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有机硅对称分子的制备与应用研究
李培
Subtype硕士
Thesis Advisor高林
2015-05-22
Degree Grantor中国科学院大学
Place of Conferral北京
Degree Discipline材料工程
Keyword有机硅单体 三甲基氯硅烷 二甲基一氯硅烷 六甲基二硅氧烷 六甲基二硅氮烷 四(二甲基硅氧基)硅烷
Abstract

Rochow反应合成有机硅单体这一生产技术的发明,大大促进了有机硅工业的快速发展。国内外生产有机硅单体主要产物为二甲基二氯硅烷,其他副产物如三甲基氯硅烷产量较少,尤其是二甲基一氯硅烷几乎没有。但是,我们的生产装置通过独特的设计,生产二甲基二氯硅烷的同时可产出大量高纯度的三甲基氯硅烷和二甲基一氯硅烷。因此,利用三甲基氯硅烷和二甲基一氯硅烷进行合成及应用研究,对实现其利用价值有很重要的意义。本文分别从三甲基氯硅烷和二甲基一氯硅烷出发合成了六甲基二硅氧烷、六甲基二硅氮烷以及四(二甲基硅氧基)硅烷,并且通过正交实验均筛选出了最佳反应条件。三甲基氯硅烷水解制备六甲基二硅氧烷的最优工艺条件为:反应温度25℃、反应时间30min、水:三甲基氯硅烷体积比1:1、0.40molNaOH;三甲基氯硅烷进行氨化反应制备六甲基二硅氮烷的最优工艺条件为:三甲基氯硅烷:六甲基二硅氧烷体积比1:5、反应温度35℃、反应时间4h、NaOH浓度0.40mol/L;利用二甲基一氯硅烷制备四(二甲基硅氧基)硅烷的最佳工艺条件为:反应温度20℃、反应时间2.5h、四氯化硅和二甲基一氯硅烷摩尔比1:7.5、四氯化硅和水摩尔比1:5。通过重复最佳工艺条件验证了上述实验均有较好的重复性和稳定性。

Other Abstract

Rochow reaction is a great way for the synthesis of the organosilicon monomer. It greatly promoted the rapid development of organic silicon industry. However, the main products for domestic and foreign production of organic silicon monomer are dimethyldichlorosilane, other by-products such as trimethylchlorosilane production are only in small scale, especially dimethylchlorosilane almost don’t exist. Our production route feature unique design, with the production of dimethyldichloride silane at the same time, a large number of high purity trimethylchlorosilane and dimethylchlorosilane can also be produced. Further more, the use of trimethylchlor- osilane and dimethylchlorosilane in synthesis and various application is very important. This paper reported the synthesis of hexamethyldisiloxane and hexamethy- ldisilazane with trimethylchlorosilane, and tetrakis(dimethylsilyloxy)silane with dimethylchlorosilane. The optimal reaction conditions were selected by the orthogonal experiment. Trimethylchlorosilane hydrolysis’s optimum process conditions for preparation of hexamethyldisiloxane are as follows: reaction temperature is 25 ℃, reaction time is 30 min, water : trimethylchlorosilane volume ratio is 1:1 and concentration of NaOH is 0.40 mol/L. Trimethylchlorosilane ammonification reaction’s optimum process conditions for preparation of hexamethyldisilazane are as follows: trimethylchlorosilane : solvent volume is 1:5, water bath temperature is 35 ℃, reaction time is 4 h, concentration of NaOH is 0.40 mol/L. Dimethylchlorosilane hydrolysis’s optimum process conditions for preparation of tetrakis(dimethylsilyloxy)silane are as follows: reaction temperature is 20 ℃, reaction time is 2.5 h, silicon tetrachloride : dimethylchlorosilane mole ratio is 1:5, silicon tetrachloride : water mole ratio is 1:5. Repeating experiments of the designed process and optimal conditions proved the experiment above have great repeatability and the process is viable for industrial application.

Document Type学位论文
Identifierhttp://ir.xjipc.cas.cn/handle/365002/4233
Collection资源化学研究室
Affiliation中国科学院新疆理化技术研究所
Recommended Citation
GB/T 7714
李培. 有机硅对称分子的制备与应用研究[D]. 北京. 中国科学院大学,2015.
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