乳液聚合法制备水溶性有机硅膏

Preparation of Water-Soluble Silicone Paste by Emulsion Polymerization

以八甲基环四硅氧烷(D_(4))、甲基三甲氧基硅烷、甲基丙烯酰氧基丙基三甲氧基硅烷为原料,异构十三醇聚氧乙烯醚与磷酸单十二烷基酯钠盐(PAMES)复配物为乳化剂,聚乙二醇为助乳化剂,十二烷基苯磺酸为催化剂,通过乳液聚合法制得有机硅膏。考察了乳化剂复配质量比和用量、原料滴加速率、催化剂用量、反应温度、D_(4)用量对有机硅膏性能的影响。结果表明,较佳的制备条件为:异构十三醇聚氧乙烯醚与PAMES质量比35∶1、乳化剂用量2.5份、D_(4)与硅烷混合物滴加速率3.5 g/min、催化剂用量2.5份、反应温度75℃、D_(4)用量25份。此时,制得的有机硅膏综合性能较佳,平均粒径为2.34μm,离心稳定性、稀释稳定性、耐电解质稳定性良好,有机硅膏质量分数10%的水溶液透光率为62.7%。

Using octamethylcyclotetrasiloxane (D_(4)), methyltrimethoxysilane, and methacryloxypropyltrimethoxysilane as raw materials, isomeric tridecanol polyoxyethylene ether (1305 ) and monododecyl phosphate sodium salt (PAMES ) as emulsifier, PEG-400 as auxiliary agent, dodecylbenzene sulfonic acid as catalyst, and silicone paste was prepared by emulsion polymerization. The effects of emulsifier compound mass ratio and dosage, raw material loading speed, catalyst dosage, reaction temperature and D_(4) dosage on the properties of silicone paste were investigated. The results show that the best preparation conditions are: the mass ratio of 1305 to PAMES is 35∶ 1, the amount of emulsifier is 2.5 phr, the loading speed of the mixture of D_(4) and silane is 3.5 g/min, the amount of catalyst is 2.5 phr, the reaction temperature is 75 ℃, and the amount of D_(4) is 25 phr. At this condition, the prepared silicone paste has good comprehensive performance, the average particle size is 2.34 μm, the centrifugal stability, dilution stability and electrolyte resistance stability are good, and the light transmittance of the aqueous solution with a mass fraction of 10% of the silicone paste is 62.7% .