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Method for preparing 2,4-toluene dichloride

A dichlorotoluene and production method technology, applied in two fields, can solve problems such as unfavorable separation of reaction products and sodium chloride, uneven distribution of chlorine gas at reaction temperature, easy formation of vortex phenomenon in reaction liquid, etc., so as to improve the distribution of chlorine gas, Facilitate separation and shorten reaction time

Inactive Publication Date: 2004-11-17
株洲化工集团诚信有限公司
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

The synthesis reaction temperature of this method is between 55-65 ° C, and the way of introducing chlorine gas into p-chlorotoluene is an inlet pipe. Due to the high reaction temperature and uneven distribution of chlorine gas, polychlorides in the reaction product The content is high, the reaction yield is only about 70%, and the utilization rate of chlorine gas is only about 80%.
Although the synthesis reaction is carried out under stirring, because the stirring speed is about 60 rpm, the reaction liquid is easy to form a vortex phenomenon, which reduces the residence time of chlorine gas, and the reaction time is as long as more than 20 hours, which increases the energy consumption of the system
Simultaneously, the alkaline cleaning method of the process is carried out in an alkaline cleaning tank. The alkaline cleaning agent used to wash hydrogen chloride in the synthetic reaction product is a sodium hydroxide solution. The material after the alkaline cleaning has free water to exist, so that the layering of the material is not obvious. It is not conducive to the separation of reaction products and sodium chloride, so that the waste liquid containing toxic and harmful substances is directly discharged, which seriously pollutes the environment; in addition, the rectification of this method is carried out in a rectification tower, and the packing selected for the rectification tower is BX type Net wave packing, its film-forming effect is not good, and its rectification yield is only about 85%
To sum up, this method has long reaction time, many by-products, high energy consumption, and the discharge of three wastes is difficult to meet the standards. Improving the process conditions to increase the yield and reduce environmental pollution is the expectation of the manufacturer and the purification of the natural environment.

Method used

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  • Method for preparing 2,4-toluene dichloride

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Embodiment 1

[0017] A kind of production method of 2,4-dichlorotoluene, take p-chlorotoluene, chlorine as raw material, synthesize 2,4-dichlorotoluene through catalytic chlorination, contain synthesis, alkali washing, rectifying steps, add p-chlorotoluene In the reaction kettle with stirring, add catalyst in proportion, heat up, two inlet pipes pass into chlorine gas in p-chlorotoluene simultaneously in proportion, carry out synthesis reaction, its stirring speed is 20 revs / min, the temperature control of synthesis reaction is 35°C, the reaction solution did not form a vortex, and the reaction time was about 13 hours; the reaction product after the reaction was washed with sodium carbonate crystals containing crystal water as an alkali cleaning agent in an alkali cleaning tank, and the reaction product after alkali washing showed obvious Layering, the upper layer is the organic reaction product, the lower layer is the sodium chloride crystal containing crystal water, the organic reaction pr...

Embodiment 2

[0019] A kind of production method of 2,4-dichlorotoluene, take p-chlorotoluene, chlorine as raw material, synthesize 2,4-dichlorotoluene through catalytic chlorination, contain synthesis, alkali washing, rectifying steps, add p-chlorotoluene In the reaction kettle with stirring, add the catalyst in proportion, heat up, and three inlet pipes feed chlorine gas into p-chlorotoluene in proportion to carry out the synthesis reaction. The stirring speed is 30 rpm, and the temperature of the synthesis reaction is controlled at 45 ℃, the reaction solution did not form a vortex, and the reaction time was about 13 hours; the reaction product after the reaction was washed in the alkali washing tank with sodium carbonate crystals containing crystal water as the alkali washing agent, and the reaction product after alkali washing showed obvious separation. layer, the upper layer is the organic reaction product, and the lower layer is the sodium chloride crystal containing crystal water, the...

Embodiment 3

[0021] A kind of production method of 2,4-dichlorotoluene, take p-chlorotoluene, chlorine as raw material, synthesize 2,4-dichlorotoluene through catalytic chlorination, contain synthesis, alkali washing, rectifying steps, add p-chlorotoluene In the reaction kettle with stirring, add catalyzer in proportion, heat up, four inlet pipes pass into chlorine gas in p-chlorotoluene simultaneously in proportion, carry out synthetic reaction, its stirring speed is 40 rev / min, and the temperature control of synthetic reaction is At 40°C, the reaction solution did not form a vortex, and the reaction time was about 13 hours; the reaction product after the reaction was washed in the alkali washing tank with sodium carbonate crystals containing crystal water, and the reaction product after alkali washing showed obvious Layering, the upper layer is the organic reactant containing 2,4-dichlorotoluene, the lower layer is the sodium chloride crystal containing crystal water, the organic reaction...

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Abstract

The invention relates to a process for preparing 2, 4-dichlorotoluene by using p-chlorotoluene, chlorine as raw material for synthesizing 2, 4-dichlorotoluene through catalyzed chloridization, which comprises the steps of synthesizing, alkaline cleaning, rectifying, the synthesizing reaction temperature is between 35-45 deg. C, the alkaline cleaning agent for washing synthetic reaction product in the alkaline cleaning step is sodium carbonate crystal containing crystal water. The invention increases the yield of 2, 4-dichlorotoluene and improves the chlorine distribution status during reaction.

Description

technical field [0001] The invention relates to a production method of 2,4-dichlorotoluene. Background technique [0002] 2,4-Dichlorotoluene is an important chemical raw material, it is a colorless transparent liquid, and its structural formula is CI- Mainly used in organic synthesis, pharmaceutical and dye industries. At present, the main production routes at home and abroad are: [0003] 1. Use p-chlorotoluene and chlorine gas as raw materials, and synthesize it in a batch kettle in the presence of Lewis acid. The method has low selectivity to 2,4-dichlorotoluene in industrial production, and has many by-products, acid waste water, and large catalyst consumption. [0004] 2. Obtained by the isomerization of dichlorotoluene, and the isomerized product is separated by its medium-pore molecular sieve. The production cost of this method is relatively high, and industrial production is difficult. [0005] 3. Using 3-chloro-p-toluidine as raw material, carry out heavy chl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/12C07C25/08
Inventor 侯青麟李波崔永信袁志明刘奇志陈龙曹卓黄忠谢设平
Owner 株洲化工集团诚信有限公司
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