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Method for preparing o-chloro-p-nitroaniline diazosalt

A technology of p-nitroaniline and diazonium salt, which is applied in the direction of organic chemistry, can solve the problems of low pollution of three wastes and low energy consumption, and achieve the effects of reducing manufacturing costs, saving equipment, and eliminating separation procedures

Active Publication Date: 2009-12-30
HANGZHOU JIHUA JIANGDONG CHEMICAL CO LTD
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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 to extend the synthesis process of o-chloro-p-nitroaniline to its diazotization process, thereby obtaining high-quality, low-cost products; the technical method has strong operability, low requirements for equipment, The pollution of the three wastes is small, the energy consumption is low, and it has the conditions to realize industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 15 g of p-nitroaniline into 400 g of 5% hydrochloric acid solution, and beat at 10° C. for 5 hours. Add 0.5g Tween 60 (polyol polyoxyethylene ether), at 15°C, add 200g of 5% sodium hypochlorite solution, heat up to 20°C for chlorination reaction for 5 hours, and obtain o-chloro-p-nitroaniline hydrochloric acid solution or suspension , the content of o-chloro-p-nitroaniline detected by high performance liquid chromatography is 92.2%; 24.5g of 30% sodium nitrite solution is added at 15°C for diazotization reaction, and kept for 2 hours to obtain o-chloro-p-nitroaniline diazonium salt solution.

[0018] The obtained diazonium salt solution was coupled with 35g m-acetamido-N, N-diacetoxyethylaniline according to the prior art method to obtain 53g of disperse red 167:1 (C.I.Disperse Red 167:1) dyestuff, and the yield was 96.45 %.

Embodiment 2

[0020] Add 15 g of p-nitroaniline to 200 g of 10% sulfuric acid solution, add 10 g of acetic acid, beat at 10° C. for 1 hour, and add 0.5 g of polyoxyethylene oleate (polyoxyethylene fatty acid ether ester). At 10°C, add 200g of 5% sodium hypochlorite solution, heat up to 20°C and react for 5 hours to obtain o-chloro-p-nitroaniline hydrochloric acid solution, the content of o-chloro-p-nitroaniline is 93.2% as detected by high performance liquid chromatography; at 10°C Add 25 g of 30% sodium nitrite solution and keep for 2 hours to obtain o-chloro-p-nitroaniline diazonium salt solution.

[0021] The obtained diazonium salt solution was coupled with 35g m-acetamido-N, N-diacetoxyethylaniline according to the prior art method to obtain 53.5g of disperse red 167:1 (C.I.Disperse Red 167:1) dyestuff, yield 97.36 %.

Embodiment 3

[0023] Add 15 g of p-nitroaniline to 200 g of 30% acetic acid solution, add 10 g of phosphoric acid, beat for 3 hours at 10° C., and add 0.3 g of oleic acid polyoxyethylene ether (polyoxyethylene fatty acid ether ester). At 10°C, add 200g of 10% sodium hypochlorite solution, heat up to 20°C and react for 5 hours to obtain o-chloro-p-nitroaniline hydrochloric acid solution, the content of o-chloro-p-nitroaniline is 92.8% as detected by high performance liquid chromatography; 25.2 g of 20% sodium nitrite solution was kept for 2 hours to obtain o-chloro-p-nitroaniline diazonium salt solution.

[0024] The obtained diazonium salt solution was coupled with 35g m-acetamido-N, N-diacetoxyethylaniline according to the prior art method to obtain 53.5g of disperse red 167:1 (C.I.Disperse Red 167:1) dyestuff, yield 97.36 %.

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Abstract

The invention relates to a method for preparing an o-chloro-p-nitroaniline diazosalt and aims to solve a technical problem of extending a process for synthesizing o-chloro-p-nitroaniline into a diazotization process to obtain high-quality and low-cost products. The method comprises the following steps: using paranitroaniline as a raw material to pulp in a 5 to 30 mass percent acid medium; adding a chlorinating agent and a surfactant in an amount of 1 to 5 percent of the dosage of the paranitroaniline for chlorination; and after the chlorination is finished, directly adding a diazotizing agent to complete diazotization to obtain solution of the diazosalt. The molar ratio of the paranitroaniline to the acid medium to the chlorinating agent to the diazotizing agent is 1:2-10:1-1.3:1-1.3. The method has the advantages of simple synthesis method, high yield, small amount of three wastes, and the like.

Description

technical field [0001] The invention relates to a preparation method of an organic compound, in particular to a preparation method of o-chloro-p-nitroaniline diazonium salt. Background technique [0002] O-chloro-p-nitroaniline is a commonly used synthetic raw material for red disperse dyes. When it is used in the synthesis of dyes, it must undergo a diazotization process. At present, the relatively mature diazotization process in China generally uses the solid of o-chloro-p-nitroaniline ( Wet product or dry powder) is further subjected to diazotization reaction after heating and dissolving. The disadvantage of this process is that the raw material of o-chloro-p-nitroaniline used must be purified through cumbersome post-treatment methods. This process inevitably produces A large amount of waste acid and waste water cause industrial pollution and also increase the manufacturing cost of the final product. Contents of the invention [0003] The technical problem to be solved...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C245/20
Inventor 简卫周火良张立富陈美芬陆洪汇
Owner HANGZHOU JIHUA JIANGDONG CHEMICAL CO LTD
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