湖北拟建万吨级硅烷偶联剂中间体项目

湖北武大有机硅新材料股份有限公司在葛店经济技术开发区建设直接法合成三乙氧基硅烷,并用三乙氧基硅烷（后面简称三乙）合成硅烷偶联剂中间体卜氯丙基三乙氧基硅烷,第一步是以硅粉和乙醇为主要原料,合成三乙氧基硅烷,附产品四乙氧基硅烷（后面简称四乙）;第二步是以三乙氧基硅烷和氯丙烯为主要原料,     

耐高温有机硅改性不饱和聚酯树脂的制备及性能研究

以甲基三乙氧基硅烷、二苯基硅二醇和乙烯基三乙氧基硅烷为原料首先合成出了有机硅树脂预聚体,然后将其添加到不饱和聚酯合成步骤中。通过有机硅预聚体上的硅羟基和乙氧基与不饱和聚酯上的羟基进行缩合反应来完成整个改性过程,最终制备出耐高温有机硅改性不饱和聚酯树脂。采用IR、TGA对不饱和聚酯改性前后的结构与性能进行了表征和分析。IR测试结果表明:有机硅树脂的分子结构成功的引入到不饱和聚酯树脂的分子链上。TGA测试结果表明:不饱和聚酯树脂经有机硅改性之后其起始分解温度从295℃上升到了340℃,耐热性能得到了显著的提高。此外,对有机硅改性前后不饱和聚酯树脂的体积电阻率和吸水率进行了测试,结果显示有机硅分子结构的引入不但可以提高不饱和聚酯树脂的耐热性能,还可以改善其电性能和防水性。     

环氧松香封端有机硅聚合物的合成及性能研究

以松香为原料先制备了环氧松香酰氯,然后以二甲基甲酰胺为溶剂,与羟基硅油通过酰化反应合成了环氧松香封端有机硅聚合物。研究了反应温度和物料配合比对合成反应的影响,并对产物进行了红外光谱(FT-IR)分析和热失重分析。实验结果表明:环氧松香酰氯与羟基硅油的质量配合比为2.2∶1,吡啶用量为松香酰氯的10%(wt,质量分数),反应温度40℃,反应3h条件下,松香封端有机硅聚合物的产率达到90.1%,黏度达到158.2mPa·s,环氧值达到0.156mol/100g。红外光谱(FT-IR)和环氧值分析测试表明在环氧松香引入了聚硅氧烷结构,热失重表明环氧松香封端有机硅聚合物具有较好的热稳定性能。     

甲基有机硅树脂的无溶剂合成研究

以甲基三乙氧基硅烷单体和二甲基二乙氧基硅烷单体为原料,采用水解-缩聚的方法合成了甲基有机硅树脂,并研究了无溶剂合成甲基有机硅树脂的条件。结果表明,一定配比,水解温度为70℃,缩聚温度为80～85℃,反应时间为4h,可合成无溶剂体系的甲基有机硅树脂;红外光谱(IR)表明,合成的甲基有机硅树脂在Si-O-Si处有较宽的吸收峰;固化温度为140℃,固化4h,得到无色透明甲基有机硅树脂。     

耐高温有机硅树脂的合成

以甲基和苯基烷氧基硅烷为原料,采用水解-缩聚的方法合成了有机硅树脂,并研究了合成硅树脂的工艺条件对硅树脂性能的影响.结果表明,一定配方,水解温度为65℃,反应时间为4～5h时,可合成出易溶于二甲苯、易成膜、适于作涂料基体树脂的有机硅树脂;红外光谱(IR)表明,合成的硅树脂含有端羟基,加入硅氮低聚物后,能室温固化;凝胶渗透色谱(GPC)分析表明,所合成的有机硅树脂分子量在6500左右;热失重(TG)表明,硅树脂有很好的耐热性能,在500℃时的失重仅为7.12%;机械性能及交流阻抗分析表明,300℃下,合成硅树脂所制清漆的机械物理性能及抗渗性能优良,可以用于制备耐高温涂层.     

硅烷改性醇溶性丙烯酸酯胶粘剂的制备和性能

利用乙烯基三乙氧基硅烷对醇溶性聚丙烯酸酯进行了改性,合成了一种可用于塑料薄膜的环保型胶粘剂。讨论了有机硅单体的加入对聚合反应、胶粘剂粘接强度的影响,并探讨了影响粘接强度的因素。研究表明,有机硅单体的最佳用量为3%,过量的有机硅会导致材料结构缺陷,从而影响粘接强度。     

γ-甲基丙烯酰氧基烃基硅烷大分子的合成研究

以八甲基环四硅氧烷(D4)、γ-甲基丙烯酰氧基丙基三乙氧基硅烷(KH-570)、六甲基二硅氧烷(MM)为原料,在Me4NOH催化和二甲基亚砜(DMSO)促进作用下,通过本体聚合合成了有机硅大分子.确立了最佳反应条件,温度为90℃、Me4NOH的用量为0.12%时,通过控制MM的用量,可制得一定分子量侧链含双键的有机硅大分子.红外光谱图表明,分子结构达到了预期结果.     

二乙氧基硅烷与三乙氧基硅烷共聚物的合成及表征

利用盐酸为催化剂,以二甲基乙氧基硅烷、二苯基乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三甲氧基硅烷及水进行水解缩聚反应,制备了具有反应活性的有机-无机杂化有机硅树脂共聚物。通过正交实验研究了催化剂浓度、原料配比、温度及水对树脂产率的影响,得出适宜的合成工艺条件为酸浓度为0.05mol/L、原料配比为1.5∶2.5∶6、温度为70℃、水量为0.1mol。采用红外光谱、核磁对最优配比产物结构进行了表征,表明树脂中具有可反应性基团,其主链为硅氧链。采用GPC分析,数均分子量为43040,分散系数为2.3,分布较宽。     

C级无溶剂有机硅浸渍树脂的制备及表征

以甲基苯基硅烷单体和特种硅烷单体制备有机硅氧烷预聚物出发合成了一种有机硅浸渍树脂,该浸溃树脂不含任何有机溶剂,在常温下为低黏度流动液体.采用红外光谱、核磁共振、扫描电镜和凝胶色谱对浸渍树脂的结构和物理特性进行了表征.结果表明,该类浸渍树脂分子结构中含有硅氢和乙烯基团的聚有机硅氧烷,属分子量较小的低聚物.     

一种碳硼烷改性有机硅树脂的制备及其耐热性能

碳硼烷改性有机硅树脂是一种耐热性能优异的高分子材料,具有广阔的应用前景.然而由于聚合单体碳硼烷改性硅氧烷的合成条件苛刻,严重影响碳硼烷改性有机硅树脂的制备和应用.本研究利用羟基与异氰酸酯基间的加成反应,在温和的条件下合成了一种新型结构的碳硼烷改性硅氧烷-碳硼烷改性氨酯桥接丙基三乙氧基硅烷(CBR-Si),在此基础上经水...     

耐高温乙炔基封端聚酰亚胺的制备与性能

基于单体4-苯基醚-1,3-二胺制备了一种新型乙炔基封端热固性聚酰亚胺.利用傅里叶变换红外光谱仪、核磁共振氢谱仪和X射线衍射仪对其结构进行表征,其结果表明制备得到了相应结构的预聚体.利用差示扫描量热仪测得预聚体的玻璃化转变温度(Tg)仅为155℃.预聚体在有机溶剂中具有高的溶解性,常温下在N-甲基吡咯烷酮中的溶解度高于...     

UV curable lens production using molecular weight controlled PEEK based acrylic oligomer (Ac-PEEK)

We produced UV curable lenses with properties blocking short wave UV light. In the UV-curable formulations, we used an oligomer (Ac-PEEK) with another urethan oligomer (Mw = 2000). Radically active, molecular weight controlled Ac-PEEK was obtained by reacting 2-hydroxyl ethyl methacrylate with molecular- weight- controlled and isocyanate terminated PEEK (Mn = 4500). We characterized all synthesized monomer, oligomer and optical materials with UV/Vis spectrophotometer with interferogram, elemental analyser, mass spectrophotometer, proton nuclear magnetic resonance, Fourier transform infrared spectroscopy, thermal gravimetric analyzer, differential scanning calorimeter, scanning electron microscopy and gas chromatography. Results suggested that newly synthesized oligomer with the structure of PEEK absorbs short wave UV-light. Ageing tests [ISO 11979-5, Ophthalmic implants—intraocular lenses (IOL)—Part 5: Biocompatibility] performed on the IOL materials were successful. High contact angle of the obtained lenses suggests that all lenses were hydrophobic and SEM results revealed that lenses are morphologically homogeneous. Based on all positive properties just mentioned, we safely conclude that the lenses produced in this study are very promising for IOL production.     

Synthesis and characterization of polystyrene brushes for organic thin film transistors

We synthesized and characterized polystyrene brushes on a silicon wafer using surface-initiated atom transfer radical polymerization. The thickness of the polymer brush was controlled by adjusting the reaction time. We investigated monomer conversion as well as the molecular weight and density of the polymer brushes. When the monomer conversion reached 100%, the number-average molecular weight and film thickness reached 135,000 and 113 nm, respectively. The estimated densities of the synthesized polystyrene brushes were in the range 0.34-0.54 chains/nm2, high enough to be categorized in the "concentrated brush" regime. The synthesized polymer brush was used as an insulating layer in an organic thin-film transistor. Organic thin-film transistors were fabricated using pentacene as an active p-type organic semiconductor and a polystyrene brush on a SiO2 layer as a gate dielectric. The pentacene based organic thin-film transistor with the polystyrene brush exhibited a field-effect mobility microFET of 0.099 cm2/(V x s).     

Immobilization of aromatic aldehyde molecules on indium tin oxide surface using acetalization reaction

We demonstrated an acetalization reaction as a versatile method to immobilize aromatic aldehyde molecules on surfaces of metal oxides, silicon dioxide, and indium tin oxide. First, a trimethylsily (TMS) terminated surface was formed using a silylation reaction between a chloride group of trimethylsilychloride and a hydroxyl group of the substrate surfaces. Second, terephthalaldehyde (TPA) was immobilized on the surfaces using an acetalization reaction between the TMS-terminated surface and an aldehyde group of TPA. Results of contact angle, X-ray photoelectron, and ultraviolet absorption spectra revealed that the TPA molecules on the surfaces were well-packed with a high surface density.     

从配位硅出发低温合成脂肪族含硅聚酯及其结构表征

从二氧化硅与乙二醇、氢氧化钾反应生成的高反应活性的五配位硅钾化合物出发,首先以此为原料与2-氯乙醇反应制备双羟基四配位有机硅单体,然后再将其与己二酰氯进行低温溶液缩聚合成脂肪族含硅聚酯。探讨了不同反应条件对聚合物结构和性能的影响,并对合成的聚合物作了红外光谱、热重分析、分子量的测定等结构表征。     

直接由SiO2低温合成含硅聚酯及其结构表征

研究了直接从无定型二氧化硅出发，与乙二醇、氢氧化钾反应，生成高反应活性的五配位硅钾化合物，并以此为原料与2-氯乙醇反应制备双羟基四配位有机硅单体，然后该单体再与对苯二甲酰氯进行低温溶液缩聚反应合成含硅聚酯，并对合成的物质作了红外光谱，热重分析、分子量测定、能谱元素分析等结构表征。     

溶胶-凝胶法制备的PMMA/四配位硅杂化材料及其性能

以无定形二氧化硅为起始原料,与乙二醇、氢氧化钾反应,生成高反应活性的五配位硅钾化合物,再与2-氯乙醇反应生成双羟基四配位硅化合物(DHTS)。并以DHTS为前驱体与甲基丙烯酸甲酯(MMA)、γ-(甲基丙烯酰氧基)丙基三甲氧基硅烷(KH-570)反应,用BPO引发聚合,在酸催化下通过溶胶-凝胶法制备了PMMA/四配位硅杂化材料。并用IR光谱表征了杂化材料的结构;同时研究了其硬度、透光率、热稳定性等问题。     

Synthesis and structure evolution of phenolic resin/silicone hybrid composites with improved thermal stability

Phenolic resin/silicone hybrid composites (MPR) were prepared by a facile and low-cost method. FTIR results show that polycondensation of siloxane occurs in the presence of catalyst and water in the system, and siloxane oligomer was formed. During the curing process, the transesterification reaction between siloxane oligomer and phenolic resin (PR) makes silicon incorporated into PR. The TGA results indicate that introducing Si–O structure into PR can effectively improve the thermal stability of the resin. Compared with cured neat PR, temperatures at 5 and 10% mass loss of cured MPR can be improved by 43 and 36 °C. Its char yield at 800 °C was increased by about 9.1%. Cured MPR has been characterized by FTIR, XPS, XRD and Raman spectra to discuss the chemical state changes of silicon during pyrolysis process, as well as the effect of silicon on the char yield. On the one hand, the formation of Si–O–C structure can reduce the number of phenyl hydroxyl groups, which contributes to the reduced weight loss. On the other hand, the results indicate that Si–O_x structure was formed from the oxidation of Si–CH₃ and hydrolysis of Si–O–C structures. According to Raman analyses, introducing silicone into the system cannot help to promote the formation of a more ordered structure. Additionally, the mechanical properties of cured MPR have also been improved.     

Photofunctional terbium centered inorganic/organic hybrid material with the functionalized 5-dihydroxybenzoate linkage

In this study, silica-based organic-inorganic hybrids were prepared using sol-gel methods. A new kind of monomer (DHBA-TESPI) was derived by modifying the double hydroxyl groups of 3, 5-dihydroxybenzoic acid (DHBA) with 3-(triethoxysilyl)-propyl isocyanate (TESPI) through the addition reaction. Then, the obtained compound and tetraethoxysilane (TEOS) were used as the inorganic and organic counterparts respectively. Coordination reaction between Tb³⁺ and the carboxylic groups of the monomer happen simultaneously. IR, NMR, UV/Vis absorption, low-temperature phosphorescence spectroscopy and fluorescence spectroscopy were used to characterize the hybrids. The final materials exhibited strong green-colored fluorescence (Tb³⁺), which can be explained by the intramolecular energy transfer caused by coordination of the organic counterpart. The spectroscopic data also revealed that the triplet state energy of the organic ligand matches the emissive energy level of Tb³⁺.     

羟化聚天冬氨酸水凝胶的制备及药物缓释性能

以L天冬氨酸为单体进行缩聚反应所得到的高分子量聚琥珀酰亚胺(PSI)为母体,己二胺为交联荆,采用乙醇胺对其进行改性,制备了羟化聚天冬氨酸水凝胶.研究了反应温度、交联剂及乙醇胺用量对水凝胶溶胀性能的影响;以水杨酸为模型药物,研究了其载药性能及在不同释放介质中的释放行为.结果表明,反应温度为40℃,交联剂用量为PSI用量的...