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Production process of paranitrobenzoyl chloride intermediate

A nitrobenzoyl chloride intermediate and a production process technology, applied in the production process field of p-nitrobenzoyl chloride intermediate, can solve the problems of increased energy consumption, low production efficiency, difficulty in control, etc., and save reaction time , Improve production efficiency, reduce the effect of production

Inactive Publication Date: 2016-01-20
ANHUI GUANGXIN AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are certain deficiencies in the existing several preparation methods: as phosgene and phosphorus oxychloride are highly toxic substances, it is easy to cause harm to personnel safety and the environment; phosphorus pentachloride is a solid, and it is necessary to add a solvent to accelerate the reaction, which is easy Increase impurities and separation operations; when thionyl chloride is used as the chlorination agent, the reaction time is longer, and column distillation is required to remove impurities, increasing energy consumption, etc.
[0005] The existing production process of p-nitrobenzoic acid, an intermediate of p-nitrobenzoyl chloride, is relatively complicated, difficult to control, and generates more impurities, and the reaction time is longer, so the production efficiency is very low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] First add 1.0mol of xylene solution into the reaction kettle, then add 0.5mol of p-nitrotoluene into the xylene solution, and raise the temperature in the reaction kettle to 60°C, which can increase the reaction rate and reduce the late reaction time;

[0025] Then feed 1.0mol of air into the reactor, and keep the pressure in the reactor at 0.1MPa, which can increase the reaction efficiency;

[0026] Add dropwise the vitriol oil of 1.5mol in reactor again, and carry out dripping slowly, and drop time is 30 minutes, and constantly stirs reactor, and rate of addition is 50ml / s, wherein the concentration of vitriol oil is 75%, avoids concentrated Sulfuric acid is over-reacted, and the strong heat release will cause more by-products in the reaction, so it is added slowly, and at the same time, it can avoid high-intensity reactions that cause the reactor to explode;

[0027] Add the NaOH solution of 0.7mol again in the reactor, and the concentration of NaOH solution is 1%, ...

Embodiment 2

[0031] First add 1.1mol xylene solution to the reaction kettle, then add 0.6mol p-nitrotoluene to the xylene solution, and raise the temperature in the reaction kettle to 65°C, which can increase the reaction rate and reduce the late reaction time;

[0032] Then feed 1.0mol of air into the reactor, and keep the pressure in the reactor at 0.5MPa, which can increase the reaction efficiency;

[0033] Add dropwise the vitriol oil of 1.6mol in reactor again, and carry out dripping slowly, and drop time is 35 minutes, and constantly stirs reactor, and rate of addition is 60ml / s, wherein the concentration of vitriol oil is 76%, avoids concentrated Sulfuric acid is over-reacted, and the strong heat release will cause more by-products in the reaction, so it is added slowly, and at the same time, it can avoid high-intensity reactions that cause the reactor to explode;

[0034] Add the NaOH solution of 0.7mol again in the reactor, and the concentration of NaOH solution is 2%, and consta...

Embodiment 3

[0038] First add 1.2mol of xylene solution into the reaction kettle, then add 0.8mol of p-nitrotoluene into the xylene solution, and raise the temperature in the reaction kettle to 70°C, which can increase the reaction rate and reduce the late reaction time;

[0039] Then feed 1.1mol of air into the reactor, and keep the pressure in the reactor at 1.0MPa, which can increase the reaction efficiency;

[0040] Add dropwise the vitriol oil of 1.7mol in reactor again, and carry out dripping slowly, and drop time is 40 minutes, and constantly stirs reactor, and rate of addition is 70ml / s, wherein the concentration of vitriol oil is 77%, avoids concentrated Sulfuric acid is over-reacted, and the strong heat release will cause more by-products in the reaction, so it is added slowly, and at the same time, it can avoid high-intensity reactions that cause the reactor to explode;

[0041] Add the NaOH solution of 1.8mol again in the reactor, and the concentration of NaOH solution is 3%, ...

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PUM

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Abstract

The invention provides a production process of a paranitrobenzoyl chloride intermediate. The production process comprises the following steps that a xylene solution is added to a reaction kettle, then paranitrotoluene is added to the xylene solution, and air is fed into the reaction kettle; concentrated sulfuric acid is drop added to the reaction kettle again; an NaOH solution is added to the reaction kettle; finally, water is added to the reaction kettle, and exhausting, filtering and crystallization are performed, so that the paranitrobenzoyl chloride intermediate is obtained. Materials can be further diluted, products can be separated favorably, and the product yield is improved. With the adoption of the production process, the process is simpler, control is easy, the production amount of impurities is reduced in the production process, the reaction time is saved, and accordingly, the production efficiency is improved.

Description

technical field [0001] The invention relates to the field of plastic fine chemical production, in particular to a production process of a p-nitrobenzoyl chloride intermediate. Background technique [0002] p-Nitrobenzoyl chloride is a medical raw material used to prepare procaine hydrochloride, p-aminobenzoyl glutamic acid and folic acid, etc.; it can be used as a dye raw material to prepare direct dye brown 100 for leather and paper; It can be used to make acid dyes, food additives (milk powder conditioners), color developing agents and organic synthesis intermediates, identification of alcohols, phenolic reagents, etc. [0003] p-Nitrobenzoyl chloride is an important intermediate in the synthesis of folic acid, procaine hydrochloride, N-p-aminobenzoyl-L-glutamic acid and other vitamin pharmaceutical products, and is also widely used in the production of pigments and color developers . Especially in recent years, with the rise of the feed industry and the development of t...

Claims

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Application Information

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IPC IPC(8): C07C205/57C07C201/12
Inventor 过学军胡安胜吴建平高焰兵戴玉婷张军刘长庆徐小兵黄显超朱张
Owner ANHUI GUANGXIN AGROCHEM
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