响应面法优化合成1,1,1,3,5,5,5-七甲基三硅氧烷

doi:10.3969/j.issn.0438-1157.2013.10.020

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

• 催化、动力学与反应器 • 上一篇下一篇

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. 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

收稿日期:2013-04-17 修回日期:2013-06-29 出版日期:2013-10-05 发布日期:2013-10-05
通讯作者: 廖列文
作者简介:龚红升(1986-),男,本科。

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. 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

摘要/Abstract

摘要： 选用六甲基二硅氧烷(MM)和高含氢硅油(D^H)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(MD^HM)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MD^HM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,MD^HM的最佳合成条件为:反应物质量比为m(D^H):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MD^HM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

Abstract: The systhesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane(MD^HM)from hexamethydi-siloxane(MM)and highly hydrogen-containing polyhydrosiloxane(D^H)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 MD^HM by regression analysis.The optimal conditions at which the highest yield of MD^HM(40.62%)was obtained,were in agreement with predicted value(41.23%).The reaction mass ratio of m(D^H):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

中图分类号:

TQ423.91

龚红升, 胡文斌, 廖列文, 罗泽保, 张素梅, 尹国强. 响应面法优化合成1,1,1,3,5,5,5-七甲基三硅氧烷[J]. 化工学报, 2013, 64(10): 3633-3639.

GONG Hongsheng, HU Wenbin, LIAO Liewen, LUO Zebao, ZHANG Sumei, YIN Guoqiang. Synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane by response surface methodology[J]. CIESC Journal, 2013, 64(10): 3633-3639.

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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

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