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Preparation method of azo compounds

A compound and azo-based technology, which is applied in the field of preparation of azo-based compounds, can solve the problems of harsh reaction conditions and environmental protection, and achieve the effects of high reaction temperature, reduced emissions, and mild reaction conditions

Inactive Publication Date: 2017-11-03
SHANGHAI ANOKY GRP +4
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is the defects such as harsh reaction conditions and environmental protection in the preparation method of the existing azo compounds. Therefore, the invention provides a kind of preparation method of the azo compounds, the method reaction conditions are mild (reaction High temperature, can be carried out at room temperature), environmental protection (reduce the discharge of acid water)

Method used

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  • Preparation method of azo compounds
  • Preparation method of azo compounds
  • Preparation method of azo compounds

Examples

Experimental program
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Effect test

Embodiment 1

[0033]

[0034] Drop 50 grams of 98% sulfuric acid into 30 grams of water, stir, add 17.3 grams of o-chloro-p-nitroaniline below 25 ° C, and beat for 30 minutes. Below 20°C, add 32.6 grams of nitrosylsulfuric acid dropwise, and the drop will be completed in about 2-3 hours. After the drop is completed, keep for 2 hours, and wait for coupling after the diazotization is complete. Detection method: Dip a few drops of diazo solution with a glass rod and put it into ice water. The ice water is clear and the potassium iodide test paper turns blue, which means the end point is reached. If the end point is not reached, continue stirring until the end point is reached.

[0035] Add 300ml of bottom water into a 1000ml beaker, add 1 gram of Pingping, 65.76 grams of 48% ruby ​​esterification solution (N,N diacetoxyethyl m-acetamidoaniline), and then add 0.5 gram of sulfamic acid or urea. Lower the temperature below 20°C and add the diazonium salt dropwise. The dropwise addition was c...

Embodiment 2

[0037] Drop 60 grams of 98% sulfuric acid into 28 grams of water, stir, add 17.3 grams of o-chloro-p-nitroaniline below 25 ° C, and beat for 30 minutes. Below 20°C, add 32.6 grams of nitrosylsulfuric acid dropwise, and the drop will be completed in about 2-3 hours. After the drop is completed, keep for 2 hours, and wait for coupling after the diazotization is complete. Detection method: Dip a few drops of diazo solution with a glass rod and put it into ice water. The ice water is clear and the potassium iodide test paper turns blue, which means the end point is reached. If the end point is not reached, continue stirring until the end point is reached.

[0038] Add 400ml of bottom water into a 1000ml beaker, add 1 gram of Pingping, 65.76 grams of 48% ruby ​​esterification solution (N,N diacetoxyethyl m-acetamidoaniline), and then add 0.5 gram of sulfamic acid or urea. Lower the temperature below 20°C and add the diazonium salt dropwise. The dropwise addition was completed in ...

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Abstract

The invention discloses a preparation method of azo compounds. The preparation method of the azo compounds comprises the following steps: (1) in a sulfuric acid aqueous solution with the mass concentration being 60 to 80 percent by weight, performing diazo-reaction on a compound 4 and nitrosyl sulfuric acid to prepare a mixture containing diazo salt as shown in a formula 2, and performing coupling reaction on the mixture and a compound 3 to obtain a compound 1. The method is mild in reaction condition and environmentally-friendly. (The formula is as shown in the description).

Description

technical field [0001] The invention relates to a preparation method of azo compounds. Background technique [0002] As people's awareness of environmental protection increases, the requirements for waste acid water in synthetic dyes are getting higher and higher. The invention reduces the discharge of waste water in the synthesis, saves the cost, and has no influence on the shade and performance improvement of the dye. Contents of the invention [0003] The technical problem to be solved by the present invention is the defects such as harsh reaction conditions and environmental protection in the preparation method of the existing azo compounds, therefore, the invention provides a kind of preparation method of the azo compounds, the method reaction conditions are mild (reaction High temperature, can be carried out at room temperature), environmental protection (reduce the discharge of acid water). [0004] The present invention provides a kind of preparation method of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/01C09B29/085C07C245/20
CPCC09B29/0003C07C245/20C09B29/0836
Inventor 燕美芳顾宇洁韩伟鹏杨建
Owner SHANGHAI ANOKY GRP