机构地区: 仲恺农业工程学院化学化工学院绿色化工研究所
出 处: 《化工学报》 2013年第10期3633-3639,共7页
摘 要: 选用六甲基二硅氧烷(MM)和高含氢硅油(DH)为原料,强酸型离子交换树脂作催化剂,采用响应面优化法对1,1,1,3,5,5,5-七甲基三硅氧烷(MDHM)的合成工艺进行优化。在单因素实验的基础上,依次采用Plackett-Burman设计,最陡爬坡实验及Box-Behnken设计法进行工艺优化,以MDHM的质量分数为响应值作响应面,然后进行回归分析。实验结果表明,MDHM的最佳合成条件为:反应物质量比为m(DH)∶m(MM)=1∶13.45,反应温度为62.5℃,催化剂用量为7.09%。在反应时间10h的条件下,产物中MDHM的质量分数为40.62%,与模型预测值基本相符。通过研究温度对反应动力学的影响,进一步验证了所取温度和时间的合理性。 The systhesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane (MDHM) from hexamethydi-siloxane (MM) and highly hydrogen-containing polyhydrosiloxane (DH) was optimized after applying response surface methodology (RSM) in the presence of strong acidic cation ion exchange resin as catalyst. Based on the single-factor testing results, RSM measurements were performed with respect to mass concentration of MDHM by regression analysis. The optimal conditions at which the highest yield of MDHM (40. 62%) was obtained, were in agreement with predicted value (41.23%). The reaction mass ratio of m(DH) : m(MM)=1 : 13.45, the amount of solid acid catalyst was 7.09%, and reaction temperature and time were 62.5℃ and 10 h, respectively. Furthermore, the research on polymerization kinetics at different temperatures was performed and the results showed that the optimal temperature and time were right.
关 键 词: 七甲基三硅氧烷 响应面法 设计 最徒爬坡实验 设计 强酸型离子交换树脂
领 域: [化学工程]