论文总字数：19791字

摘 要

在现代生产生活中二硅烷是一类重要的化合物。二硅烷的合成对于低聚硅烷的合成有很大的参考价值。 常规的合成方法是通过Wurtz反应实现的，卤化硅烷在碱存在下脱卤，形成乙硅烷。 虽然这种方法广泛适用，但有很多缺点。 首先，由于在与碱金属反应过程中存在氧原子，最终形成氧硅烷或聚氧乙烷杂质。 其次，卤化硅烷不易保存，反应环境差。 此外，反应条件相对苛刻，反应过程不易控制，环境友好性差，所以本课题研究出一种新的合成二硅烷的方法，通过金属铜化合物作为催化剂，对三取代硅烷进行偶联反应，使有机硅烷直接脱氢，耦合形成二硅烷。相比之前合成二硅烷的方法，此方法反应条件更简单，反应易控制，副产物较少。另外铜类化合物由于制备简单，化学危害性低，经济实惠故作为催化剂可以减少贵重金属的浪费，节约开支，有利于保护环境，符合当前国家提出的可持续发展理念，符合当前所提倡的绿色化学思想。

本篇文章中共筛选了三种铜类化合物作为催化剂进行试验，并在研究过程中，对不同的氧化剂进行筛选，反应体系的溶剂也进行了细致的筛选，最后，对反应各物质的用量进行了细致的调整，最终结果显示，当反应物为MePh₂SiH,以适量氯化亚铜作为催化剂，以适量叔丁基过氧化氢(TBHP)作为氧化剂，以适量N,N-二甲基甲酰胺(DMF)作为溶剂时，可以获得相应的高收率的二硅烷。

关键词：铜 三取代硅烷 偶联反应 二硅烷

Study on Catalytic Silane Coupling Reaction of Copper

ABSTRACT

In modern production life, disilane is a class of important compounds. The synthesis of disilane has a great reference value for the synthesis of oligosilanes. The conventional process for the synthesis of disilane is achieved by the Wurtz reaction, the halogenated silane is dehalogenated in the presence of a base to form a disilane. Although this method is widely applicable. but there are many shortcomings. First, since oxygen atoms are present during the reaction with the alkali metal. a siloxane or polyoxyethane impurity is finally formed. Second. the halogenated silane is not easy to save. The reaction environment is poor. Finally. the reaction conditions are relatively harsh. The reaction process is not easy to control. Poor environmental friendliness. Therefore, this study has developed a new method of synthesizing disilane by coupling the trisubstituted silane through a metal copper compound as a catalyst to directly dehydrogenate the organosilane and form a disilane. Compared with the previous synthesis of disilane method, this method is more simple reaction conditions. In addition, the copper compounds can reduce the waste of precious metals and save the expenses, which is beneficial to the protection of the environment and conform to the sustainable development concept put forward by the current countries. It is in line with the current green chemistry thought.

In this paper, one of the best copper compounds is selected from among the three copper compounds as catalysts. The different oxidants were screened and the solvent of the reaction system was also carefully screened. Tinally. the amount of the reaction of the material was carefully adjusted. The final results show that when the reaction is MePh₂SiH. Appropriate amount of cuprous chloride as the catalyst. Appropriate amount of t-butyl hydroperoxide (TBHP) as the oxidant. The appropriate amount of N,N-dimethylformamide (DMF) as solvent. the corresponding high yield of disilane can be obtained.

Key words: copper; trisubstituted silane; coupling reaction; disilane

目录

摘要 I

ABSTRACT II

第一章 绪论 1

1.1引言

1.2 Cu催化剂

1.2.1 Cu催化剂的优点

1.2.2 Cu催化偶联反应的发展历程

1.2.3 Cu催化剂的应用

1.3二硅烷合成研究现状 4

1.4本课题主要创新点 8

1.5本课题主要研究内容 9

第二章Cu类化合物催化硅烷偶联反应实验 10

2.1引言 10

2.2实验原理 10

2.3实验试剂与仪器 10

2.4实验过程 11

第三章实验结果与讨论 13

3.1筛选Cu类催化剂，氧化剂，溶剂 13

3.2对三取代硅烷自身偶联反应的优化 15

第四章 展望 17

参考文献 18

附 录 20

致谢 26

第一章 绪论

1.1引言

二硅烷和聚硅烷是硅烷之间通过聚合形成Si-Si键而产生的一种高分子材料, 具备各种反应功能基团的有机硅化合物的研究日益受到重视随着研究工作深入,由于含活泼H原子的物质, ,可与含有化学性质较为活泼二功能基的二硅烷类化合物,或反应性聚合物等物质进行化学反应,所以可作为二硅烷基化材料中的试剂, 从而赋予材料的耐热稳定性、光学、电子学方面的特殊性能. 故广泛用于化学材料改性、现代有机合成等。

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