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A kind of preparation method of three (pentabromophenoxy) isocyanurates

A technology of isocyanurate and pentabromophenoxy, applied in the field of preparation of triisocyanurate, can solve the problem of restricting the market application and industrial production of tris(pentabromophenoxy) isocyanurate, The synthesis steps are cumbersome and the production cost is high, and the effects of saving resources, scientific, reasonable and simple methods and low synthesis costs are achieved.

Active Publication Date: 2022-03-11
WEIFANG YUCHENG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, domestic studies on tris(pentabromophenoxy)isocyanurate and intermediate pentabromophenol are few and rarely reported. At present, there are literatures using pentabromophenol as the starting raw material, which is expensive and the synthesis steps are cumbersome. The production cost is higher, which seriously restricts the market application and industrialized production of tris(pentabromophenoxy)isocyanurate

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  • A kind of preparation method of three (pentabromophenoxy) isocyanurates
  • A kind of preparation method of three (pentabromophenoxy) isocyanurates

Examples

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Effect test

Embodiment 1

[0026] A method for preparing three (pentabromophenoxy) isocyanurates, comprising the following steps:

[0027] 1) preparation of sodium pentabromophenate aqueous solution:

[0028] Add 94g of phenol and 282g of organic solvent dichloromethane into the four-neck flask, then add the catalyst I CuCl 2 0.94g, control the reaction temperature at 0-5°C, start to slowly add 577g of brominating agent bromine chloride dropwise, with the dropwise addition of bromine chloride, the temperature of the system rises slightly, until the dropwise addition is completed, start to raise the temperature to 25°C and keep it warm After reacting for 4 hours, add reducing agent sodium sulfite to remove residual brominating agent, and reclaim the solvent under reduced pressure to obtain pentabromophenol material; after dissolving the pentabromophenol material with 400 g of a mass concentration of 10% sodium hydroxide solution, filter to remove insoluble impurities After that, an aqueous solution of s...

Embodiment 2

[0032] A method for preparing three (pentabromophenoxy) isocyanurates, comprising the following steps:

[0033] 1) preparation of sodium pentabromophenate aqueous solution:

[0034] Add 94g of phenol and 658g of organic solvent dichloroethane in the four-neck flask, then add the catalyst ⅠAlCl 3 4.7g, control the reaction temperature at 0-5°C, start to slowly add 634.7g of bromide bromine chloride dropwise, with the dropwise addition of bromine chloride, the temperature of the system rises slightly, until the dropwise addition is completed, start to raise the temperature to 30°C After insulation reaction 6h, add reductive agent sodium bisulfite to remove residual brominating agent, reclaim solvent under reduced pressure, obtain pentabromophenol material; After pentabromophenol material is dissolved with 30% sodium hydroxide aqueous solution with 140g mass concentration, After removing insoluble impurities by filtration, an aqueous solution of sodium pentabromophenolate was o...

Embodiment 3

[0038] Prepare a kind of preparation method of three (pentabromophenoxy) isocyanurates, comprise the following steps:

[0039] 1) preparation of sodium pentabromophenate aqueous solution:

[0040] Add 94g of phenol and 308g of organic solvent chloroform into the four-neck flask, then add the catalyst ISbCl 3 1.5g, control the reaction temperature at 0-5°C, start to slowly add 596g of brominating agent bromine chloride dropwise, with the dropwise addition of bromine chloride, the temperature of the system rises slightly, until the dropwise addition is completed, start to raise the temperature to 26°C to keep the temperature After reacting for 5 hours, add reducing agent sodium pyrosulfite to remove residual brominating agent, and reclaim solvent under reduced pressure to obtain pentabromophenol material; after dissolving pentabromophenol material with 200 g of mass concentration of 20% sodium hydroxide aqueous solution, filter to remove insoluble After removing impurities, an...

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Abstract

The invention relates to a preparation method of tris(pentabromophenoxy)isocyanurate and the preparation method thereof, which solves the technical problems of cumbersome steps, high cost and unfavorable industrial production in the prior art. The present invention provides a kind of preparation method of tris (pentabromophenoxy) isocyanurate, comprises the following steps: 1) preparation of aqueous solution of sodium pentabromophenate: phenol is added in the organic solvent, then add catalyst I, react When the temperature is 0-5°C, start to add the bromination agent dropwise. After the insulation reaction is completed, an aqueous solution of sodium pentabromophenate is made; 2) the preparation of three (pentabromophenoxy) isocyanurates: mix water and catalyst II Add it into a reaction vessel, control the water temperature to 0-5°C, add cyanuric chloride, start to drop the aqueous solution of sodium pentabromophenolate prepared in step 1), then heat up and reflux for reaction, and after cooling to room temperature, tris(pentabromophenate) will be obtained. Phenoxy)isocyanurate white powder. The invention is widely used in the field of flame retardant synthesis.

Description

technical field [0001] The invention relates to the field of flame retardant synthesis, in particular to a preparation method of tris(pentabromophenoxy)isocyanurate. Background technique [0002] Tris(pentabromophenoxy)isocyanurate is a brominated aromatic triazine compound, which is an additive flame retardant product, with a theoretical bromine content of 78%. Its molecular structure is different from that of polybrominated diphenyl ethers. There is a Dioxin problem. In addition to good fluidity, it also improves the flame retardant efficiency, and has good thermal stability and light stability. It is mainly used in ABS and HIPS. Tris (pentabromophenoxy) isocyanurate has high thermal stability, and there are triazine groups in its molecular structure. Triazine group light stabilizers are a new generation of UV absorbers, so they are resistant Optical activity and UV stability, no precipitation and good impact resistance. At the same time, it has the synergistic effect o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/34
CPCC07D251/34
Inventor 吴多坤秦善宝杨效禹郑伟欣王桂福
Owner WEIFANG YUCHENG CHEM