Method of preparing chloropinacolone by gas-phase photocatalysis chlorination and special device thereof

Abstract

The invention relates to a preparation method of chloropinacolone and a special device thereof. The method comprises the following steps: pinacolone is adopted as a raw material inside a chlorination reaction device and has chlorination reaction with the chlorination gas under the radiation of the light source to obtain the chloropinacolone, the chlorination reaction device comprises a reaction kettle with a heating device, a rectifying column which is arranged above an outlet of the reaction kettle, a gas-phase reactor which is arranged at a chlorination gas access inlet and a condenser, and also comprises a gas-liquid separator and a backflow liquid sealing pipe; and in the reaction kettle, the rectifying raw material gas and the chlorination gas or the chlorination mixed gas are undertaken the gas-phase photocatalysis chlorination reaction inside a gas-phase reactor from top to bottom to generate the chloropinacolone.The method is not only simple and easy, is easy to be industrialized, has low cost, less side product and high conversion rate and can prepare the chloropinacolone with high content, but also the special device for preparing the chloropinacolone is applicable to the industrialized production.

Description

(1) Technical field [0001] The invention relates to a preparation method of chloropinatone and a special device thereof. (2) Background technology [0002] Chlorpinatone is an important pesticide and pharmaceutical intermediate, usually obtained by direct chlorination of pinazone. [0003] At present, industrial production of chloropinatone mostly adopts the low-temperature solvent method, such as Zhang Weimin et al. reported "Synthesis and Application of chloropinatone" ["Henan Chemical Industry", 06, 1993], using methanol as a solvent to dilute the pinaquinone Ketone, or with N 2 Gas diluted Cl 2 Gas, chlorination at a low temperature below 0°C to reduce the formation rate of dichloropinatone; but limited by raw materials and process conditions, usually the product purity is only about 90%, and the content of dichloropinatone is as high as 7% , because the boiling points of dichloropinatone and chloropinatone only differ by 0.6° C., and their properties are similar, it ...

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Problems solved by technology

Reaction exothermic can get rid of rapidly, and process temperature is easy to control; But the content of dichloropinatone still surpasses 2.3% in the product that obtains, can not well solve the raw material cost of downstream products, polychlorides such as dichloropinaone The impact of impurities on the quality of downstream products and the pollution to the environment

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