Synthetic method of 2,6-dibromo-4-nitroaniline diazosalt

The technology of a nitroaniline and a synthesis method is applied in 2 fields, can solve the problems such as insufficient operation, large floor space, complicated process, etc., and achieves the effects of shortening production process, improving production efficiency, and simple and convenient process

Active Publication Date: 2010-03-17
HANGZHOU JIHUA JIANGDONG CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are disadvantages such as cumbersome process, not easy to operate, large floor are

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 220.0 g of 60% sulfuric acid into the flask, add 27.6 g of p-nitroaniline under stirring, and beat for 2.0 hours. Add 35.2g of bromine, the reaction temperature is 20-25°C, and keep at 20-25°C for 4.0 hours after the addition; add 25.0g of 30% hydrogen peroxide, and the reaction temperature is 20-25°C. The reaction was continued at this temperature for 4.0 hours, and the purity of 2,6-dibromo-4-nitroaniline was 99.32%.

[0020] Add 64.0 g of 40% nitrosyl sulfuric acid to the above mixture, and react at 20-30° C. for 2.0-3.0 hours to obtain 2,6-dibromo-4-nitroaniline diazonium salt solution. The obtained diazonium salt solution was coupled with 34.8 g of N-ethyl-N-cyanoethylaniline according to a conventional method, then filtered and washed with water to obtain a dye cake. The dye purity is 98.81%.

Embodiment 2

[0021] Example 2. Add 196.0 g of 50% sulfuric acid into the flask, add 27.6 g of p-nitroaniline under stirring, and beat for 3.0 hours. Add 45.3g of sodium bromide, the reaction temperature is 60-70°C, and keep at 60-70°C for 4.0 hours after the addition; add 48.0g of 30% hydrogen peroxide, and the reaction temperature is 60-70°C. The reaction was continued at this temperature for 4.0 hours, and the purity of 2,6-dibromo-4-nitroaniline was 98.83%.

[0022] Add 70.0 g of 40% nitrosyl sulfuric acid to the above mixture, and react at 20-30° C. for 2.0-3.0 hours to obtain 2,6-dibromo-4-nitroaniline diazonium salt solution. The obtained diazonium salt solution was coupled with 34.8 g of N-ethyl-N-cyanoethylaniline according to a conventional method, then filtered and washed with water to obtain a dye cake. The dye purity is 98.78%.

Embodiment 3

[0024] Add 457.0 g of 30% sulfuric acid into the flask, add 27.6 g of p-nitroaniline under stirring, and beat for 5.0 hours. Add 40.0g of bromine, the reaction temperature is 35-45°C, keep at 35-45°C for 4.0 hours after the addition is completed; pass chlorine gas for 4.0 hours, the reaction temperature is 35-45°C. The reaction was continued at this temperature for 4.0 hours after passing through the chlorine gas, and the purity of 2,6-dibromo-4-nitroaniline was 99.05%.

[0025] Add 70.0 g of 40% nitrosyl sulfuric acid to the above mixture, and react at 20-30° C. for 2.0-3.0 hours to obtain 2,6-dibromo-4-nitroaniline diazonium salt solution. The obtained diazonium salt solution was coupled with 34.8 g of N-ethyl-N-cyanoethylaniline according to a conventional method, then filtered and washed with water to obtain a dye cake. The dye purity is 98.93%.

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PUM

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Abstract

The invention relates to a synthetic method of 2,6-dibromo-4-nitroaniline diazosalt, solving the technical problems of simplified technique and operation, low requirement for production field and equipment, and energy consumption and 'three wastes' reduction. The invention comprises the following steps: using paranitroaniline as a raw material, pulping in sulphuric acid medium at the mass percentof 20% to 98%, adding brominated compound and oxidant for bromination, and directly diazotizing the mixture with the diazotizd agent after bromination to obtain product, wherein the molar ratio of paranitroaniline, sulphuric acid, brominated compound, oxidant and diazotized agent is 1:2.0 to 8.0:1.0 to 2.5:0.4 to 2.5:1.0 to 1.2.

Description

technical field [0001] The invention relates to a preparation method of an organic compound, in particular to a synthesis method of 2,6-dibromo-4-nitroaniline diazonium salt. technical background [0002] 2,6-dibromo-4-nitroaniline is an important dye intermediate, and the commonly used process is to brominate p-nitroaniline in hydrochloric acid medium with bromine, and then use chlorine gas or sodium chlorate, etc. The oxidant replaces bromine in the reaction system and further brominates, and then obtains solid 2,6-dibromo-4-nitroaniline through filtration, washing and drying; the obtained solid 2,6-dibromo-4-nitroaniline Then diazotization reagents such as sulfuric acid and nitrosyl sulfuric acid or nitrite can be used to obtain diazonium salts. There are disadvantages such as cumbersome process, inconvenient operation, large area required for production, more equipment, high energy consumption and more three wastes. Contents of the invention [0003] The technical pr...

Claims

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Application Information

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IPC IPC(8): C07C245/20
Inventor 简卫陈星海陈美芬陆洪汇
Owner HANGZHOU JIHUA JIANGDONG CHEMICAL CO LTD
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