Production method of bromo-3-chloro-5,5-dimethylhydantoin (BCDMH) serving as chemical intermediate

A technology of bromochlorohydantoin and its production method, which is applied in the production field of bromochlorohydantoin, can solve problems such as inability to use, achieve the effects of increasing process steps, easy control of heating temperature, and improving product purity

Active Publication Date: 2013-10-02
河北利仕化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of iron ion, manganese ion and calcium ion in bromochlorohydantoin prepared by this invention is too high, although it can be well used for the preparation of disinfectant, but when it is used as chemical intermediate product to prepare medicine and other products can not be used when

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023]Add 2,700 liters of pure water into a 3,000 liter enamel reaction kettle, then add 231kg ​​of 5,5-dimethylhydantoin and 104.4kg of flaky caustic soda into the reaction kettle, stir and dissolve, and at the same time, pass through the jacket of the reaction kettle below -18°C Cool the frozen brine; stir for 20 minutes. After the material is completely dissolved, the thermometer reads 32°C and the acidity meter reads 13.86. Continue to cool down. When the thermometer reads 11°C, open the bromine valve and add industrial bromine dropwise to the reactor. (The amount of liquid bromine added is 135kg). After the bromine is added dropwise, the reading of the acidity meter is 9.6. Slowly pass chlorine gas into the reactor, and keep the reading of the thermometer at 6-18°C. When the reading of the acidity meter reaches 6.6, the reaction ends , close the chlorine and chilled brine valves.

[0024] Put the material in the reaction kettle into the scraper discharge centrifuge for dr...

Embodiment 2

[0027] Add 2,500 liters of purified water into a 3,000 liter enamel reaction kettle, then add 215kg of 5,5-dimethylhydantoin and 134.4kg of flake caustic soda into the reaction kettle, stir and dissolve, and at the same time, feed -19°C into the reaction kettle jacket The following frozen brine is cooled; stir for 23 minutes, the material is completely dissolved, the thermometer reads 35°C, and the acidity meter reads 14; continue to cool down, when the thermometer reads 11°C, open the bromine valve and add bromine dropwise to the reactor (the amount of liquid bromine added is 180kg), after the bromine is added dropwise, the reading of the acidity meter is 9.75, and chlorine gas is slowly passed into the reaction kettle, and the reading of the thermometer is kept at 6-18°C. When the reading of the acidity meter reaches 6.49, the reaction is over. Close the chlorine and chilled brine valves.

[0028] Put the reaction material obtained in the reaction kettle into the scraper dis...

Embodiment 3

[0031] Add 2,800 liters of pure water into a 3,000 liter enamel reaction kettle, then add 301.5kg of 5,5-dimethylhydantoin and 188.4kg of flaky caustic soda into the reaction kettle, stir and dissolve, and at the same time, feed -18 Cool the frozen brine below ℃; stir for 30 minutes, the material is completely dissolved, the thermometer reads 33 ℃ and the acidity meter reads 13.86; continue to cool down, when the thermometer reads 9 ℃, open the bromine valve and add bromine dropwise to the reactor (the amount of liquid bromine added is 180kg), when the reading of the acidity meter is 9.59 after the addition of bromine, slowly pass chlorine gas into the reactor, and keep the reading of the thermometer at 6-18°C. When the reading of the acidity meter reaches 6.57, the reaction is over , close the chlorine and chilled brine valves.

[0032] Put the reaction material obtained in the reaction kettle into a scraper discharge centrifuge for drying operation, the drying time is 20 min...

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PUM

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Abstract

The invention discloses a production method of bromo-3-chloro-5,5-dimethylhydantoin (BCDMH) serving as a chemical intermediate. The production method comprises the following steps that A, 5,5-dimethylhydantoin, flake caustic soda, liquid bromine and chlorine react; a reaction material is obtained; B, the reaction material is subjected to centrifugal spin-drying by a scraper bottom unloading centrifuge, subjected to centrifugal washing by deionized water, and spin-dried; a wet product after centrifugal treatment is dried to form a dry product; and C, the dry product is dissolved by acetone, and filtered; after the deionized water is added for diluting and cooling, BCDMH is separated through crystallization; and the dried wet product is BCDMH capable of serving as a chemical oxidizing agent. The content of BCDMH prepared by the method reaches above 99.3%; the content of bromine is 32.85%; the content of chlorine is 14.70%; a trichloromethane insoluble substance is less than or equal to 0.03%; iron ions are less than or equal to 8mg/kg; calcium ions are less than or equal to 24mg/kg; and BCDMH can serve as the chemical intermediate.

Description

technical field [0001] The invention relates to a production method of bromochlorohydantoin, in particular to a production method of bromochlorohydantoin used as a chemical intermediate. Background technique [0002] Hydantoin compounds refer to five-membered heterocyclic compounds containing various substituents, also known as hydantoin compounds, and their derivatives can be used as intermediates for the synthesis of pharmaceutical products, disinfection, sterilization and algicides, and photosensitive materials. In 1861, German chemist Baeyer discovered hydantoin for the first time in his research on uric acid, and synthesized hydantoin for the first time in 1864. In 1870, Strecker determined the structure of hydantoin. In 1950, Ware made hydantoin and its many derivatives. A comprehensive literature summary is provided. In 1975, Europe began to use dibromohydantoin as a disinfectant for swimming pool water. Almost at the same time, a kind of bromochlorohydantoin produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/82
Inventor 李武成周保良李爱军赵晓利娄献之李丽敏李伟光
Owner 河北利仕化学科技有限公司
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