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[1]曹健,伍川,董红,等.邻、间和对位苯甲基官能化甲基二乙氧基硅烷的合成[J].南京工业大学学报(自然科学版),2013,35(02):80-85.[doi:10.3969/j.issn.1671-7627.2013.02.016]
 CAO Jian,WU Chuan,DONG Hong,et al.Synthesis of o-,m-,and p-tolylmethyldiethoxysilane[J].Journal of NANJING TECH UNIVERSITY(NATURAL SCIENCE EDITION),2013,35(02):80-85.[doi:10.3969/j.issn.1671-7627.2013.02.016]
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邻、间和对位苯甲基官能化甲基二乙氧基硅烷的合成()
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《南京工业大学学报(自然科学版)》[ISSN:1671-7627/CN:32-1670/N]

卷:
35
期数:
2013年02期
页码:
80-85
栏目:
出版日期:
2013-03-20

文章信息/Info

Title:
Synthesis of o-,m-,and p-tolylmethyldiethoxysilane
文章编号:
1671-7627(2013)02-0080-06
作者:
曹健伍川董红武侠张引弟程大海
杭州师范大学 有机硅化学及材料技术教育部重点实验室,浙江 杭州 310012
Author(s):
CAO JianWU ChuanDONG HongWU XiaZHANG YindiCHENG Dahai
Key Laboratory of Organosilicon Chemistry and Material Technology of Ministry of Education,Hangzhou Normal University,Hangzhou 310012,China
关键词:
甲基三乙氧基硅烷 伍尔兹反应 邻、间、对苯甲基甲基二乙氧基硅烷 正交试验
Keywords:
methyltriethoxysilane Wurtz reaction o-m-p-tolylmethyldiethoxysilane orthogonal experiment
分类号:
O627.41+3
DOI:
10.3969/j.issn.1671-7627.2013.02.016
文献标志码:
A
摘要:
以甲基三乙氧基硅烷、金属Na、邻氯甲苯、间氯甲苯或对氯甲苯为原料,通过伍尔兹反应合成邻、间和对位苯甲基官能化的甲基二乙氧基硅烷,利用傅里叶红外光谱(FT-IR)、核磁共振仪(NMR)、气相色谱-质谱联用仪(GC-MS)等手段对产物结构进行表征。通过正交试验方法考察反应温度、原料滴加时间、原料物质的量之比等因素对目标产物产率的影响,利用方差分析确定各个反应的最佳反应条件。结果表明:温度对3种产物的产率影响都是显著的,而原料滴加时间和物质的量之比对3种产物产率影响均不显著,利用密度-折射率联用仪测定得到25 ℃时3种产物的密度分别为0.962 43、0.950 55和0.948 87 g/cm3,折射率分别为1.476 18、1.469 88和1.470 69。
Abstract:
The o-,m- and p-tolylmethyldiethoxysilane were prepared from the Wurtz reaction of methyltriethoxysilane,sodium and o-chlorotoluene or m-chlorotoluene or p-chlorotoluene,and characterized by Fourier transform infrared spectrometry(FT-IR),gas chromatography-mass spectrometry(GC-MS)and nuclear magnetic resonance(NMR).The orthogonal design method was used to investigate the influences of the molar ratio among the feed stocks,the reaction temperature and the feeding time on the yield of the final product.The optimum conditions in the preparation of each chemical were determined through the variance analysis.The results indicated that the yields of these three compounds were significantly influenced by the reaction temperature while insignificantly affected by the feeding time and the molar ratio between the feed stocks.The densities and the refractive indexes of these three compounds were simultaneously measured by the density-refraction index analyzer at 25 ℃. Results were 0.962 43,0.950 55, and 0.948 87 g/cm3 for densities,and 1.476 18,1.469 88, and 1.470 69 for refractive index,respectively.

参考文献/References:

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备注/Memo

备注/Memo:
收稿日期:2012-04-18
基金项目:浙江省自然科学基金(Y4090016); 杭州市科技局科技创新基金(20100331T17); 浙江省公益技术应用研究(2011C21026)
作者简介:曹健(1985—),男,山东潍坊人,硕士,主要研究方向为有机硅特种单体; 伍川(联系人),研究员,E-mail:chaunwu@yahoo.com..
更新日期/Last Update: 2013-03-31