乙酰氧基硅烷收率和纯度的研究

介绍了采用分馏技术合成乙酰氧基硅烷的方法,讨论了几种不同的分馏柱对产物收率和纯度的影响,使合成甲基三乙酰氧基硅烷的收率达到９５％,纯度达到９８％;二甲基二乙酰氧基硅烷收率达到８２％。     

介孔分子筛SBA-15的乙基化修饰和表征

以乙基三乙氧基硅烷（ethanetriethoxy silane,其分子式为C2H5-Si（OC2H5）3）为偶联制,将乙基官能团接枝于SBA-15介孔分子筛孔道中,制备了无机-有机复合介孔材料C2H5-SBA-15,川小角X射线衍射,N2气吸附-脱附,元素分析,红外光谱和滴定法对复合材料进行了表征。结果表明,乙基有机基团不仅成功被接枝到了SBA-15孔道中,而月．保持了SBA-15的有序孔道结构。由于非极性官能团乙基的引入,使得合成的复合介孔材料具有很强的疏水性     

合成甲基三乙酰氧基硅烷的研究

本文提出了由甲基三氯硅烷和醋酐反应制备一种硅烷偶联剂－甲基三乙酰氧基硅烷。本文论述了对合成工艺的研究及对合成中有重要影响因素的研究过程。     

乙酰氧基硅烷收率和纯度的研究

介绍了采用分馏技术合成乙酰氧基硅烷的方法，讨论了几种不同的分馏柱对产物收率和纯度的影响，使合成甲基三乙酰氧基硅烷的利用达到９５％，纯度达到９８％，二甲基二乙酰氧基硅烷收率达到８２％。     

β-(3,4-环氧环己基)乙基三甲氧基硅烷的合成研究

以三甲氧基硅烷与4-乙烯基环氧环己烷为原料、氯铂酸-吩噻嗪-三苯基磷异丙醇溶液为催化剂,通过硅氢加成反应得β-(3,4-环氧环己基)乙基三甲氧基硅烷,讨论了影响硅氢加成反应的主要因素。最佳合成工艺:铂的质量分数为3×10-6、反应温度95~105℃、反应时间为1.5 h、原料配比三甲氧基硅烷/4-乙烯基环氧环己烷的量之比为1.05,在此条件下β-(3,4-环氧环己基)乙基三甲氧基硅烷的收率达92.3%。     

氰乙基三氯硅烷衍生物改性玻璃纤维增强PA6的应用及性能表征

以氰乙基三氯硅烷为初始反应物合成氰乙基三乙酰氧基硅烷(N1-A),并将其应用于玻璃纤维(GF)的表面改性处理,再通过双螺杆挤出机将改性玻纤与尼龙6(PA6)共混制备了玻璃纤维增强尼龙6复合材料(PA6/GF).考察了硅烷偶联剂N1-A处理液质量分数对复合材料力学性能的影响,并将其与氨基硅烷KH550改性玻纤及市售玻纤进行应用对比.结果 表明:硅烷偶联剂N1-A可以与玻璃纤维发生反应,经过硅烷偶联剂N1-A处理过的玻纤与PA6基体的粘接能力更强,硅烷偶联剂N1-A处理液质量分数对处理效果有影响.复合材料的力学性能随硅烷偶联剂N1-A处理液质量分数的升高,先升高后降低,硅烷处理液的最佳质量分数为0.50％,经硅烷偶联剂N1-A处理的玻纤制备的复合材料比经KH550处理的玻纤及市售玻纤制备的PA6/GF复合材料具有更好的综合力学性能.     

乙烯基三烷氧基硅烷对聚硅氧烷乳液聚合的影响

武汉理工大学的吴自强等人研究了乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、γ -甲基丙烯酰氧丙基三甲氧基硅烷对聚硅氧烷乳液聚合反应的影响。结果发现 ,乙烯基三甲氧基硅烷和γ -甲基丙烯酰氧丙基三甲氧基硅烷能明显加快乳液聚合反应的速度 ,提高其聚合稳定性和聚硅氧烷乳液的固含量 ;三种乙烯基三烷氧基硅烷的水解反应速度是 :乙烯基三甲氧基硅烷 >γ -甲基丙烯酰氧丙基三甲氧基硅烷 >乙烯基三乙氧基硅烷。从乳液聚合稳定性看 ,选择乙烯基三甲氧基硅烷的效果最佳。乙烯基三烷氧基硅烷对聚硅氧烷乳液聚合的影响     

γ—氯丙基三乙基硅烷的合成研制

用三氯氢硅和氯丙烯在氯铂酸催化下合成的γ-氯丙基三氯硅烷（γ1），再与无水乙醇反应制得γ-氯丙基三乙基硅烷（γ2），收率达90%以上；它可做为各种卤代橡胶的偶联剂，也是制备其他硅烷偶联剂的重要原料。     

氰乙基三乙氧基硅烷改性玻璃纤维增强尼龙6研究

通过浸渍工艺对玻璃纤维进行了表面改性,并制得玻璃纤维增强型尼龙6复合材料.研究了玻璃纤维浸渍液中氰乙基三乙氧基硅烷质量分数对复合材料力学性能的影响,并与γ-氨丙基三乙氧基硅烷(KH 550)和γ-(2,3-环氧丙氧)丙基三甲氧基硅烷(KH 560)处理的玻璃纤维制得的尼龙6复合材料性能进行了对比.结果表明,随着玻璃纤维...     

环氧基有机硅季铵盐的合成与应用

以N，N-二乙基氨丙基甲基二甲氧基硅烷和环氧氯丙炕为原料，合成了含环氧基的有机硅烷季铵盐。考察了反应溶剂、反应温度、反应时间对产物收率的影响及产物的抗菌性能，优化的工艺条件为：以无水甲醇为溶剂、在55℃下反应10h；在此条件下产物的收率在80M以上。当季铵盐在大肠杆菌菌液中的质量分数达到0．10％时，可有效杀死菌液中的大肠杆菌。     

混炼硅橡胶的配合技术(八)

介绍了2种汽车部件（密封图、汽车挡风玻璃刮片）装配用混炼硅橡胶的配制，以及硫化过程中能与接触基材粘接的混炼硅橡胶（通过添加各种增粘剂如含乙烯烃碳酸酯基或巯基乙酸酯基化合物、烷氧基硅烷、含乙烯基硅官能基过氧化物为硫化剂）的配制。     

单组分室温硫化硅橡胶的配制(八)

介绍了改进脱醇型单组分室温硫化(RTV-1)硅橡胶贮存稳定性的方法(包括采用六甲基二硅氮烷、三烷基硅酸酯、烷氧基硅酸酯、异氰酸根合烃基烷氧基硅烷、氯化钙、氯化镁作醇清除剂及选择适当的钛酸酯作催化剂）和采用双螺杆挤出机配制脱醇型RTV-1硅橡胶的方法。     

NMR spectroscopic studies of dimethyldiethoxy silane hydrolysis and polysiloxane conversion

The hydrolysis rate of alkoxy silane (dimethyldiethoxy silane, DMDES, etc.) is a linear relationship vs. the reaction time under the moisture flux control. The hydrolysis process results in formation of the linear polysiloxane products by a subsequent condensation reaction. An amidized alkoxy silane (3‐(2‐aminoethyl)aminopropylmethyldimethoxy silane, KLM‐602 or γ–aminopropyl‐ triethoxy silane, γ–APS) serves as an internal standard of DMDES hydrolysis kinetics measurements. The hydrolysis kinetics of DMDES with the amidized alkoxy silane and the subsequent linear polysiloxanes conversion have been evaluated and characterized by ²⁹Si‐ and ¹³C‐NMR NMR spectroscopic measurements. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 468–477, 2002     

Mechanistic aspects of silane coupling agents with different functionalities on reinforcement of silica‐filled natural rubber compounds

Silane coupling agents containing different specific functionalities are studied to gain understanding of their roles in silica‐filled natural rubber (NR) compounds. Five different silane coupling agents, that is bis‐(triethoxysilylpropyl) tetrasulfide (TESPT), bis‐(triethoxysilylpropyl) disulfide (TESPD), octyltriethoxysilane, vinyltrimethoxysilane, and bis‐(trimethyl‐silylmethyl) tetrasulfide (TMSMT), are comparatively investigated, by taking the most commonly used TESPT as a reference. The results reveal that alkoxy‐based silanes can effectively reduce the filler–filler interaction and lower compound viscosity owing to the effect of silane‐to‐silica hydrophobation which contributes to better compatibility between silica and NR. The alkoxy‐silanes with a sulfur moiety, that is TESPT and TESPD, show more pronounced improvement in overall properties as a result of filler–rubber interactions. The use of TMSMT which has no alkoxy groups but contains only a sulfur moiety elucidates that there are three reaction mechanisms involved in systems with sulfur‐alkoxy‐based silane. These are as follows: (1) the silane‐to‐silica or silanization/hydrophobation reaction; (2) the silane‐to‐rubber or coupling reaction; and (3) rubber–rubber crosslinking originating from active sulfur released by the polysulfide‐based silane TESPT. These simultaneous reactions are temperature dependent, and show an optimum level at a dump temperature of approximately 140–150°C, as depicted by filler–filler and filler–rubber interactions, as well as mechanical properties of such compounds. POLYM. ENG. SCI., 55:836–842, 2015. © 2014 Society of Plastics Engineers     

Surface structure of silane-treated glass beads and its influence on the mechanical properties of filled composites

The surface treatment of glass beads, chosen as a model filler, was carried out using four different silane coupling agents with multilayer coverage. For this purpose, silanes having an aminopropyl or a methacryloxypropyl group as an organofunctional group with di- or tri-alkoxy structures were used. The amount of silane detected on the bead surface was four to six times that required for a monolayer coverage. The topography of the silane layer on the bead surface was observed using an atomic force microscope. The topography was strongly affected by the composition of the silane solution and the number of alkoxy groups in the silane. The effects of the organofunctional group and the number of alkoxy groups of the silanes on the mechanical properties of bead-filled poly(vinyl chloride), chosen as a typical ductile polymer, were investigated. A higher yield stress was observed for the silane with an aminopropyl group than for that with a methacryloxypropyl group. Furthermore, for each organofunctional group, the yield stress was higher for the silane with a dialkoxy structure than for that with a trialkoxy structure. However, their effects on the elongation-at-break were contrary to the above tendencies.     

乙烯基硅氧烷改性丙烯酸酯乳液聚合的动力学及成核机理分析

用种子乳液聚合法研究了硅氧烷改性丙烯酸酯的乳液聚合,对影响种子乳液聚合动力学的因素进行讨论,并分析了乳液聚合的成核机理.实验结果表明：反应温度、引发剂浓度、乳化剂浓度和有机硅氧烷用量对有机硅改性丙烯酸酯乳液聚合动力学有较大的影响.反应温度越高,引发剂浓度越高、乳化剂浓度越高、有机硅氧烷用量相对较小,乳液聚合反应的转化率越高;此外,体系的pH值在6～8之间时也有利于反应的进行.种子乳液聚合中R_P∝［E］^0.72,R_P∝［I］^0.56,表观活化能E_a为143.92 kJ•mol^-1.种子乳液聚合初期,反应主要是单体液滴成核;进入壳层反应时,反应成核主要是以胶束成核为主.     

金属表面有机硅烷钝化膜的研究与进展

阐述了有机硅烷的种类和钝化机理,指出了影响硅烷成膜的主要因素,并对硅烷钝化的研究进展进行了介绍。认为采用复配技术,在硅烷中添加缓蚀剂、纳米粒子等添加剂,应是硅烷钝化的主要研究方向。     

Structure of silane layer formed on silica particle surfaces by treatment with silane coupling agents having various functional groups

The surface treatment of spherical silica particles with silane coupling agents having various organic functional groups was conducted and the effect of the alkoxy group number on the molecular flexibility of the silane chain with multilayer coverage was investigated using ¹H-pulse nuclear magnetic resonance spectroscopy. The silica particles were treated with 2-propanol solution and heated at 120?°C for 24?h after solvent evaporation to accelerate the polycondensation reaction of silanol groups. For multilayer coverage, flexible linear chain and rigid network structures were expected to form on the surface from the di- and trialkoxy structures, respectively. However, the rigid network structure was formed from both the di- and trialkoxy structures with glycidoxy, amino, and methacryloxy functional silanes. Ring opening of the epoxy group occurred, followed by reaction to form the network structure, even with the dialkoxy structure of the glycidoxy functionality. Ring opening of the epoxy group could be reduced by pH adjustment of the treatment solution and the linear chain structure was formed from the dialkoxy structure. In the case of amino and methacryloxy functional groups, hydrogen bonds were formed between the amino or methacryloxy groups and the silanol groups on the silica surface or silane molecules.     

有机硅改性VAc/BA/AA共聚乳液胶粘剂的研究

介绍了有机硅改性 VAc/BA/AA共聚乳液胶粘剂的合成工艺 ,讨论了预乳化工艺、乳化剂体系、PVC及改性共聚单体对粘接强度、耐水性等乳液性能的影响 ;结果表明 ,通过采用预乳化工艺、适宜的乳化剂体系和 PVA,引入有机硅、BA、AA等单体对 PVAc乳液进行共聚改性 ,可以合成综合性能优异的乳液胶粘剂     

γ-氨丙基二甲基乙氧基硅烷修饰蒙脱土及硅烷化蒙脱土的性能

用单官能团硅烷偶联剂γ-氨丙基二甲基乙氧基硅烷（APMS）修饰蒙脱土（MMT）, IR 分析表明APMS通过化学键与蒙脱土键合。利用偶联剂上的氨基与水杨醛显色生成黄色希夫碱对404 nm处可见光的吸收特性进行定量测试,确定了蒙脱土可和偶联剂反应的活性硅羟基数目为29.6 mmol/(100gMMT),最佳烘干温度为120 ℃。XRD结果说明蒙脱土的活性硅羟基分布在其端面不是在层间。推断出蒙脱土和单官能团硅烷偶联剂的反应分两步进行：偶联剂的烷氧基先在水醇溶液中水解生成硅醇,然后和蒙脱土端面上的硅羟基高温干燥脱水形成硅烷化蒙脱土。偶联剂修饰蒙脱土后其阳离子交换容量（CEC）不变,分散性实验显示硅烷化蒙脱土在水中的分散性变差,在甲苯和乙醇中的分散性提高,说明偶联剂的修饰提高了MMT在有机溶剂中的分散性。