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Synthesis method of 2,4-binitro-6-bromaniline diazonium salt

A technology of dinitroaniline and a synthesis method, applied in 2 fields, can solve the problems such as not easy and simple operation, large floor space, complicated process, etc., and achieve the effects of shortening production process, improving production efficiency, and simple and convenient process

Inactive Publication Date: 2011-06-15
ZHEJIANG JIHUA GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the current 2,4-dinitro-6-bromoaniline diazonium salt synthesis method, there are cumbersome processes, not easy to operate, a large area required for production, more equipment, high energy consumption and more three wastes, etc. shortcoming

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 210.0g of 60% sulfuric acid into the flask, add 36.6g of 2,4-dinitroaniline under stirring, and beat for 2.0 hours; add 19.2g of bromine, the reaction temperature is 20-25°C, after the addition is completed, the temperature is 20-25°C Keep it for 4.0 hours; add 13.6g of 30% hydrogen peroxide, the reaction temperature is 20-25°C, continue the reaction at this temperature for 4.0 hours, the purity of 2,4-dinitro-6-bromoaniline is 99.09%; add to the above mixture 64.0g of 40% nitrosyl sulfuric acid was reacted at 20-30°C for 2.0-3.0 hours to obtain 2,4-dinitro-6-bromoaniline diazonium salt solution.

[0021] The obtained diazonium salt solution was coupled with 41.2 g of N,N-diethyl-m-acetaniline according to a conventional method, then filtered and washed with water to obtain a dye cake. The dye purity is 93.85%.

Embodiment 2

[0023] Add 313.6g of 50% sulfuric acid into the flask, add 36.6g of 2,4-dinitroaniline under stirring, and beat for 3.0 hours; add 25.8g of sodium bromide, and the reaction temperature is 45-50°C. Keep at ℃ for 4.0 hours; add 25g of 30% hydrogen peroxide, the reaction temperature is 45~50℃, continue to react at this temperature for 4.0 hours, the purity of 2,4-dinitro-6-bromoaniline is 98.55%; add to the above mixture 66.0g of 40% nitrosyl sulfuric acid was reacted at 20-30°C for 2.0-3.0 hours to obtain 2,4-dinitro-6-bromoaniline diazonium salt solution.

[0024] The obtained diazonium salt solution was coupled with 41.2 g of N,N-diethyl-m-acetaniline according to a conventional method, then filtered and washed with water to obtain a dye cake. The dye purity is 93.08%.

Embodiment 3

[0026] Add 460.0g of 30% sulfuric acid into the flask, add 36.6g of 2,4-dinitroaniline under stirring, and beat for 5.0 hours; add 20.0g of bromine, the reaction temperature is 20-25°C, after the addition is completed, the temperature is 20-25°C Keep for 4.0 hours; pass chlorine gas for 4.0 hours, the reaction temperature is 20-25°C, continue to react at this temperature for 4.0 hours after passing chlorine gas, the purity of 2,4-dinitro-6-bromoaniline is 98.45%; Add 66.0 g of 40% nitrosyl sulfuric acid and react at 20-30°C for 2.0-3.0 hours to obtain 2,4-dinitro-6-bromoaniline diazonium salt solution.

[0027] The obtained diazonium salt solution was coupled with 41.2 g of N,N-diethyl-m-acetaniline according to a conventional method, then filtered and washed with water to obtain a dye cake. The dye purity is 92.93%.

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PUM

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Abstract

The invention relates to a synthesis method of 2,4-binitro-6-bromaniline diazonium salt. The synthesis method is characterized in that 2,4-dinitroaniline is used as a raw material; 2,4-binitro-6-bromaniline sulfuric acid solution or suspending liquid is obtained by bromination reaction in an acidic medium; and then diazotization reagent is directly added for diazotization, so as to obtain the 2,4-binitro-6-bromaniline diazonium salt. The synthesis method has the advantages of simple process, low equipment requirement, less three wastes and low energy consumption, and is easy to be industrialized.

Description

technical field [0001] The invention relates to a method for preparing an organic compound, in particular to a method for synthesizing a 2,4-dinitro-6-bromoaniline diazonium salt. technical background [0002] 2,4-Dinitro-6-bromoaniline is an important dye intermediate, and the commonly used process is to bromine 2,4-dinitroaniline in hydrochloric acid medium, and then use chlorine or Sodium chlorate and other oxidants replace bromine in the reaction system and further brominate, and then obtain solid 2,4-dinitro-6-bromoaniline through filtration, washing and drying; the obtained solid 2,4-dinitro- 6-Bromoaniline can obtain diazonium salt under the action of diazotization reagents such as sulfuric acid and nitrosyl sulfuric acid or nitrite. There are disadvantages such as cumbersome process, inconvenient operation, large area required for production, more equipment, high energy consumption and more three wastes. [0003] The Chinese patent with application number CN 200910...

Claims

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Application Information

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IPC IPC(8): C07C245/20
Inventor 简卫陈美芬刘伟
Owner ZHEJIANG JIHUA GROUP
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