u003cstrong\u003e=\u003c/strong\u003e\u0026thinsp;CH\u003csub\u003e2\u003c/sub\u003e. The hydrosilylation reaction is also widely used as the vulcanization reaction at both high temperature and room temperature \u003csup\u003e[\u003cspan class=\"CitationRef\"\u003e17\u003c/span\u003e\u0026ndash;\u003cspan class=\"CitationRef\"\u003e22\u003c/span\u003e]\u003c/sup\u003e. In the hydrosilylation vulcanization system, the hydrogen silicone oil that provides Si-H groups is the essential component as the crosslinker. In this work, S-H-Oil-PFCBAE which had both the PFCBAE group in the backbone and the hydrogen group in the pendant group was used as the crosslinker to achieve the vulcanization of fluorosilicone rubber (Fig. \u003cspan class=\"InternalRef\"\u003e1\u003c/span\u003e).\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec11\" class=\"Section2\"\u003e\n \u003ch2\u003e3.4 Mechanical properties of fluorosilicone rubber\u003c/h2\u003e\n \u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u003ctable id=\"Tab6\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 6\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003eThe mechanical properties of P\u003csub\u003e1\u003c/sub\u003e to P\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003ccolgroup cols=\"5\"\u003e\u003c/colgroup\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eSample\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eTensile strength\u003c/p\u003e\n \u003cp\u003e(MPa)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eTear strength (kN/m)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eElongation at break\u003c/p\u003e\n \u003cp\u003e(%)\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eHardness\u003c/p\u003e\n \u003cp\u003e(ShA)\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e1\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e9.42\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e44.59\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e804\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e69\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e9.86\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e29.96\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e844\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e70\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.10\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e30.98\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e729\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e71\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e4\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.94\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e28.70\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e854\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e71\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e10.95\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e28.57\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e900\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e71\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n \u003cp\u003eAs the most significant properties, the mechanical properties of the rubber reflect the comprehensive properties and are closely related to the other properties. And according to the mechanical properties, the potential application field of the rubber can be predicted. The influence factors of the mechanical properties of rubber are very complex, which is the comprehensive results of many factors such as the molecular structure of raw rubber, vulcanization state, reinforce effect, process condition and so on. The results of mechanical properties are showed in Table \u003cspan class=\"InternalRef\"\u003e6\u003c/span\u003e. With the increase of PFCBAE, the tensile strength and the hardness increased, while the elongation at break and the tear strength decreased. The PFCBAE group which was a rigid structure increased the rigidity of the vulcanization system and reduced the toughness of the vulcanization system. The irregular trend with the increase of PFCBAE can be attributed to the effect of vulcanization state by the PFCBAE structure.\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec12\" class=\"Section2\"\u003e\n \u003ch2\u003e3.5 Thermal properties of fluorosilicone rubber\u003c/h2\u003e\n \u003cp\u003eThe thermal properties of P\u003csub\u003e1\u003c/sub\u003e to P\u003csub\u003e5\u003c/sub\u003e were measured by DSC (Fig. \u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003e) and TGA (Fig. \u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003e). In Fig. \u003cspan class=\"InternalRef\"\u003e4\u003c/span\u003e, the DSC traces of the samples containing PFCBAE (P\u003csub\u003e2\u003c/sub\u003e, P\u003csub\u003e3\u003c/sub\u003e, P\u003csub\u003e4\u003c/sub\u003e and P\u003csub\u003e5\u003c/sub\u003e) were similar to that of the sample without PFCBAE (P\u003csub\u003e1\u003c/sub\u003e). Such results illustrate that PFCBAE group has little effect on both the glass transition and the crystallization behavior of the vulcanizate. The influence of PFCBAE structure on the thermal stability of fluorosilicone rubber is complicated (Fig. \u003cspan class=\"InternalRef\"\u003e5\u003c/span\u003e). It should be considered the effects of both the PFCBAE structure and the chain length of S-H-Oil-PFCBAE. T\u003csub\u003e5\u003c/sub\u003e of all the samples was more than 400 \u003csup\u003eo\u003c/sup\u003eC, which illustrated that compared to -CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e structure PFCBAE structure did not damage the thermal stability of vulcanizate. In detail, T\u003csub\u003e5\u003c/sub\u003e of P\u003csub\u003e2\u003c/sub\u003e and P\u003csub\u003e3\u003c/sub\u003e was lower than that of P\u003csub\u003e1\u003c/sub\u003e, which can be attributed to the relatively short chain length of S-H-Oil-PFCBAE. In the thermal degradation process PFCBAE group could disrupt the ordering of molecular chain and restrict the backbite cyclization reaction. But the chain length of S\u003csub\u003e2\u003c/sub\u003e and S\u003csub\u003e3\u003c/sub\u003e was shorter than S\u003csub\u003e1\u003c/sub\u003e, which takes the dominate. Correspondingly, T\u003csub\u003e5\u003c/sub\u003e of P\u003csub\u003e4\u003c/sub\u003e and P\u003csub\u003e5\u003c/sub\u003e was higher than that of P\u003csub\u003e1\u003c/sub\u003e. It can be attributed to the relatively high content of PFCBAE, which takes the dominate. Interestingly, the residual char of P\u003csub\u003e2\u003c/sub\u003e, P\u003csub\u003e3\u003c/sub\u003e, P\u003csub\u003e4\u003c/sub\u003e and P\u003csub\u003e5\u003c/sub\u003e was higher than that of P\u003csub\u003e1\u003c/sub\u003e, which also improves that the PFCBAE group can generally restrict the thermal degradation process of fluorosilicone rubber.\u003c/p\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec13\" class=\"Section2\"\u003e\n \u003ch2\u003e3.6 Hydrophobic properties of fluorosilicone rubber\u003c/h2\u003e\n \u003cp\u003eThe hydrophobicity of the vulcanizate was detected by the contact angle (Fig. 6) and the water absorption rate (Table \u003cspan class=\"InternalRef\"\u003e7\u003c/span\u003e). It was obviously found that with the increase of PFCBAE content from P\u003csub\u003e1\u003c/sub\u003e to P\u003csub\u003e5\u003c/sub\u003e, the contact angle of samples increased and the water absorption rate was decreased. All the results were simply attributed the hydrophobicity PFCBAE structure improved the hydrophobicity of silicone rubber. It was also noted that the water absorption rate of P\u003csub\u003e4\u003c/sub\u003e and P\u003csub\u003e5\u003c/sub\u003e was higher than that of P\u003csub\u003e2\u003c/sub\u003e and P\u003csub\u003e3\u003c/sub\u003e, which can be attributed to that the increase of PFCBAE content may affect the vulcanization system of the rubber.\u003c/p\u003e\n \u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u003ctable id=\"Tab7\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 7\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003eThe water absorption of P\u003csub\u003e1\u003c/sub\u003e to P\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003ccolgroup cols=\"6\"\u003e\u003c/colgroup\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eSample\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e1\u003c/sub\u003e\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e4\u003c/sub\u003e\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eWater absorption(%)\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.48\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.13\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.10\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.18\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003e0.17\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n\u003c/div\u003e\n\u003cdiv id=\"Sec14\" class=\"Section2\"\u003e\n \u003ch2\u003e3.7 Solvent resistance of fluorosilicone rubber\u003c/h2\u003e\n \u003cdiv class=\"gridtable\"\u003e\u0026nbsp;\u003ctable id=\"Tab8\" border=\"1\"\u003e\n \u003ccaption language=\"En\"\u003e\n \u003cdiv class=\"CaptionNumber\"\u003eTable 8\u003c/div\u003e\n \u003cdiv class=\"CaptionContent\"\u003e\n \u003cp\u003eThe solvent absorption of P\u003csub\u003e1\u003c/sub\u003e to P\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e\n \u003c/div\u003e\n \u003c/caption\u003e\n \u003ccolgroup cols=\"4\"\u003e\u003c/colgroup\u003e\n \u003cthead\u003e\n \u003ctr\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eSample\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eToluene\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eAcetone\u003c/p\u003e\n \u003c/th\u003e\n \u003cth align=\"left\"\u003e\n \u003cp\u003eTHF\u003c/p\u003e\n \u003c/th\u003e\n \u003c/tr\u003e\n \u003c/thead\u003e\n \u003ctbody\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e1\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e120.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e20.1\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e153.8\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e112.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e12.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e145.2\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e3\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e117.8\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e13.7\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e145.9\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e4\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e116.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e14.5\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e146.6\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003ctr\u003e\n \u003ctd align=\"left\"\u003e\n \u003cp\u003eP\u003csub\u003e5\u003c/sub\u003e\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e118.9\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e14.3\u003c/p\u003e\n \u003c/td\u003e\n \u003ctd align=\"char\"\u003e\n \u003cp\u003e147.1\u003c/p\u003e\n \u003c/td\u003e\n \u003c/tr\u003e\n \u003c/tbody\u003e\n \u003c/table\u003e\n \u003c/div\u003e\n \u003cp\u003eThe solvent resistance of P\u003csub\u003e1\u003c/sub\u003e to P\u003csub\u003e5\u003c/sub\u003e is shown in Table \u003cspan class=\"InternalRef\"\u003e8\u003c/span\u003e. Toluene, acetone and THF were used to test the solvent resistance. Compared to the sample without PFCBAE (P\u003csub\u003e1\u003c/sub\u003e), the samples with PFCBAE (P\u003csub\u003e2\u003c/sub\u003e, P\u003csub\u003e3\u003c/sub\u003e, P\u003csub\u003e4\u003c/sub\u003e, and P\u003csub\u003e5\u003c/sub\u003e) have the lower absorption rate, which implies that the PFCBAE structure enhances the solvent resistance of rubber. However, there was an irregular rise of the mass change rate with the increase of PFCBAE. Similar to the mechanical properties and the hydrophobic properties, the vulcanization system was affected with the increase of PFCBAE group. And the solvent could permeate into the rubber.\u003c/p\u003e\n\u003c/div\u003e"},{"header":"4. Conclusions","content":"\u003cp\u003e\u0026nbsp; \u0026nbsp; \u0026nbsp; \u0026nbsp; \u0026nbsp;In summary, S-H-Oil-PFCBAE with the PFCBAE group in the backbone and the hydrogen group in the pendant group was first synthesized. And S-H-Oil-PFCBAE was used as the crosslinker to prepare a new kind of fluorosilicone rubber by the hydrosilylation addition reaction. We found that the PFCBAE structure could improve the tensile strength, the thermal stability, the hydrophobicity, and the solvent resistance of fluorosilicone rubber. Especially, compared to the traditional -CH\u003csub\u003e2\u003c/sub\u003eCH\u003csub\u003e2\u003c/sub\u003eCF\u003csub\u003e3\u003c/sub\u003e structure PFCBAE structure can improve the thermal stability of fluorosilicone rubber, which has a reference in enriching the types of fluorosilicone rubber and improving the performance of fluorosilicone rubber. But the PFCBAE group had some effect on the hydrosilylation vulcanization system.\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e\u003cbr\u003e\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eEthics approval\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThis study does not contain any human-related information and no animals were used.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConsent to participate\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eConsent was obtained from every researcher who participated in the experiment.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConsent for publication\u0026nbsp;\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eAll authors approved the version of the manuscript to be published.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAvailability of data and materials\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eResearch data are not shared.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eCompeting interests\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors declare no conflict of interest.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eFunding and Acknowledgments\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThis work was supported by the Natural Science Foundation of Shandong Province, China (ZR2023MB161), the National Natural Science Foundation of China (NSFC, No. 51603178), the open funds of the Shandong Key Laboratory of Advanced Organosilicon Materials and Technologies, the Foundation of Key Laboratory of Special Functional Aggregated Materials, Ministry of Education, P.R. China.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthors' contributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eShen Diao and Lele Huang wrote the main manuscript text. Lele Huang, Mingying Wang and Shen Diao did the experimental work. Yuqiang Zhang prepared the figures. All authors reviewed the manuscript.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n \u003cli\u003eY. Cui, W. Jiang, D. Li, C. Niu, S. Feng, Preparation and properties of fluorosilicone and fluorosilicone elastomer with various contents of trifluoropropyl groups, e-Polymers, 2011,11, 27. https://doi.org/10.1515/epoly.2011.11.1.302.\u003c/li\u003e\n \u003cli\u003eK. Indulekha, P.K. Behera, R.S. Rajeev, C. Gouri, K.N. Ninan, Polyfluoroalkyl siloxanes with varying trifluoropropyl content: Synthesis, characterization and solvent resistance studies, Journal of Fluorine Chemistry, 2017, 200, 24-32. https://doi.org/10.1016/j.jfluchem.2017.05.007.\u003c/li\u003e\n \u003cli\u003eK. Indulekha, A. 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Hou, Enhanced ablation resistance of Divinyl-POSS modified additional liquid silicone rubber and its fiber reinforced composite, Polymer Composites, 2022, 43, 2896. https://doi.org/10.1002/pc.26585\u003c/li\u003e\n\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":"silicon","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"scon","sideBox":"Learn more about [Silicon](https://www.springer.com/journal/12633)","snPcode":"12633","submissionUrl":"https://submission.nature.com/new-submission/12633/3","title":"Silicon","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"fluorosilicone rubber, perfluorocyclobutyl, hydrosilylation addition reaction","lastPublishedDoi":"10.21203/rs.3.rs-4218684/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-4218684/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eFluorsilicone rubber as a new type of special functional rubber has attracted attention, which combines the advantages of the organic silicone materials and the organic fluorine materials. Herein, we reported fluorosilicone rubber vulcanized at high temperature by the hydrosilylation addition reaction. The silicone oil containing hydrogen in the pendant group and the perfluorocyclobutyl aryl ether (PFCBAE) group in the backbone (S-H-Oil-PFCBAE) was prepared by the hydrolytic polycondensation and ring opening reaction of silane with PFCBAE (M\u003csub\u003e4\u003c/sub\u003e), octamethylcyclotetrasiloxane (D\u003csub\u003e4\u003c/sub\u003e), and tetramethylcyclotetrasiloxane (D\u003csub\u003e4\u003c/sub\u003e\u003csup\u003eH\u003c/sup\u003e) by the traditional catalysis of concentrated sulfuric acid. And S-H-Oil-PFCBAE was used as the crosslinker to vulcanize fluorosilicone rubber. The mechanical property, the thermal stability, the hydrophobicity, and the solvent resistance of vulcanizates were studied in detail. The result showed that S-H-Oil-PFCBAE could improve the comprehensive performances of fluorosilicone rubber.\u003c/p\u003e","manuscriptTitle":"Preparation of High Temperature Vulcanized Fluorosilicone Rubber by Hydrosilylation Addition Reaction","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-04-26 14:18:40","doi":"10.21203/rs.3.rs-4218684/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2024-06-06T00:07:57+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-06-05T16:30:52+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"293928098929537303483221084037556403235","date":"2024-06-05T12:17:27+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2024-04-23T01:10:10+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2024-04-23T00:59:59+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2024-04-23T00:59:59+00:00","index":"","fulltext":""},{"type":"submitted","content":"Silicon","date":"2024-04-04T15:16:51+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"silicon","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"scon","sideBox":"Learn more about [Silicon](https://www.springer.com/journal/12633)","snPcode":"12633","submissionUrl":"https://submission.nature.com/new-submission/12633/3","title":"Silicon","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"dab3831f-ca52-4153-adfe-5e659401919a","owner":[],"postedDate":"April 26th, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2024-06-21T15:22:27+00:00","versionOfRecord":{"articleIdentity":"rs-4218684","link":"https://doi.org/10.1007/s12633-024-03066-w","journal":{"identity":"silicon","isVorOnly":false,"title":"Silicon"},"publishedOn":"2024-06-18 15:22:27","publishedOnDateReadable":"June 18th, 2024"},"versionCreatedAt":"2024-04-26 14:18:40","video":"","vorDoi":"10.1007/s12633-024-03066-w","vorDoiUrl":"https://doi.org/10.1007/s12633-024-03066-w","workflowStages":[]},"version":"v1","identity":"rs-4218684","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-4218684","identity":"rs-4218684","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}