响应面法优化合成1,1,1,3,5,5,5-七甲基三硅氧烷  

Synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane by response surface methodology

作　　者：龚红升[1] 胡文斌[1] 廖列文[1] 罗泽保 张素梅[1] 尹国强[1] 

机构地区：[1]仲恺农业工程学院化学化工学院绿色化工研究所,广东广州510225 [2]韶关市科韶开发中心,广东韶关512026

出　　处：《化工学报》2013年第10期3633-3639,共7页CIESC Journal

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：1 1 1 3 5 5 5-七甲基三硅氧烷 响应面法 PLACKETT-BURMAN设计 最徒爬坡实验 Box-Benhnken设计 强酸型离子交换树脂 

分 类 号：TQ423.91[化学工程]