Preparation method of N-[3-(trimethoxy silicon substrate) propyl] n-butylamine

Abstract

The invention discloses a preparation method of N-[3-(trimethoxy silicon substrate) propyl] n-butylamine. The preparation method comprises the following steps: (1) firstly adding n-butylamine and chloropropyl trimethoxysilane into a reaction kettle for stirring and reaction at 80 to 90 DEG C, thus obtaining a reaction solution containing N-[3-(trimethoxy silicon substrate) propyl] n-butylamine, n-butylamine hydrochloride and excessive n-butylamine; (2) then adding ethylenediamine at 40 to 80 DEG C, carrying out stirring for full replacement reaction of ethylenediamine and the n-butylamine hydrochloride to generate ethylenediamine hydrochloride, stewing the ethylenediamine hydrochloride at 40 to 70 DEG C in a heat preservation manner, and separating liquid, thus obtaining upper reaction liquid containing the N-[3-(trimethoxy silicon substrate) propyl] n-butylamine and n-butylamine and lower reaction liquid containing the ethylenediamine hydrochloride; (3) carrying out vacuum distillation on the upper reaction liquid obtained by liquid separation in the step (2), thus obtaining the N-[3-(trimethoxy silicon substrate) propyl] n-butylamine. The process of the preparation method disclosed by the invention is simple; the yield of an obtained product is 88 percent or more than 88 percent, and the purity is 99 percent or higher than 99 percent.

Description

technical field [0001] The invention relates to the field of organic chemical industry, in particular to a preparation method of N-[3-(trimethoxysilyl)propyl]n-butylamine. Background technique [0002] Silane coupling agent is a very special class of compounds in organosilicon chemistry, because silane coupling agent not only contains carbon functional groups that can react with organic polymers, but also has the characteristics of easy hydrolysis and polycondensation, and can also form The surface chemically bonded silicon functional groups are widely used in various fields of the national economy. N-[3-(trimethoxysilyl)propyl]n-butylamine, as a new type of aminosilane coupling agent, can replace KH-550 for the treatment of inorganic powder and glass fiber and other products, and can significantly improve the The mechanical properties such as hardness and toughness of composite materials can also be used in the fields of textile auxiliaries, adhesives and coating tackifier...

AI Technical Summary

Problems solved by technology

[0003] At present, there are usually two methods for preparing N-[3-(trimethoxysilyl) propyl] n-butylamine: one is to carry out hydrosilylation by hydrogen-containing alkoxysilane and n-butylallylamine. The shortcoming of method is: not only the raw material that adopts and catalyzer are expensive, and the product that obtains has two kinds of isomers and is difficult for separation, causes the purity of N-[3-(trimethoxysilyl) propyl group] n-butylamine to be low, N -[3-(Trimethoxysilyl)propyl]n-butylamine less than 97% pure

The other is the reaction of halohydrocarbyl alkoxysilane and n-butylamine. The shortcoming of this method is: in the reaction solution of this method, the solubility of n-butylamine hydrochloride in n-butylamine is very large, and the Disposal is a relatively big problem. At present, the sodium alkoxide treatment process is generally used to treat n-butylamine hydrochloride, but this process will cause more solid waste and is not friendly to the environment. When sodium alkoxide is introduced, in order to ensure that the reaction liquid The n-butylamine hydrochloride is thoroughly treated, and the amount of sodium alkoxide added is generally excessive. Excessive sodium alkoxide is not easy to remove and affects rectification. The filtrate has an obvious decomposition impurity peak next to the main peak during rectification, which is difficult to pass through. Separation by rectification causes the purity of N-[3-(trimethoxysilyl) propyl] n-butylamine to be low, and the purity of N-[3-(trimethoxysilyl) propyl] n-butylamine is lower than 97%, use sodium alkoxide to process and relate to solid-liquid separation simultaneously, but filter residue all has certain moisture content, and then causes the yield of N-[3-(trimethoxysilyl) propyl group] n-butylamine to be on the low side, The yield of N-[3-(trimethoxysilyl)propyl]n-butylamine is less than 80%