Refining process of paranitrobenzoyl chloride intermediate

A technology of nitrobenzoyl chloride intermediate and refining method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as increased energy consumption, difficulty in control, long reaction time, etc., and achieve reaction saving time, improve production efficiency, and reduce the amount 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, longer reaction time, and lower product purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 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; Air, and keep the pressure in the reactor to be 0.1MPa; Add 0.8mol of sodium dichromate in the reactor, and carry out constant stirring, reduce the reaction time, improve production efficiency, and reduce the generation of by-products;

[0027] Add the concentrated sulfuric acid of 0.5mol dropwise in the reaction kettle again, and carry out dripping slowly, and the dropping time is 30 minutes, and constantly stirs the reaction kettle, and the dropping speed is 50ml / s, has improved production efficiency, has reduced the generation of by-product ;

[0028] Then stop stirring the reactor, and let it stand for 0.5 days, and keep the temperature in the reactor at 80°C, which can make the material react more completely;

[0029] Add NaOH solution in the reactor again, until the pH in the reactor is...

Embodiment 2

[0034] First add 1.1mol of xylene solution into the reaction kettle, then add 0.6mol of p-nitrotoluene into the xylene solution, and raise the temperature in the reaction kettle to 65°C; Air, and keep the pressure in the reactor to be 0.5MPa; Add 0.9mol of sodium dichromate in the reactor, and keep stirring, reduce the reaction time, improve production efficiency, and reduce the generation of by-products;

[0035] Add the concentrated sulfuric acid of 0.7mol dropwise in the reaction kettle again, and carry out dripping slowly, and the dropping time is 35 minutes, and constantly stirs the reaction kettle, and the dropping speed is 60ml / s, has improved production efficiency, has reduced the generation of by-product ;

[0036] Then stop stirring the reactor, and let it stand for 0.7 days, and keep the temperature in the reactor at 83°C, which can make the material react more completely;

[0037] Add NaOH solution in reactor again, till the pH in reactor is 7, wherein the concent...

Embodiment 3

[0042] 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; air, and keep the pressure in the reactor at 0.8MPa; add 1.0mol of sodium dichromate to the reactor, and keep stirring, which reduces the reaction time, improves production efficiency, and reduces the generation of by-products;

[0043] Add the concentrated sulfuric acid of 0.8mol dropwise in the reaction kettle again, and carry out dripping slowly, and the dropping time is 40 minutes, and constantly stirs the reaction kettle, and the dropping speed is 70ml / s, has improved production efficiency, has reduced the generation of by-product ;

[0044] Then stop stirring the reactor, and let it stand for 0.8 days, and keep the temperature in the reactor at 85°C, which can make the material react more completely;

[0045] Add NaOH solution in reactor again, till the pH in reactor is 7, wherein the c...

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PUM

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Abstract

The invention provides a refining process of a paranitrobenzoyl chloride intermediate. The refining process comprises the following steps that a xylene solution is added to a reaction kettle, then paranitrotoluene is added to the xylene solution, air is fed into the reaction kettle, and sodium dichromate is added to the reaction kettle; concentrated sulfuric acid is drop added to the reaction kettle; stirring of the reaction kettle is stopped, an NaOH solution is added to the reaction kettle until the PH of the reaction kettle is 7; the solution is transferred to a rectifying kettle, the heated solution is heated, nitrogen is fed for exhausting, then the solution after exhausting is cooled, and crystallization is performed, so that the paranitrobenzoyl chloride intermediate is obtained. 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 method for refining p-nitrobenzoyl chloride intermediates. 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 the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C201/16C07C205/57
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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