Synthesis method of multi-element tertiary amine

Abstract

The invention discloses a synthesis method of multi-element tertiary amine, wherein the synthesis method comprises the steps: under the action of a catalyst, carrying out methylation reaction on N,N-dimethyl-1,3-propane diamine, N,N,N'-trimethyl-1,3-propane diamine and methanol which serve as reaction raw materials in a microreactor to obtain N,N,N',N'-tetramethyl-1,3-propane diamine, wherein thecatalyst comprises a carrier and an active component loaded on the carrier, the active component is a combination of one or more of aluminum silicate, zinc silicate and calcium silicate and one or twoof tin oxide and antimony oxide. According to the method, N,N-dimethyl-1,3-propane diamine, N,N,N'-trimethyl-1,3-propane diamine and methanol serve as raw materials, the tertiary amine is produced through direct methylation under the catalyst and the microreactor, the reaction route is short, few byproducts are produced, the product is easy to recycle, the reaction time is short, and the conversion rate is high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and specifically relates to a synthesis method of N,N,N',N'-tetramethyl-1,3-propanediamine. Background technique [0002] N,N,N',N'-Tetramethyl-1,3-propylenediamine, referred to as tetramethylpropylenediamine, is used as catalyst for polyurethane foam, microporous elastomer, curing catalyst for epoxy resin, Intermediates for the preparation of quaternary ammonium compounds, etc., have a large market demand. [0003] CN101735068 discloses a kind of with 1,3-propanediol and dimethylamine as raw material, with Cu-Co-Ni / Al 2 o 3 As a catalyst, the method for preparing tetramethylpropylenediamine by mixing and heating with hydrogen produces by-product 3-dimethylaminopropanol, and the conversion rate of tetramethylpropylenediamine is only about 70%; CN110317138 discloses a method based on Paraformaldehyde solution and ethylenediamine are used as raw materials to prepare tetramethylethylene...

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Problems solved by technology

[0003] CN101735068 discloses a kind of with 1,3-propanediol and dimethylamine as raw material, with Cu-Co-Ni / Al 2 o 3 As a catalyst, the method for preparing tetramethylpropylenediamine by mixing and heating with hydrogen produces by-product 3-dimethylaminopropanol, and the conversion rate of tetramethylpropylenediamine is only about 70%; CN110317138 discloses a method based on Paraformaldehyde solution and ethylenediamine are used as raw materials to prepare tetramethylethylenediamine by catalytic hydrogenation. The imine generated by this reaction contains C=N bonds, which are easy to form polymers during the reaction and affect the reaction yield. ; CN109206319 discloses a method for preparing tertiary amines under the action of a catalyst with primary or secondary amines or nitro derivatives and alcohols as raw materials. The reaction of raw materials with low boiling point, the reaction time reaches 24h, and the yield is only about 70%; CN 105481698A discloses a method for the co-production of tetramethylpropylenediamine, which uses protonic acid, Lewis acid or organic carboxylic acid as catalyst , some of the mentioned acids can form salts with amines to affect the catalytic performance, and at the same time obtain difficult high-boilers. At the same time, the reaction time of this method is 3~15h, and the reaction time is long