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Method for co-producing m-toluic acid nitride and isophthalic acid

A technology of toluic acid and isophthalic acid, applied in chemical instruments and methods, preparation of nitro compounds, preparation of organic compounds, etc., can solve the problems of large amount of solid waste and low yield of target products, and achieve three wastes. The effect of reducing the amount of rectification, avoiding distillation residues, and improving the yield

Active Publication Date: 2021-03-05
山东友道化学有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The purpose of the present invention is to solve the problems of low yield of target product and large amount of solid waste existing in the prior art, and provide a nitration method with simple process, low equipment investment, environmental protection and good comprehensive benefits for co-production of m-toluic acid and methods for isophthalic acid

Method used

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  • Method for co-producing m-toluic acid nitride and isophthalic acid
  • Method for co-producing m-toluic acid nitride and isophthalic acid
  • Method for co-producing m-toluic acid nitride and isophthalic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080]Put 500 g of concentrated nitric acid with a mass fraction of 92% into a four-necked glass bottle with a volume of 1000 mL, start mechanical stirring, and cool down to -15°C. Slowly add 50 g of crude distillation tower liquid (0.3643 mol moles converted into xylene) into a glass bottle for reaction, keep stirring during the reaction and control the reaction temperature at -15°C, and stop the reaction after 10 minutes to obtain the main product It is the nitration reaction solution of 2-nitro-3-methylbenzoic acid. Through HPLC analysis, the conversion rate of raw materials m-toluic acid, m-methylbenzyl alcohol and m-methylbenzaldehyde is more than 99.5%, and the nitration reaction Liquid was filtered to obtain a filtrate and a filter cake. The filter cake was washed with water and dried to obtain 30.2 g of the product 2-nitro-3-methylbenzoic acid. The above-mentioned filtrate was mixed with water to form a 65wt% nitric acid aqueous solution, then the temperature was raise...

Embodiment 2

[0082] Put 500 g of concentrated nitric acid with a mass fraction of 94% into a four-neck glass bottle with a volume of 1000 mL, turn on mechanical stirring, and cool down to -17°C. Slowly add 66.6g of crude distillation tower liquid (0.4852mol moles converted into xylene) into a glass bottle for reaction, keep stirring during the reaction and control the reaction temperature at -17°C, and stop the reaction after 120 minutes to obtain the main The product is the nitration reaction solution of 2-nitro-3-methylbenzoic acid. Through HPLC analysis, the transformation rate of raw material m-toluic acid, m-methylbenzyl alcohol and m-tolualdehyde is all above 99.0%. The reaction solution was filtered to obtain a filtrate and a filter cake. The filter cake was washed with water and dried to obtain 41.3 g of the product 2-nitro-3-methylbenzoic acid. The above filtrate was mixed with water to form a nitric acid aqueous solution with a concentration of 45wt%, and then the temperature was...

Embodiment 3

[0084] Put 500 g of concentrated nitric acid with a mass fraction of 96% into a four-neck glass bottle with a volume of 1000 mL, turn on mechanical stirring, and cool down to -17.8°C. Slowly add 74.7g of crude distillation tower liquid (0.5443mol moles converted into xylene) into a glass bottle for reaction, keep stirring during the reaction and control the reaction temperature -17.8°C, and stop the reaction after 35 minutes to obtain the main The product is the nitration reaction solution of 2-nitro-3-methylbenzoic acid. Through HPLC analysis, the transformation rate of raw material m-toluic acid, m-methylbenzyl alcohol and m-tolualdehyde is all above 99.0%. The reaction solution was filtered to obtain a filtrate and a filter cake. The filter cake was washed with water and dried to obtain 47.1 g of the product 2-nitro-3-methylbenzoic acid. The above filtrate was mixed with water to form a 30wt% aqueous solution of nitric acid, then stirred and heated to 85° C., and reacted at...

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Abstract

The invention discloses a method for co-producing m-toluic acid nitride and m-phthalic acid. The method takes a coarse distillation tower bottom liquid in an m-toluic acid production process as a rawmaterial and comprises the following steps: (1) adding the coarse distillation tower bottom liquid into nitric acid for reaction to obtain a nitration reaction solution; (2) filtering the nitration reaction solution obtained in the step (1) to obtain a first filtrate and a first filter cake, and washing and drying the first filter cake to obtain a product 2-nitro-3-methyl benzoic acid; (3) mixingthe first filtrate obtained in the step (2) with water to obtain a nitric acid aqueous solution, and carrying out an oxidation reaction to obtain a nitric acid oxidation reaction solution; and (4) crystallizing and filtering the nitric acid oxidation reaction solution obtained in the step (3) to obtain a second filtrate and a second filter cake, and refining the second filter cake to obtain the products 2-nitro-3-methyl benzoic acid, 2-nitro-5-methyl benzoic acid, 3-methyl-4-nitro benzoic acid and isophthalic acid. The method has the advantages of simple process, low equipment investment, environmental protection and good comprehensive benefits.

Description

technical field [0001] The invention relates to the technical field of fine chemical industry, in particular to a method for co-producing m-toluic acid nitrates and isophthalic acid by using crude distillation tower liquid in the production process of m-toluic acid as raw material. [0002] technical background [0003] One of the important industrial uses of m-toluic acid is the production of 2-nitro-3-methylbenzoic acid, 3-methyl-4-nitrobenzoic acid and 2-nitro-5-methylbenzene by nitration reaction Formic acid, the chemical reaction that takes place is: [0004] [0005] 2-nitro-3-methylbenzoic acid is the core starting material for the production of the blockbuster insecticides chlorantraniliprole and cyantraniliprole, and 3-methyl-4-nitrobenzoic acid is the production of clinically effective antihypertensive agents The core starting material of the first-line drug telmisartan, 2-nitro-5-methylbenzyl is also the core starting material for the production of many importa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/57C07C51/27C07C63/24
CPCC07C51/27C07C201/08C07C63/24C07C205/57
Inventor 熊振华贺逍俊
Owner 山东友道化学有限公司
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