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Preparation method of tris(tri-bromophenoxy) triazine

A technology of tribromophenoxy and tribromophenol, applied in the field of preparation of tritriazine, can solve the problems of large solvent loss, side reactions, and high material consumption, and achieves improved product quality and yield, good thermal stability, and reaction mild conditions

Active Publication Date: 2012-02-08
RUDONG JINKANGTAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Since the advent of tris(tribromophenoxy)triazine, although people have continuously improved its synthesis process, the existing synthesis process still has the following problems: using strong alkaline substances such as KOH\NaOH as raw materials will not only corrode production Equipment, and will cause the side reaction of the etherification of tribromophenol itself; carry out in a water reaction system, resulting in the hydrolysis of a part of cyanuric chloride, there is a bottleneck in conversion rate and product purity; adopt cooling crystallization and solvent extraction crystallization method , the solvent loss is large, the product state is poor, there is a lot of dust, the material consumption is high, and the environment is polluted

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Put 1200L of anhydrous chlorobenzene and 600kg of tribromophenol into a dry 2000L reactor, stir at room temperature for 30 minutes, put in 48kg of DMF, and cool the jacket with frozen brine; Cool the brine, and at the same time, add 110.4kg of cyanuric chloride in three batches under the condition of stirring, with an interval of 2 to 3 minutes between each batch. , drain the jacket frozen brine, stop cooling, turn on the steam to keep the kettle temperature at 40-45°C, and keep the temperature at this temperature for 2.5 hours; take a small amount of reaction material liquid and carry out PLC point plate analysis, and the developing agent is petroleum ether: acetic acid Ethyl ester = 20:1, the intermediate point completely disappears, and the reaction is complete; after the reaction, lower the temperature of the kettle to 30-35°C, add 200L deionized water to the reaction kettle, and adjust the pH to 9-9 with 5% NaOH aqueous solution 10. Stir for 5 minutes, re-test PH =...

Embodiment 2

[0026] Put 1350L of anhydrous chlorobenzene and 600kg of tribromophenol into a dry 2000L reactor, stir for 30 minutes at room temperature, put in 54kg of DMF, and cool the jacket with frozen brine; Cool the brine, and at the same time, add 110.0kg of cyanuric chloride in three batches under the condition of stirring, with an interval of 2 to 3 minutes between each batch. , drain the jacket frozen brine, stop cooling, turn on the steam to keep the kettle temperature at 40-45°C, and keep the temperature at this temperature for 2.5 hours; take a small amount of reaction material liquid and carry out PLC point plate analysis, and the developing agent is petroleum ether: acetic acid Ethyl ester=20:1, the intermediate point completely disappears, and the reaction is complete; after the reaction, lower the temperature of the kettle to 30-35°C, add 200L of distilled water to the reaction kettle, adjust the pH to 9-10 with 5% NaOH aqueous solution, Stir for 5 minutes, re-test PH = 9~10...

Embodiment 3

[0029] Put 1275L of anhydrous chlorobenzene and 600kg of tribromophenol into a dry 2000L reactor, stir for 30 minutes at room temperature, put in 60kg of DMF, and cool the jacket with frozen brine; Cool the brine, and at the same time, add 109.65kg of cyanuric chloride in three batches under the condition of stirring, with an interval of 2 to 3 minutes between each batch. , drain the jacket frozen brine, stop cooling, turn on the steam to keep the kettle temperature at 40-45°C, and keep the temperature at this temperature for 2.5 hours; take a small amount of reaction material liquid and carry out PLC point plate analysis, and the developing agent is petroleum ether: acetic acid Ethyl ester = 20:1, the intermediate point completely disappears, and the reaction is complete; after the reaction, lower the temperature of the kettle to 30-35°C, add 160L deionized water to the reactor, and adjust the pH to 9-9 with 5% NaOH aqueous solution 10. Stir for 5 minutes, re-test PH = 9~10, ...

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Abstract

The invention discloses a preparation method of tris(tri-bromophenoxy) triazine. The method comprises steps of: adding anhydrous chlorobenzene and tribromophenol in a mass ratio of 2.0-2.25:1; adding a catalyst DMF with a weight of 8-10% of the tribromophenol; adding cyanuric chloride for three times with stirring at 25-35 DEG C, wherein a molar ratio of the cyanuric chloride to the tribromophenol is 1:3.03-3.05, and insulating at 40-45 DEG C for 2.5 h after addition; after reaction, adding deionized water with a weight of 1 / 6-1 / 8 of the organic solvent at 30-35 DEG C, adjusting a pH to 9-10 with 5% NaOH, stirring, washing and removing a water layer to obtain an organic feed liquid; transferring the washed organic feed liquid to a water azeotropic crystallization apparatus to carry out water azeotropic crystallization, centrifuging to obtain a wet product, drying the wet product at 110-120 DEG C for 4 h, controlling a water content lower than 0.2% to obtain the tris(tri-bromophenoxy) triazine product. The preparation method can reduce energy consumption and material consumption, increase product quality; and the product has good crystallization state and no dust, and is safe and environment friendly.

Description

technical field [0001] The invention relates to a preparation method of a brominated flame retardant product, in particular to a preparation method of tris(tribromophenoxy)triazine. Background technique [0002] The production and use of brominated flame retardants has a history of more than 30 years, and there are about 70 kinds of brominated flame retardants currently produced. Because bromine series flame retardants are traditional varieties in the field of flame retardants, with a prominent status, historical background and performance and price advantages, domestic and foreign researchers are still full of enthusiasm for the development of new products of bromine series flame retardants. [0003] Tris(tribromophenoxy)triazine has the characteristics of heat resistance, light resistance, dialysis resistance, non-migration, and little impact on material properties, and its flame-retardant plastics can be recycled. Features not available. It also utilizes the different a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/30
Inventor 吴昊万学明
Owner RUDONG JINKANGTAI CHEM CO LTD
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