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A kind of preparation method of chloranil

A technology of tetrachlorobenzoquinone and tetrachlorohydroquinone, which is applied in the preparation of quinone oxide, organic chemistry, etc., can solve the problems of low product purity and yield, unsuitable for industrialized production, long reaction time, etc. The effect of short reaction route and easy availability of raw materials

Active Publication Date: 2022-05-03
ZHEJIANG SHENZHOU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has long reaction time, many impurities, low product purity and low yield; and the solvent methanol in this method is also easily oxidized to generate toxic and harmful formaldehyde, which is not suitable for industrial production

Method used

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  • A kind of preparation method of chloranil

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preparation example Construction

[0025] The invention provides a kind of preparation method of chloranil, comprising the following steps:

[0026] Chloroquinone and glacial acetic acid are mixed, and nitric acid or chlorine gas is used as an oxidizing agent to carry out oxidation reaction to obtain chlorobenzoquinone; when the oxidizing agent is chlorine gas, the oxidation reaction is carried out under the condition of the presence of a catalyst.

[0027] The present invention uses glacial acetic acid as a solvent and nitric acid or chlorine as an oxidizing agent to oxidize tetrachloroquine to obtain tetrachlorobenzoquinone. The reaction formula is as follows:

[0028]

[0029] The preparation method of chloranil provided by the present invention will be described in detail below according to the different types of oxidants.

[0030] In the present invention, when the oxidant is nitric acid, specifically, chloranil and glacial acetic acid are mixed, and an oxidation reaction (referred to as the first oxida...

Embodiment 1

[0040] Mix 50g of tetrachlorohydroquinone with 250mL of glacial acetic acid, control the temperature at 10°C, add dropwise 10mL of nitric acid with a concentration of 98wt%, and finish the dropwise addition in 30 minutes, stir and react at 10°C for 1 hour, and monitor the reaction by thin-layer chromatography to complete; The obtained product system was filtered, the obtained filter cake was washed to neutrality, and dried at 60° C. for 10 h to obtain 49.1 g of chlorobenzoquinone with a product purity of 99.2% and a yield of 98.2%.

Embodiment 2

[0042] Mix 50g of tetrachlorohydroquinone with 500mL of glacial acetic acid, control the temperature at 20°C, add 25mL of nitric acid with a concentration of 70wt% dropwise, complete the dropwise addition in 45min, stir and react at 20°C for 0.5h, and monitor the reaction by thin-layer chromatography The obtained product system was filtered, the obtained filter cake was washed to neutrality, and dried at 60° C. for 10 hours to obtain 49.2 g of chloranil, the product purity was 99.1%, and the yield was 98.4%.

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Abstract

The invention provides a preparation method of chloranil, which belongs to the technical field of chemical production. The present invention uses glacial acetic acid as solvent, and glacial acetic acid has certain solubility to tetrachloroquinone, but the solubility to product tetrachlorobenzoquinone is very little, helps to improve product yield; And glacial acetic acid has acidity, when using nitric acid as oxidant , can increase the oxidation of nitric acid. The present invention uses nitric acid or chlorine as an oxidant to oxidize tetrachlorohydroquinone to prepare tetrachlorobenzoquinone. The raw materials are cheap and easy to obtain, the operation method is simple, the reaction route is short, and equipment investment is small, and the production cost has a very high market. Competitive, and the product yield is higher than 98%, no special purification treatment is required, and the final product purity is higher than 99.0%.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a preparation method of chloranil. Background technique [0002] Chlorobenzoquinone, the molecular formula is C 6 Cl 4 o 2 , with a molecular weight of 245.88, golden leafy crystals, and a melting point of 290°C. Chlorobenzoquinone can be used as a dye intermediate and agricultural seed dressing agent, and is an intermediate of pesticides and polymer compounds; Production of Tiloxetin. [0003] The current industrial production method is specifically to use aniline as a raw material, chlorinate it with hydrogen chloride in an anhydrous organic solvent to generate 2,4,6-trichloroaniline, and chlorinate it in anhydrous sulfuric acid at 110°C to obtain Chlorobenzoquinone. The method has harsh reaction conditions and needs to be carried out under anhydrous conditions, which requires extremely high equipment, and the hydrogen chloride gas and anhydrous sulfuric acid ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C46/06C07C50/24
CPCC07C46/06C07C50/24
Inventor 邵振平王荣王炳乾王洪福黄橙橙雷灵芝王友富
Owner ZHEJIANG SHENZHOU PHARMA
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