[1]谢贤清,吴良发.电子级三甲基硅烷的合成与提纯工艺改进[J].江西师范大学学报(自然科学版),2019,(02):172-176.[doi:10.16357/j.cnki.issn1000-5862.2019.02.10]
　XIE Xianqing,WU Liangfa.The Process Improvement of Synthesis and Purification Process of Electronic Grade Trimethylsilane[J].Journal of Jiangxi Normal University:Natural Science Edition,2019,(02):172-176.[doi:10.16357/j.cnki.issn1000-5862.2019.02.10]
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电子级三甲基硅烷的合成与提纯工艺改进()
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《江西师范大学学报》（自然科学版）[ISSN:1006-6977/CN:61-1281/TN]

卷:
期数:
2019年02期
页码:
172-176
栏目:
化学与生命科学
出版日期:
2019-04-10

文章信息/Info

Title:
The Process Improvement of Synthesis and Purification Process of Electronic Grade Trimethylsilane
文章编号:
1000-5862(2019)02-0172-05
作者:
谢贤清1; 吴良发2
1.江西师范大学国家单糖化学合成工程技术研究中心,江西 南昌 330027; 2.江西省药品检验检测研究院,江西省药品与医疗器械质量工程技术研究中心,江西 南昌 330029
Author(s):
XIE Xianqing1; WU Liangfa2
1.National Monosaccharide Chemical Synthesis Engineering Technology Research Center,Jiangxi Normal University,Nanchang Jiangxi 330027,China; 2.Jiangxi Provincial Institute for Drug Control,Jiangxi Provincial Engineering Research Center for Drug and Medica
关键词:
电子级;  有机纯度;  无机纯度;  回流比;  加压精馏
Keywords:
electron grade;  organic purity;  inorganic purity;  reflux ratio;  pressurized distillation
分类号:
TQ 2
DOI:
10.16357/j.cnki.issn1000-5862.2019.02.10
文献标志码:
A
摘要:
以氯甲烷、二甲基一氯硅烷为原料,经格氏反应生成格氏试剂再与二甲基一氯硅烷反应得到三甲基硅烷,经加压精馏得到电子级三甲基硅烷,总收率达到 68.2%(以二甲基一氯硅烷计),最终产物结构通过1H NMR、ESI-MS进行表征.气相色谱检测产品有机纯度达99.99%以上,ICP-MS检测无机纯度达到99.999 99%.考察了溶剂的种类、卤代烷的种类、二甲基一氯硅烷的用量及其他反应条件对三甲基硅烷收率的影响.结果表明: 2-甲基四氢呋喃为最佳的溶剂,氯甲烷是较经济又方便提纯的原料,确定了二甲基一氯硅烷最佳摩尔比为n(二甲基一氯硅烷):n(格氏试剂)= 1.0:1.2,最佳反应温度为30 ℃,合成收率为92.3%.对精馏提纯的回流比、精馏压力和产品接收方式进行研究,确定最佳回流比为5:1,精馏压力为200 kPa时,提纯效果最佳.
Abstract:
The trimethylsilane is obtained from chloromethane and Chlorodimethylsilane as raw materials,and the reagent is reacted with Chlorodimethylsilane after the Grignard reaction to obtain trimethylsilane,and the electron-grade trimethylsilane is rectified under pressure.The total yield reached 68.2%(measured as Chlorodimethylsilane).The final product structure is characterized by 1H NMR and ESI-MS.The organic purity of the product is 99.99%,and the inorganic purity of ICP-MS is 99.999 99%.The effects of solvent types,halogenated alkanes,amount of Chlorodimethylsilane and reaction conditions on the yield of trimethylsilane are investigated.The results show that 2-methyltetrahydrofura is the best solvent,and chloromethane is a more economical and convenient purification raw material.The optimum molar ratio of Chlorodimethylsilane is determined to be n(Chlorodimethylsilane):n(Grignard reagent)=1.0:1.2,the optimum reaction temperature is 30 ℃,and the synthetic yield is 92.3%.The reflux ratio,distillation pressure and product receiving mode of distillation and purification are studied.The optimal reflux ratio is 5:1 and the distillation pressure is 200 kPa,and the purification effect is best.

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备注/Memo

备注/Memo:
收稿日期:2018-06-21 基金项目:国家重点研发计划(2017YFB0404303)和江西省青年科学基金(20161BAB213068)资助项目. 作者简介:谢贤清(1980-),男,湖南邵阳人,助理研究员,主要从事精细化学品合成研究.E-mail:xxqhjh117@163.com
更新日期/Last Update: 2019-04-10