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

GONG Hongsheng; HU Wenbin; LIAO Liewen; LUO Zebao; ZHANG Sumei; YIN Guoqiang

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

更新时间：2025-12-10

- Synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane by response surface methodology
- CIESC Journal Issue 10, Pages: 3633-3639(2013)
- 作者机构：
  
  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
- 作者简介：
- 基金信息：
- DOI：10.3969/j.issn.0438-1157.2013.10.020
  CLC： Q423.91
- Online First：05 October 2013，
  
  Published：05 October 2013
- 稿件说明：
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GONG Hongsheng, HU Wenbin, LIAO Liewen, et al. Synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane by response surface methodology[J]. CIESC Journal, 2013, (10): 3633-3639.
DOI：

GONG Hongsheng, HU Wenbin, LIAO Liewen, et al. Synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane by response surface methodology[J]. CIESC Journal, 2013, (10): 3633-3639. DOI： 10.3969/j.issn.0438-1157.2013.10.020.

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

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。

Abstract

The systhesis of 1

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.

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