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以低含氢硅油、自制甲基丙烯酸十四酯为原料,氯铂酸为催化剂,通过硅氢加成反应合成了丙烯酸酯改性硅油。通过单因素考查了反应温度、反应时间、α-甲基丙烯酸/十四醇摩尔比和催化剂用量对酯化率的影响,确定了最佳工艺条件:n(α-甲基丙烯酸):n(十四醇)为1.1:1,对甲苯磺酸用量1.5%(质量分数),反应温度130℃,反应时间6 h,酯化率达到95.44%。通过正交实验得到硅氢加成优化工艺条件为:n(Si-H):n(C=C)为1:1.20,催化剂用量30μg·g-1,反应温度85℃,反应时间5 h,此条件下转化率达92.89%。产物结构经过红外光谱和核磁共振氢谱进行了确证,配制的消泡剂乳液消泡时间12 s,抑泡时间长达860 s。
Acrylate-modified silicone oil was synthesized by hydrosilylation using low hydrogen silicone oil, self-made tetradecyl methacrylate as raw material and chloroplatinic acid as catalyst. The effects of reaction temperature, reaction time, the molar ratio of α-methacrylic acid / tetradecyl alcohol and the amount of catalyst on the esterification rate were investigated by single factor. The optimum technological conditions were as follows: n (α-methacrylic acid) Tetradecyl alcohol) was 1.1: 1, the amount of p-toluenesulfonic acid was 1.5% (mass fraction), the reaction temperature was 130 ℃ and the reaction time was 6 h. The esterification rate reached 95.44%. The optimal conditions for the hydrosilylation were obtained by orthogonal experiments: the molar ratio of n (Si-H): n (C = C) was 1: 1.20, the catalyst dosage was 30μg · g-1, the reaction temperature was 85 ℃, the reaction time was 5 h, Under this condition, the conversion rate reached 92.89%. The structure of the product was confirmed by IR and 1H NMR spectra. The defoaming time of the defoamer emulsion was 12 s and the defoaming time was 860 s.