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Chloranil and preparation method thereof

A technology for tetrachlorobenzoquinone and polychlorinated phenol, which is applied in the field of tetrachlorobenzoquinone and its preparation, can solve problems such as difficulty in ensuring effective supply of tetrachlorobenzoquinone, and achieves stable supply and price, and easy-to-obtain and strong auxiliary raw materials. Environmentally friendly effects

Active Publication Date: 2017-06-20
NANTONG SHUCHUANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The second object of the present invention is to provide a kind of chloranil, to alleviate the problem that chloranil is difficult to ensure effective supply in the prior art

Method used

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Examples

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Effect test

preparation example Construction

[0057] One aspect of the present invention provides a kind of preparation method of chloranil, the method comprises the following steps:

[0058] a) phenol reacts with chlorine to obtain polychlorinated phenol;

[0059] b) reacting polychlorinated phenol with chlorine gas after adding an oxidizing agent in the presence of an organic solvent to obtain the chlorobenzoquinone.

[0060]The preparation method of chlorobenzoquinone provided by the invention uses phenol as a raw material, and can obtain chlorobenzoquinone through a two-step synthesis method. The price of phenol is low and the supply is stable. Using phenol as a raw material can solve the problem that chloranil cannot be produced normally due to the high and unstable prices of p-diphenol and p-aminophenol, and make the supply and price of chloranil more stable. The preparation of chloranil by using phenol as a raw material can reduce the cost of chloranil by 35%-50%.

[0061] In addition, since the present inventio...

Embodiment 1

[0143] Chlorobenzoquinone in the present embodiment is prepared by the following method:

[0144] Step a): Heat and dissolve phenol under stirring at room temperature, and then pass in chlorine gas. The ratio of phenol to chlorine gas is 1mol:4.5mol. The reaction temperature is controlled at 40°C. After the reaction reaches a certain level, detect the concentration of polychlorinated phenol More than 95%, when the reaction raw material phenol is less than 0.5%, stop feeding chlorine gas, obtain the first step reaction intermediate product polychlorinated phenol;

[0145] Introduce nitrogen into the reaction system, replace the chlorine gas in the reaction system, introduce the gas into the gas absorption tower through the vacuum system, and absorb the gas generated in the reaction system with 30% sodium hydroxide;

[0146] Step b): Dissolve the polychlorinated phenol prepared in step a) in an organic solvent composed of methanol and ethyl acetate (the ratio of methanol to ethy...

Embodiment 2

[0150] Chlorobenzoquinone in the present embodiment is prepared by the following method:

[0151] Step a): Dissolve phenol in an organic solvent composed of methanol and ethyl acetate under stirring at room temperature, the ratio of methanol to ethyl acetate is 1:1, the ratio of phenol to organic solvent is 1mol:5L, and then feed chlorine gas , the ratio of phenol to chlorine is 1mol: 4.5mol, and the reaction temperature is controlled at 40°C. After the reaction reaches a certain level, the concentration of detected polychlorinated phenol is greater than 95%, and when the reaction raw material phenol is less than 0.5%, stop feeding chlorine;

[0152] Introduce nitrogen into the reaction system, replace the chlorine gas in the reaction system, introduce the gas into the gas absorption tower through the vacuum system, and absorb the gas generated in the reaction system with 30% sodium hydroxide;

[0153] The temperature of the reaction system was raised to 80°C, and methanol and...

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Abstract

The invention provides chloranil and a preparation method thereof and relates to the field of organic compounds. The method for preparing the chloranil comprises the following steps: a) enabling phenol to react with chlorine so as obtain polychlorophenol; and b) adding oxidation reagents to enable the polychlorophenol to react with chlorine in the presence of an organic solvent, thereby obtaining the chloranil. According to the method, synthesis is performed by taking phenol as a raw material, and the technical problem in the prior art that the chloranil cannot be normally produced because p-diphenol and p-aminophenol are high in price and unstable is solved. According to the method, a two-step synthesis process is adopted, the problems that multiple preparation steps are needed formerly and more wastewater is produced in the process can be solved. The preparation method has the advantages that the raw material cost is low, the process flow is simple, the auxiliary raw materials are readily available, the reacted solvent can be repeatedly used, much wastewater is not produced in the process flow, and the like.

Description

technical field [0001] The invention relates to the technical field of organic compounds, in particular to a chlorobenzoquinone and a preparation method thereof. Background technique [0002] Chlorobenzoquinone is an important industrial intermediate of dyes, medicines and pesticides. In the dye industry, it can be used as a raw material to prepare various high-end dyes such as permanent violet. In the pharmaceutical industry, it can be used in the production of anti-cancer drug iminoquinone and anti-aldosterone drug spironolactone. 2,3,5,6-Tetrachlorobenzoquinone is a golden yellow leaf-like crystal with a melting point of 290°C. Soluble in ether, slightly soluble in alcohol, hardly soluble in chloroform, carbon tetrachloride and carbon disulfide, almost insoluble in cold alcohol and water. [0003] At present, domestic production of 2,3,5,6-tetrachlorobenzoquinone is carried out by hydroquinone chlorination or p-aminophenol chlorination. The above method has the disadva...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/06C07C50/24
CPCC07C37/62C07C46/06C07C50/24C07C39/27
Inventor 郑书岩董红峰韩金亮曹志奎汤庆刚
Owner NANTONG SHUCHUANG PHARMA
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