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机构地区:[1]陕西科技大学教育部轻化工助剂化学与技术重点实验室,陕西西安710021
出 处:《石油化工》2016年第5期570-575,共6页Petrochemical Technology
基 金:陕西省科学技术研究发展计划项目(2013K11-19);陕西省科技统筹创新工程计划项目(2014KTCL01-11)
摘 要:采用溶液聚合法,根据硅氢加成反应原理,以1-十二烯和苯基含氢硅油为原料、异丙醇为溶剂、氯铂酸为催化剂,制备长链烷基改性苯基含氢硅油。采用FTIR和1H NMR技术对试样的结构进行表征,并采用正交实验确定了产物合成的最佳工艺条件。表征结果显示,苯基含氢硅油与1-十二烯发生了接枝反应,长链烷基成功接枝到了聚硅氧烷链上。实验结果表明,在反应时间5.0 h、反应温度115℃、催化剂加入量30μg/g、n(Si—H)∶n(C-C)=1∶1.10、1-十二烯的滴加时间25 min的最佳工艺条件下,Si—H键的转化率高达82.25%。产物长链烷基改性苯基含氢硅油为油溶性单体,且相对分子质量较高,具有较好的破乳效果。Phenyl hydrogen-containing silicone oil with long-chain alkyl was prepared through the hydrosilylation reaction of 1-dodecene and phenyl hydrogen-containing silicone oil with isopropanol as the solvent and chloroplatinic acid as the catalyst. The structure of the product was verified by means of FTIR and 1H NMR. The effects of temperature,reaction time,catalyst dosage,molar ratio of Si—H to C-C and dropping way of 1-dodecene on the conversion of Si—H were investigated. The reaction conditions were optimized through orthogonal experiments. The results showed that,under the optimized conditions of reaction time 5.0 h,temperature 115 ℃,catalyst dosage 30 μg/g,n(Si—H)∶n(C-C)=1∶1.10 and dropping time of 1-dodecene 25 min,the conversion of Si—H reached 82.25%.
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