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Preparation method of 2,4-dinitochloro benzene

A technology of dinitrochlorobenzene and p-nitrochlorobenzene is applied in 2 fields, can solve the problems of long reaction time, poor and poor product quality, and the content can only reach 95%, and achieves simplified production process and reduced reaction time. The effect of shortening and improving efficiency

Inactive Publication Date: 2004-07-21
徐德军
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Problems solved by technology

[0002] 2,4 dinitrochlorobenzene is mainly used as raw materials for dyes, pesticides, medicines, etc., and can be used to produce sulfur black dyes, ice dyes, saccharin, dinitrophenol, dinitroaniline, picric acid and other products. The preparation method of 2,4 dinitrochlorinated benzenes has two kinds ("China Chemical Products Encyclopedia" second edition, volume, the 2nd edition in May, 1998, the 840th page), 1, by chlorobenzene with mixed acid Direct nitration, neutralization, washing, and separation to obtain the product. The disadvantage of this process is that the process is complicated, the reaction time is long, the quality of the product obtained is poor, the content can only reach about 95%, and the freezing point is 46.2 ° C; The by-product co-melted oil of o-nitrochlorobenzene is nitrated with mixed acid, the waste acid is separated, neutralized, washed with water and purified by crystallization to obtain the product. The disadvantage of this process is that the quality of the obtained product is poor, and the content can only reach about 95%. Freezing point is 46.2C, and by-product 2,6-oil

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  • Preparation method of 2,4-dinitochloro benzene

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Embodiment Construction

[0007] In the production process of this embodiment, 2,4-dinitrochlorobenzene is obtained through nitration of p-nitrochlorobenzene.

[0008]

[0009] This process operation process, batching ratio: p-nitrochlorobenzene: 98% sulfuric acid: 98% nitric acid=1: 0.9: 0.45, earlier nitric acid and sulfuric acid are mixed in mixed acid pot to make mixed acid, and make it cool. Then add p-nitrochlorobenzene into the reaction pot, cool it to 55-60°C, gradually add the mixed acid, the temperature is controlled at 65-70°C, and drop it in about 4-5 hours, then put the jacket cooling water When the reaction temperature no longer rises, turn on the steam heating, about 1 hour, raise the temperature to 105 ° C, keep warm for 2 hours, take samples to measure the freezing point of the warm product ≥ 47 ° C, when the content is greater than 99%, the nitration reaction is complete, turn off Remove the steam, enter the cooling water, stop stirring, let stand for 1 hour, release the waste nitr...

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Abstract

A process for preparing 2,4-benzene dinitrochloride from nitrochloro-benzene includes nitrifying reacting between said nitrochlorobenzene and the mixture of nitric acid and inorganic at 60-90 deg.C for 5-10 hr to generate 2,4-benzene dinitrochloride, separating out the waste acid at lower layer, and neutralizing to obtain high-purity product.

Description

Technical field: [0001] The invention relates to the field of chemical industry, in particular to a preparation method of 2,4-dinitrochlorinated benzene. Background technique: [0002] 2,4 dinitrochlorobenzene is mainly used as raw materials for dyes, pesticides, medicines, etc., and can be used to produce sulfur black dyes, ice dyes, saccharin, dinitrophenol, dinitroaniline, picric acid and other products. The preparation method of 2,4 dinitrochlorinated benzenes has two kinds ("China Chemical Products Encyclopedia" second edition, volume, the 2nd edition in May, 1998, the 840th page), 1, by chlorobenzene with mixed acid Direct nitration, neutralization, washing, and separation to obtain the product. The disadvantage of this process is that the process is complicated, the reaction time is long, the quality of the product obtained is poor, the content can only reach about 95%, and the freezing point is 46.2 ° C; The by-product co-melted oil of o-nitrochlorobenzene is nitrat...

Claims

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Application Information

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IPC IPC(8): C07C201/14C07C205/11
Inventor 徐德军黄金银王兴国
Owner 徐德军
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