丙烯酸酯改性硅油消泡剂的制备

Preparation of Alkyl Acrylate Modified Silicone Oil Defoaming Agent

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。

Under the catalysis of chloroplatinic acid, alkyl acrylate modified silicone oil was synthesized by the hydrosilylation reaction taking low hydrogen silicone oil, self-made fourteen methacrylate as raw materials.The experiment of esterification reaction by single factor test was done to determine the optimum technological conditions.The esterification rate reached 95.44% under the optimum experimental conditions： the molarrate of α-methy-lacrylic acid and tetradecyl alcohol is 1.1：1, the amount of p-methy benzene sulfonic acid is 1.5%, reaction temperature is 130℃, reaction time is 6 h. The hydrosilylation optimum reaction conditions by orthogonal experiment as follow： the molar ratio of silicon-hydrogen bonds was 1：1.20, the amount of catalyst was 30 μg·g^-1, the reaction temperature was 85%2, the reaction time was 5 hr. Under this condition, the conversion rate of reation reached 91.89%. The structures were confirmed by IR spectroscopy and nuclear magnetic resonance （^1HNMR） spectrum, defoaming time of the emulsion defoamer was 12 s, inhibiting-foam time was 860 s.