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Electrochemical synthesis method for preparing halogenated hydantoin

A technology of dibromohydantoin and hydantoin, which is applied in the field of preparation of various dibromohydantoin and bromochlorohydantoin high-efficiency disinfection, sterilization and algicides, and can solve the problem of difficult production control of liquid bromine or chlorine, hydantoin Problems such as obvious decomposition and high cost of raw materials are achieved to achieve the effect of convenient and simple feeding operation, cheap and easy-to-obtain raw materials, and high product yield

Inactive Publication Date: 2013-05-15
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above synthetic processes have their own characteristics, but all have some disadvantages, such as high cost of raw materials, or too strong alkalinity of the solution in the early stage of the reaction, and obvious decomposition of hydantoin; or the production control of liquid bromine or chlorine is difficult and highly toxic, and the equipment is severely corroded; Or a large amount of waste water is produced in the production process. In summary, it is meaningful to develop a preparation process with high synthetic yield, good product purity, simple production control, low production cost, and environmentally friendly and pollution-free process.

Method used

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  • Electrochemical synthesis method for preparing halogenated hydantoin
  • Electrochemical synthesis method for preparing halogenated hydantoin

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 30mL of water, 1.28g (0.01mol) of dimethylhydantoin and 1.90g (0.02mol) of magnesium chloride into a 100mL flask, insert an electrode with both the anode and cathode of Pt, connect the circuit, energize and electrolyze, and keep the current at 0.05A (using The electrode area is 1cm 2 ), while stirring, dilute hydrochloric acid was added dropwise in the electrolysis process so that the pH was at 2, electrolysis for 21.5 hours (equal to approximately 4 times the theoretical time value), filtered, washed with water, and dried to obtain 0.49g of product dichlorodimethylhydantoin, the yield 25.0%

Embodiment 2

[0027] Add 30mL of sodium chloride solution with a concentration of 0.2g / mL, 1.28g (0.01mol) of dimethylhydantoin in a 100mL flask, insert an electrode with Au as the anode and C as the cathode, connect the circuit, energize and electrolyze, and keep the current at 0.5A (with an electrode area of ​​1cm 2 ), while stirring, dilute hydrochloric acid was added dropwise in the electrolysis process so that the pH was at 4-5, electrolysis was performed for 10.5 hours (equal to approximately 5 times the theoretical time value), filtered, washed with water, and dried to obtain 1.42 g of product dichlorodimethylhydantoin, Yield 72.3%.

Embodiment 3

[0029] Add 30mL of water, 2.80g (0.01mol) of xylylene hydantoin and 1.90g (0.02mol) of magnesium chloride into a 100mL flask, insert electrodes with both cathode and anode being Pt, connect the circuit, energize and electrolyze, and keep the current at 0.1A ( The electrode area used is 1cm 2 ), while stirring, dilute hydrochloric acid was added dropwise in the electrolysis process so that the pH was at 6-7, and the electrolysis was performed for 10.5 hours (approximately equal to the theoretical time value), filtered, washed with water, and dried to obtain 2.61g of product dichlorodiphenylhydantoin. Rate 75.0%.

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Abstract

The invention relates to an improved synthesis method for hydantoin bromo and for preparing dibromohydantoin or bromo-3-chloro-5,5-dimethylhydantoin. The method comprises the following steps of: taking various hydantoins as raw materials, dissolving the hydantoins and the corresponding amount of bromide in 0.2g / mL saturation chlorate solution, electrolyzing the bromide solution and obtaining the corresponding hypobromite, generating hypobromous acid under the condition of addition of acid, further performing bromo reaction to the hydantoin, adjusting the bromide equivalent according to demand and synthesizing the corresponding dibromohydantoin or bromo-3-chloro-5,5-dimethylhydantoin. Reaction liquid can be repeated and used, and the reaction yield can reach more than 95%. The invention has the advantages of easy obtainment of raw materials by low cost, low production cost, simple post treatment, high yield, good purity and repetitive recycle of the mother liquid. By utilizing the electrolysis process, the process is simple, and the equipment has low requirement, safe operation and no toxicity or stimulation.

Description

1. Technical field [0001] The invention belongs to the synthesis technology of bromohydantoin, and specifically relates to a preparation method for preparing various dibromohydantoin and bromochlorohydantoin high-efficiency disinfection, sterilization and algicides. 2. Background technology [0002] With the development of my country's economy, the acceleration of my country's modernization and urbanization, the large-scale and intensive development of agriculture and animal husbandry, and the rapid and large-scale circulation of livestock and poultry and their products, the infection of various bacteria and viruses has accelerated. The use of disinfectants has greatly increased, and it plays an important role in sterilization and hygiene. [0003] Dihalohydantoin is a high-efficiency disinfection, sterilization and algicide. The most common varieties are dichlorodimethylhydantoin, dibromodimethylhydantoin and bromochlorodimethylhydantoin. In addition to the advantages of h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/06
Inventor 李焰潘怡沛董建强袁振昌陈祖兴
Owner HUBEI UNIV
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