CIESC Journal ›› 2013, Vol. 64 ›› Issue (10): 3633-3639.DOI: 10.3969/j.issn.0438-1157.2013.10.020

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

GONG Hongsheng1, HU Wenbin1, LIAO Liewen1, LUO Zebao2, ZHANG Sumei1, YIN Guoqiang1   

  1. 1. Institute of Green Chemical Engineering, School of Chemistry and Chemical Engineering, Zhongkai University of Agriculture and Engineering, Guangzhou 510225, Guangdong, China;
    2. Shaoguan Ke Shao Development Center, Shaoguan 512026, Guangdong, China
  • Received:2013-04-17 Revised:2013-06-29 Online:2013-10-05 Published:2013-10-05

响应面法优化合成1,1,1,3,5,5,5-七甲基三硅氧烷

龚红升1, 胡文斌1, 廖列文1, 罗泽保2, 张素梅1, 尹国强1   

  1. 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
  • 通讯作者: 廖列文
  • 作者简介:龚红升(1986-),男,本科。

Abstract: 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.

Key words: 1,1,1,3,5,5,5-heptamethyltrisiloxane, response surface methodology, Plackett-Burman design, steepest climbing test, Box-Benhnken design, strong acidic cation ion exchange resin

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10 h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。

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

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