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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
引用本文: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. DOI: 10.3969/j.issn.0438-1157.2013.10.020
作者姓名:龚红升  胡文斌  廖列文  罗泽保  张素梅  尹国强
作者单位: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
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  
收稿时间:2013-04-17
修稿时间:2013-06-29

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. Synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane by response surface methodology[J]. Journal of Chemical Industry and Engineering(China), 2013, 64(10): 3633-3639. DOI: 10.3969/j.issn.0438-1157.2013.10.020
Authors:GONG Hongsheng  HU Wenbin  LIAO Liewen  LUO Zebao  ZHANG Sumei  YIN Guoqiang
Affiliation: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
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.
Keywords: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  
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