Method for synthesizing p-dichlorobenzene

A technology of p-dichlorobenzene and p-nitrochlorobenzene, which is applied in the field of synthesis of p-dichlorobenzene, can solve the problems of small scale, difficult separation, and poor product quality, and achieve mild reaction conditions, simple process operation, and simple equipment Effect

Inactive Publication Date: 2009-09-09
淮安嘉诚高新化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Before the 1980s, p-dichlorobenzene was recycled as a by-product of the production of chlorinated benzene in my country. The output was small, the separation was difficult, the product quality was poor, and the scale was small.
However, the reaction mixture contains monochlorinated benzene, o- and para-dichlorinated benzene, trichlorobenzene and even tetrachlorobenzene, which also caused difficulties in separation.
[0003] Therefore, in the literature research, we found that the high-temperature denitrochlorination technology of nitrochlorobenzene can solve the above problems, and there is no literature report on the preparation of p-dichlorobenzene products by high-temperature denitrochlorination of p-nitrochlorobenzene

Method used

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  • Method for synthesizing p-dichlorobenzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 15.8 grams (0.1 moles) of p-nitrochlorobenzene and 0.08 grams of catalyst benzoyl peroxide into the reaction flask, heat to 200 ° C, and feed chlorine gas to react for 6 hours to obtain the crude product of p-dichlorobenzene, which is rectified Column rectification, obtains the product 13.6 grams of purity ≥ 99.5%, yield 93%. The melting point is 52-53°C. The brown-red gas (nitroxyl chloride) produced during the reaction is absorbed with ammonia and ammonium chloride liquid.

Embodiment 2

[0024] Add 15.8 grams (0.1 moles) of p-nitrochlorobenzene and 0.08 grams of catalyst azobisisobutyronitrile into the reaction flask, heat to 200 ° C, and feed chlorine gas to react for 6 hours to obtain the crude product of p-dichlorobenzene. Distillation column rectification, obtains the product 13.8 grams of purity ≥ 99.5%, yield 94%. The melting point is 52-53°C. The brown-red gas (nitroxyl chloride) produced during the reaction is absorbed with ammonia and ammonium chloride liquid.

Embodiment 3

[0026] Add 15.8 g (0.1 mole) of p-nitrochlorobenzene and 0.1 g of catalyst azobisisobutyronitrile into the reaction flask, heat to 150° C., and feed chlorine gas to react for 6 hours to obtain the crude p-dichlorobenzene, which is refined and purified. Distillation column rectification, obtains the product 13 grams of purity ≥ 99.5%, yield 89%. The melting point is 52-53°C. The brown-red gas (nitroxyl chloride) produced during the reaction is absorbed with ammonia and ammonium chloride liquid.

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Abstract

A preparation method of p-dichlorobenzene: in the presence of a catalyst, p-nitrochlorobenzene is passed through chlorine gas at a temperature of 150-260°C for 1-10 hours to react to obtain crude p-dichlorobenzene, crude p-dichlorobenzene p-dichlorobenzene is obtained through post-treatment, and the catalyst is a peroxide or an azo compound, and the amount of the catalyst used is 0.1-1% of the mass of p-nitrochlorobenzene. The technology of the present invention adopts catalytic chlorination, the reaction conditions are milder, the process operation is simple, the equipment is simple and easy, and the product purity reaches 99.5%; it avoids the benzene monochloride, ortho- and meta-position dichlorinated benzene in the synthesis of reaction products in the prior art , trichlorobenzene and even tetrachlorobenzene separation difficulties.

Description

(1) Technical field [0001] The invention relates to a new method for synthesizing p-dichlorobenzene. (2) Background technology [0002] P-dichlorobenzene is mainly used as anti-moth agent, anti-fungal agent and deodorant, and can also be used in engineering plastic polyphenylene sulfide, synthetic pesticide, medicine, dyestuff and synthetic fiber. It is a fine chemical product with a wide range of uses. Before the 1980s, p-dichlorobenzene was recycled as a by-product of the production of chlorinated benzene in my country. The output was small, the separation was difficult, the product quality was poor, and the scale was small. In 1988, after my country introduced refining equipment and technology, domestic production of p-dichlorobenzene embarked on a track of rapid development. And through development and research, the process of producing dichlorobenzene by directional catalytic chlorination of benzene was successfully developed. However, the reaction mixture contains mo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C25/08C07C17/093
Inventor 陈志明陈生荣林士国裴文
Owner 淮安嘉诚高新化工股份有限公司
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