One-pot method for preparing 1,3,5-three (five-bromine benzyl) isocyanurate

A technology of isocyanurate and pentabromobenzyl is applied in the field of preparation of 1,3,5-tris(pentabromobenzyl)isocyanurate brominated flame retardant, which can solve the problem of product yield and The problems of partial content, complex process steps and high energy consumption can achieve the effects of reduced production energy consumption, simplified process steps and high purity

Inactive Publication Date: 2013-02-13
SHANDONG RUNKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing production process not only has complex process steps, poor working environment, partial yield and content of the prepared product, poor thermal stability, high energy consumption, and the generation of waste water and other three wastes, it has brought certain pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Under stirring, add cyanuric acid and sodium carbonate into the organic solvent at a molar ratio of 1:1, and react at a temperature of 50°C under stirring until no bubbles are formed.

[0027] After the reaction is completed, the temperature of the reaction solution is raised to 120°C, and pentabromobenzyl bromide with a molar ratio of cyanuric acid of 3:1 is added, and the reaction is maintained until the reaction solution is white and white suspended crystals appear.

[0028] The reaction material is cooled and crystallized, and the precipitated crystal is subjected to suction filtration, and the solid after suction filtration is washed with water, and then refined with an organic solvent to obtain the product 1,3,5-tris(pentabromobenzyl)isocyanurate , the yield of the product is 95.3%, and the purity is 99.2%.

Embodiment 2

[0030] Under stirring, add cyanuric acid and sodium bicarbonate into the organic solvent toluene at a molar ratio of 1:4, and react at a temperature of 30°C under stirring until no bubbles are formed.

[0031] After the reaction is completed, the temperature of the reaction solution is raised to 100°C, and pentabromobenzyl bromide with a molar ratio of cyanuric acid of 8:1 is added, and the reaction is maintained until the reaction solution is white and white suspended crystals appear.

[0032] The reaction material is cooled and crystallized, and the precipitated crystals are subjected to suction filtration, and the solid after suction filtration is washed with water, and then organic solvents such as toluene, dimethylformamide, dimethylacetamide, ethylene glycol methyl ether, ethyl ether, etc. The product 1,3,5-tris(pentabromobenzyl)isocyanurate was obtained by refining diol ethyl ether with a yield of 95.1% and a purity of 99.0%.

Embodiment 3

[0034] Under stirring, add cyanuric acid and potassium carbonate into the organic solvent dimethylformamide at a molar ratio of 1:0.8, and react at a temperature of 80°C under stirring until no bubbles are formed.

[0035] After the reaction is completed, the temperature of the reaction solution is raised to 10°C, and pentabromobenzyl bromide with a molar ratio of 4:1 to cyanuric acid is added, and the reaction is maintained until the reaction solution is white and white suspended crystals appear.

[0036] The reaction material is cooled and crystallized, the precipitated crystals are subjected to suction filtration, the solid after suction filtration is washed with water, and after suction filtration, it is placed in the organic solvent dimethylformamide, stirred and washed at a temperature of 50°C for 3 hours, and refined to obtain the product 1,3,5-tris(pentabromobenzyl)isocyanurate, the yield of the product is 95.45%, and the purity is 99.29%.

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Abstract

The invention discloses a one-pot method for preparing 1,3,5-three (five-bromine benzyl) isocyanurate. The method comprises the following steps of (1) adding cyanuric acid and alkali or salt of potassium or sodium into organic solvent, and enabling the mixture to react with stirring under the temperature of 0-100 DEG C until no bubbles is generated, wherein the mole ratio of cyanuric acid to alkali or salt of potassium or sodium is 1: (0.5-5); (2) adding five-bromine benzyl bromide into the reaction solution, and enabling the mixture to perform thermal reaction under the temperature of 100-150 DEG C until the reaction solution becomes white and white crystals are generated, wherein the mole ratio of the five-bromine benzyl bromide to the cyanuric acid is (3-10):1; and (3) cooling the reaction material to perform crystallization, and performing suction filtration, washing, suction filtration and purification on the precipitated crystals to obtain the 1,3,5-three (five-bromine benzyl) isocyanurate. By means of the one-pot method, process steps are simplified, product yield is high, production cost is reduced, environmental protection stress is relieved, and the product is high in purity, low in impurity content and high in yield.

Description

technical field [0001] The invention relates to a brominated flame retardant, in particular to the preparation of a 1,3,5-tris(pentabromobenzyl)isocyanurate brominated flame retardant. Background technique [0002] 1,3,5-Tris(pentabromobenzyl)isocyanurate is a new type of high-efficiency and environmentally friendly brominated flame retardant. Its thermal stability is superior to most existing brominated flame retardants, its melting point is higher than 340°C, and its mass loss is not higher than 2% at 350°C, which is rarely among the existing brominated flame retardants It can be widely used in polymer synthetic materials, plastics, fibers, building materials, resins, etc., especially as a flame retardant for HIPS, PBT, ABS and polyolefin engineering plastics, and can be used for flame retardant processing temperature up to 300 Engineering plastics above ℃. The good light stability and anti-ultraviolet ability of this new flame retardant make it have excellent color stab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/34
Inventor 宗先庆崔明亮吴多坤
Owner SHANDONG RUNKE CHEM
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