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Method for synthesizing p-dichlorobenzene

A technology of p-dichlorobenzene and dichlorobenzene, 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 the effects of mild reaction conditions, simple process operation, and simple equipment

Inactive Publication Date: 2007-12-12
淮安嘉诚高新化工股份有限公司
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  • Abstract
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AI Technical Summary

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

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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

The invention provides a method for preparing benzene dichloride. It comprises following steps: ventilizing chlorine gas into dichloronitrobenzene with catalyst existance at 150- 260 Deg. C for reaction for 1- 10 hours and getting coarsebenzene dichloride, treating coarse product and getting benzene dichloride. Said catalyst is oxide or azocompound, the amount of said catalyst is 0.1- 15 of that of p-nitrochlorobenzene. The inveiton is characterized by temperate reaction condition, simple operation, simple device, high product purity of 99.5%, and avoid of difficult separation of dichlorobenzene and trichlorobenzene and even tetrachlorobenzene.

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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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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