本文選題：含氟硅氧烷　切入點：氟硅橡膠　出處：《煙臺大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：有機硅材料具有優(yōu)異的耐高低溫、耐輻射、耐腐蝕、電氣絕緣、憎水等性能,因此被廣泛應(yīng)用于電子電氣、紡織、醫(yī)療、建筑、機械等各行各業(yè)。隨著時代的發(fā)展,對有機硅材料也提出了更高的要求,從而推動了有機硅材料的發(fā)展。本文基于有機硅材料,在前人研究的基礎(chǔ)上,開展了以下三部分研究內(nèi)容:(1)進行了含氟硅氧烷的合成、聚含氟硅氧烷的合成、氟硅橡膠的硫化。利用FT-IR、1H-NMR、29Si-NMR對所得化合物進行了結(jié)構(gòu)表征,并探索了含氟硅烷最佳合成單體比例、不同氟含量聚氟硅氧烷的聚合、氟硅橡膠最佳硫化條件,考察了硫化后氟硅橡膠力學(xué)性能、耐老化性能、耐溶劑性能。結(jié)果表明,通過硅氫加成的方法將含氟烯丙基醚接到八甲基環(huán)四硅氧烷中,在n氟單體:n硅單體=10:1,溶劑為反應(yīng)體系的兩倍時,有利于硅氫加成反應(yīng)的進行。經(jīng)FT-IR、1H-NMR、29Si-NMR分析,Si-H鍵完全消失,產(chǎn)物收率高達99%以上。將含氟環(huán)硅氧烷、八甲基環(huán)四硅氧烷、四乙烯基四甲基環(huán)四硅氧烷通過四甲基氫氧化銨硅醇鹽作為催化劑進行開環(huán)聚合,當(dāng)四甲基氫氧化銨為0.03%時有利于聚合物分子量達到最大值。聚氟硅氧烷的硫化需在硫化劑雙二五與DCP共同作用下于150~160℃,20~25min完成。其含氟硅氧烷鏈節(jié)達到5%時,表面能最低。將有無進行二段硫化的氟硅橡膠進行力學(xué)性能對比測試,經(jīng)驗證得二段硫化有利于橡膠力學(xué)性能的提高。(2)端含氫硅油硅氫加成反應(yīng)活性。通過FT-IR、1H-NMR、29Si-NMR表征確認了不同鏈節(jié)長度端含氫結(jié)構(gòu)的基礎(chǔ)上,采用固化反應(yīng)、示差掃描量熱分析(DSC)等方法研究了系列含氫低聚硅氧烷產(chǎn)物的硅氫加成反應(yīng)活性。經(jīng)測定固化反應(yīng)時間及DSC的方法驗證,對于含不同鏈節(jié)數(shù)的二甲基硅基封端的二苯基硅氧烷低聚物來說,隨著-Si(Ph)2-鏈節(jié)數(shù)目的增加,低聚物硅氫加成的反應(yīng)活性逐步降低。(3)支化硅油的研究。以有機硅單體工業(yè)副產(chǎn)  甲基苯基二甲氧基硅烷(D)/苯基三甲氧基硅烷(T)共混物為原料,通過酸性條件下水解,堿性條件下縮合、平衡反應(yīng),合成含乙烯基的“T”型支化乙烯基硅油。根據(jù)不同批次DT副產(chǎn)物各單體含量不同進行單體比例調(diào)節(jié),經(jīng)FT-IR、1H-NMR、29Si-NMR等測試證明,得到了所需結(jié)構(gòu)產(chǎn)物,合成工藝穩(wěn)定。合成產(chǎn)物用于封裝膠組份,并進行了性能測試,結(jié)果表明性能優(yōu)良。
[Abstract]:Silicone materials have excellent resistance to high and low temperature, radiation resistance, corrosion resistance, electrical insulation, hydrophobicity and so on, so they are widely used in electronic and electrical, textile, medical, construction, machinery and other industries. With the development of the times, The development of organosilicon materials has been promoted. Based on silicone materials and based on previous studies, the synthesis of fluorosiloxane has been carried out in the following three parts: 1). Synthesis of polyfluorosiloxane and vulcanization of fluorosilicone rubber. The structure of the compound was characterized by FT-IRN 1H-NMR-29Si-NMR. The optimum synthetic monomer ratio of fluorosilane, polymerization of polyfluorosiloxane with different fluorine content, and optimum curing conditions of fluorinated silicone rubber were explored. The mechanical properties, aging resistance and solvent resistance of vulcanized fluorosilicone rubber were investigated. The results showed that fluoroallyl ethers were connected to octamethylcyclotetrasiloxane by hydrosilylation. When n: n monomer 10: 1, the solvent is twice as the reaction system, the addition reaction of hydrosilyl is advantageous. By FT-IRN 1H-NMR-29Si-NMR analysis, the bond of Si-H disappears completely and the yield of the product reaches more than 99%. The fluorinated cyclosiloxane, octamethylcyclotetrasiloxane, octamethylcyclosiloxane, and tetrasiloxane are obtained by FT-IR and 1H-NMR-29Si-NMR analysis. The ring-opening polymerization of tetravinyltetramethylcyclotetrasiloxane was carried out by using tetramethyl ammonium hydroxide as the catalyst. When tetramethylammonium hydroxide is 0.03, the molecular weight of polyfluorosiloxane can reach its maximum. The vulcanization of polyfluorosiloxane should be completed at 150 鈩，

本文編號：1607677