Preparation method of 5-amino-1, 2, 3-benzene tricarboxylic acid

Abstract

The invention belongs to the technical field of fine chemicals, and particularly relates to a preparation method of 5-amino-1, 2, 3-benzene tricarboxylic acid, which comprises the following steps of: dissolving 1, 2, 3-benzene tricarboxylic acid in a nitric acid environment; reacting a nitric acid solution containing 1, 2, 3-benzene tricarboxylic acid with sulfuric acid to obtain 5-nitro-1, 2, 3-benzene tricarboxylic acid; dissolving the 5-nitro-1, 2, 3-benzene tricarboxylic acid in methanol; reacting the obtained mixed solution with hydrogen; and filtering, concentrating, recrystallizing and refining the reaction product to obtain 5-amino-1, 2, 3-benzene tricarboxylic acid. According to the preparation method of the 5-amino-1, 2, 3-benzene tricarboxylic acid, a micro-channel reactor has the characteristics of small liquid holdup, high heat exchange efficiency, good mass transfer efficiency and the like, so that the problems of mass transfer, heat exchange, safety and the like in nitration reaction and catalytic hydrogenation reaction can be effectively solved, and the safety is greatly improved. The nitration reaction and the nitro reductive ammoniation reaction can be continuously synthesized, the reaction can be started and stopped at any time, the amplification effect is avoided, and an effective method is provided for industrial safety production.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of 5-amino-1,2,3-benzenetricarboxylic acid. Background technique [0002] Aminobenzoic acid compounds are an important class of fine chemical intermediates, which are widely used in the preparation of pharmaceutical chemicals and MOFs materials. 5-Amino-1,2,3-benzenetricarboxylic acid is an important aminobenzoic acid compound, and its preparation is mainly based on 1,2,3-benzenetricarboxylic acid as raw material, after nitration reaction and nitro reductive amination The two-step reaction finally yields 5-amino-1,2,3-benzenetricarboxylic acid. [0003] There are two main methods for the first step nitration reaction: concentrated sulfuric acid-potassium nitrate method and concentrated sulfuric acid-concentrated nitric acid method. In the patent CN106187741A, 1,2,3-benzenetricarboxylic acid is used as raw material, and the concentrated su...

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Problems solved by technology

[0005] As can be seen from the existing literature, in the process of preparing 5-amino-1,2,3-benzenetricarboxylic acid, the two steps of nitration reaction and nitro reductive amination all adopt the traditional batch preparation method, nitration reaction and Catalytic hydrogenation is a dangerous chemical process under the national key supervision. The traditional method is difficult to control the amount of reaction materials, reaction temperature and pressure, and there are great safety hazards

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