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Method for synthesizing 2,6-dihydroxytoluene by using waste acid

A technology of dihydroxytoluene and methylaniline, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of a large amount of waste acid and alkali, high production cost, low production capacity, etc., and reduce emissions , Improve product yield, reduce the effect of three wastes treatment cost

Active Publication Date: 2021-08-06
南京美茵生命科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] The yield of this route is higher than that of the above-mentioned several processes, but a large amount of waste acid and waste alkali are produced in the reaction process, activated carbon is used many times in the refining process, there are many waste residues, and the yield is low, the production cost is high, and the production capacity is low.

Method used

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  • Method for synthesizing 2,6-dihydroxytoluene by using waste acid
  • Method for synthesizing 2,6-dihydroxytoluene by using waste acid
  • Method for synthesizing 2,6-dihydroxytoluene by using waste acid

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Experimental program
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Effect test

Embodiment 1

[0047] (1) Preparation of 3-chloro-2-methylaniline sulfate solution: prepare 7kg of sulfuric acid solution with a content of 60%, add 3kg of 3-chloro-2-methylaniline, stir at 30°C for 1 hour until the system is clear; prepare sodium nitrite Aqueous solution: Weigh 1.5kg of sodium nitrite and add it to 3.5kg of water, stir for 0.5h until the system is clarified, feed the two materials at a ratio of 2:1, control the reaction residence time to 10s, and the reaction temperature to 15°C, and the reaction is discharged Then add it directly to 16kg of 40% sulfuric acid aqueous solution (the first batch of reaction is prepared by new concentrated sulfuric acid, and the latter is the sulfuric acid solution extracted by intermediate synthesis, which is used repeatedly for 8 times), keep warm at 55°C for 1.5h, and take a sample to detect the end of the reaction. Add 9 kg of chloroform for extraction, separate the organic phase, which is a chloroform solution of 3-chloro-2 methylphenol, di...

Embodiment 2

[0050] (1) Preparation of 3-chloro-2-methylaniline sulfate solution: prepare 21kg of sulfuric acid solution with a content of 60%, add 9kg of 3-chloro-2-methylaniline, stir at 35°C for 1 hour until the system is clear; prepare sodium nitrite Aqueous solution: Weigh 4.5kg of sodium nitrite and add it to 10.5kg of water, stir for 0.5h until the system is clear, feed the two materials at a ratio of 2:1, control the reaction residence time of 13s, the reaction temperature is 20°C, and the reaction is discharged Then add it directly to 48kg of 40% sulfuric acid aqueous solution (the first batch of reaction is prepared by new concentrated sulfuric acid, and the latter is the sulfuric acid solution extracted by intermediate synthesis, which is used repeatedly for 6 times), keep warm at 50°C for 1.5h, and take a sample to detect the end of the reaction. Add 21kg of toluene for extraction, separate the organic phase, which is a toluene solution of 3-chloro-2-methylphenol, directly enter...

Embodiment 3

[0053] Comparative Experiment

[0054]

[0055] in conclusion

[0056] 1. The production process of the present invention produces 30-40 tons of acidic waste water less than the conventional process for producing one ton of product.

[0057] 2. The post-treatment scheme described in the present invention is not suitable for activated carbon, and the production of one ton of products reduces ~0.5 tons of waste activated carbon slag compared with conventional processes.

[0058] 3. Compared with the conventional process, the process scheme of the present invention can improve the yield by more than 20%.

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Abstract

The invention discloses a method for synthesizing 2,6-dihydroxytoluene by using waste acid mechanically. According to the method, 3-chloro-2-methylaniline is taken as a raw material, an intermediate 3-chloro-2-methylphenol is synthesized through diazotization and hydrolysis, the reaction is optimized in the alkali fusion, acidification and refining processes, the mechanical application of waste acid and a solvent in the reaction and the optimization of a refining scheme are emphatically optimized, the yield is effectively improved, three wastes are reduced, and 2,6-dihydroxytoluene is synthesized. The method provided by the invention greatly reduces the generation of acidic wastewater, better meets the requirement of environmental protection, and effectively increases the yield of the product, and the quality of the product reaches 99.0-99.5%.

Description

technical field [0001] The invention belongs to the technical field of chemical material preparation, and in particular relates to a method for synthesizing 2,6-dihydroxytoluene by mechanical application of waste acid. Background technique [0002] 2,6-Dihydroxytoluene has many important chemical properties, so it has very important applications in the chemical industry and is an indispensable chemical raw material. Its application fields include: medicine, materials, pesticides, dyes, explosives, etc. [0003] Due to the impact of the epidemic, a number of drugs have emerged that can effectively inhibit the new coronavirus, and 2,6-dihydroxytoluene is an important intermediate among them, which plays a very key role and has a very good market prospect in the future. 2,6-Dihydroxytoluene has a good antioxidant effect, and has a good effect in skin care products and targeted drugs, and can be used as an effective intermediate for the synthesis of different products. [0004]...

Claims

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Application Information

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IPC IPC(8): C07C39/08C07C37/02
CPCC07C37/05C07C37/02C07C39/28C07C39/08
Inventor 董海龙朱其军陈夕鹏苏长浩
Owner 南京美茵生命科技有限公司