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Production process of high-whiteness and high-thermal-stability bromo-triazine

A technology with high thermal stability and brominated triazine, which is applied in the field of flame retardants, can solve the problems of poor thermal stability and low whiteness of brominated triazine, and achieve the effects of improved purity, low cost and simple process

Inactive Publication Date: 2022-04-15
SHANDONG HAIWANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the above defects, the purpose of the present invention is to provide a production process of bromotriazine with high whiteness and high thermal stability, aiming to solve the technical problems of low whiteness and poor thermal stability of bromotriazine in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 200 kg of deionized water to the reaction kettle, add 320 kg of phenol, add 2200 kg of dichloromethane, stir and mix well, cool the reaction kettle to below 10°C, add bromine dropwise, about 5kg per minute, bromine dropwise After 20 minutes, start to add hydrogen peroxide dropwise (according to the weight ratio of phenol and hydrogen peroxide is 1:2), bromine and hydrogen peroxide are added dropwise at the same time. Decolorization and secondary decolorization, the decolorized organic phase is transferred to the condensation kettle;

[0025] Add 800 kg of deionized water to the condensation kettle, add 428 kg of lye, stir and mix, transfer to the decolorized organic phase, lower the temperature in the kettle to below 10°C, measure the pH of the water phase between 9 and 11, and add the catalyst ( 5kg of triethylamine + 7kg of tetraethylammonium bromide), stirred for 10min, put in 200kg of cyanuric chloride, raised the temperature to the reflux temperature of 39°C, a...

Embodiment 2

[0028] Add 240kg of deionized water to the reaction kettle, add 320kg of phenol, add 2400kg of dichloromethane, stir and mix, the temperature of the reaction kettle is lowered to below 10°C, and bromine is added dropwise at about 4kg per minute. After bromine is added dropwise for 13 minutes, Start to add hydrogen peroxide dropwise (according to the weight ratio of phenol and hydrogen peroxide is 1:3), bromine and hydrogen peroxide are added dropwise at the same time, after the dropwise addition, reflux at 39°C for 3 hours; Decolorization, the decolorized organic phase is transferred to the condensation kettle;

[0029] Add 800kg of deionized water to the condensation kettle, add 420kg of lye, stir and mix well, transfer to the decolorized organic phase, lower the temperature in the kettle to below 10°C, measure the pH of the water phase between 9 and 11, add catalyst (triethyl amine 5kg+tetraethylammonium bromide 8kg), stirred for 10min, put in 200kg cyanuric chloride, raised...

Embodiment 3

[0032] Add 300kg of deionized water to the reaction kettle, add 320kg of phenol, add 2600kg of dichloromethane, stir and mix well, cool down the reaction kettle to below 10°C, add bromine dropwise, about 3kg per minute, after bromine dropwise for 16min, Start to add hydrogen peroxide dropwise (according to the weight ratio of phenol and hydrogen peroxide is 1:4), bromine and hydrogen peroxide are added dropwise at the same time. After the dropwise addition, reflux at 39°C for 3 hours; Decolorization, the decolorized organic phase is transferred to the condensation kettle;

[0033] Add 800kg of deionized water to the condensation kettle, add 440kg of lye, stir and mix well, transfer to the decolorized organic phase, lower the temperature in the kettle to below 10°C, measure the pH of the water phase between 9 and 11, add catalyst (triethyl amine 5kg + tetraethylammonium bromide 10kg), stirred for 10min, put in 200kg cyanuric chloride, raised the temperature to the reflux temper...

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Abstract

The invention discloses a production process of high-whiteness and high-thermal-stability bromotriazine, and relates to the technical field of flame retardants, phenol and an organic solvent are added into a reaction kettle, and then bromine and hydrogen peroxide are added to prepare an intermediate product tribromophenol; according to the method, tribromophenol and cyanuric chloride are catalyzed to react under an alkaline condition by using a compound catalyst to prepare bromo-triazine. The bromo-triazine prepared by the method has high whiteness, high thermal stability, high purity and good product quality.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a production process of bromotriazine with high whiteness and high thermal stability. Background technique [0002] The growth rate of brominated flame retardants is slowing down. This is firstly restricted by environmental protection. Due to the pressure of environmental protection and the uncertainty of future government regulations in various countries, brominated flame retardant manufacturers around the world have expanded the production range of flame retardant products. To consolidate the dominant position of flame retardants. Some traditional brominated flame retardants have been under the pressure of increasingly stringent environmental protection and flame retardant regulations, forcing users to find substitutes for brominated flame retardants, and at the same time promoting the advent of new flame retardant materials. [0003] As a new type of environmentally ...

Claims

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Application Information

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IPC IPC(8): C07D251/30
CPCC07D251/30
Inventor 刘军东冯宝羲于兆令杨新成丁敬一张婧如张晓龙朱林生
Owner SHANDONG HAIWANG CHEM
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