A kind of preparation method of α-aminotributanone oxime base silane

Abstract

The invention relates to a preparation method of α-aminotributanone oxime silane, comprising the following steps: (1) uniformly mixing butanone oxime with an organic solvent, then evenly adding chloromethyltrichlorosilane dropwise, after the dropwise addition is completed , and reacted at 0-60°C for 1-6 hours; after the reaction, stand and separate layers, neutralize the upper liquid with an organic base, filter off the insoluble matter, and distill under reduced pressure to remove impurities to obtain chloromethyl tributylketoxime Silane; (2) Mix the organic amine and the organic solvent evenly, then evenly drop chloromethyl tributylketoxime silane, after the dropwise addition is completed, react for 2-10 hours at 10-70°C; filter off the insoluble matter, Reduced pressure distillation to remove impurities, that is, too. The invention does not need to add additional acid absorbent, the subsequent separation is simple, and the generation of by-products such as multi-substituted organic amines is less, the utilization rate of the amine is high, and the side reactions of the reaction system are easy to control; the product purity can reach more than 85%, The yield is above 85%.

Description

technical field [0001] The invention relates to a preparation method of amine-hydrocarbyl tributylketoxime silane, in particular to a preparation method of a ketoxime silane crosslinking agent with an amino group connected to the α-position carbon, and belongs to the technical field of organic synthesis. Background technique [0002] Silane crosslinking agent is a polyfunctional silane compound containing hydrolyzable groups, its general formula is R 4-a SiY a , wherein a=3 or 4, R is a carbon functional group, and Y is a hydrolyzable group. It is often used in one-component room temperature vulcanizing silicone rubber for curing and crosslinking. [0003] According to the different small molecules removed during the crosslinking of silicone rubber, it can be roughly divided into decarboxylation type, deketoxime type, dealcoholization type, deamination type, deamidation type, deacetone type and dehydroxylamine type. Different small molecules have different hydrolysis spee...

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Problems solved by technology

[0005] Amino carbon-functional silane is one of the most used silane crosslinking agents, and the room temperature vulcanized silicone rubber cured and cross-linked by it has excellent adhesion. Aminopropyl alkoxysilane is the most common amino carbon-functional silane. Although aminoketoxime silane shows excellent stability and adhesion in room temperature vulcanized silicone rubber, and α-aminoketoxime silane has also been proved to have self-catalytic properties, it has not been widely used due to the complexity of the synthesis process.

[0006] Chinese patent document CN102532186A adopts the method of mixing and heating amino-containing alkoxysilane and organic oxime to remove low-boiling point by-products under reduced pressure to prepare aminoketoxime-based silane, but the alkoxy group is difficult to completely react, thus Affect the storage stability of the product; Chinese patent document CN103342715A provides a kind of preparation method containing aminopropyl organoxime base silane, starts from chloropropyl chlorosilane, first reacts with organic amine to generate aminopropyl aminosilane, and then uses its As the raw material reacts with organic oxime to obtain aminopropyl organic oxime silane, the amount of amine is relatively large and the utilization rate is low, and the reaction conversion rate is not ideal

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