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A kind of synthetic method of 2,4,6-tribromophenyl allyl ether

A technology of tribromophenyl allyl ether and synthesis method, applied in chemical instruments and methods, ether preparation, ether preparation by ester reaction, etc., can solve the problem of slow etherification reaction process, serious hydrolysis of chloropropene, affecting market application, etc. problems, to avoid the formation of by-products, to avoid hydrolysis, and to facilitate large-scale production.

Active Publication Date: 2021-09-03
WEIFANG YUCHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the industrially produced products use tribromophenol as the starting raw material, and first form tribromophenol sodium salt with sodium hydroxide in water, and then react with allyl chloride. During the preparation process, two-phase reaction, etherification reaction process is slow , hydrolysis of allyl chloride is serious, and the yield of the product obtained is low. The product has deep color and low purity, which seriously affects the market application of the product.

Method used

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  • A kind of synthetic method of 2,4,6-tribromophenyl allyl ether
  • A kind of synthetic method of 2,4,6-tribromophenyl allyl ether

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Embodiment 1

[0025] A kind of synthesis of 2,4,6-tribromophenyl allyl ether, it comprises the following steps successively:

[0026] 1) Synthesis of the ethanol solution of tribromophenol sodium salt:

[0027] Add 94g of phenol, 470g of organic solvent dichloromethane into the four-necked flask, add 0.47g of catalyst I iron powder, and when the reaction temperature is controlled at 15°C, add 346.2g of brominating agent bromine chloride (control the reaction temperature not to exceed 20°C ), heat up to 25°C and then keep the temperature for 4 hours, then remove the catalyst I by filtration, recycle the organic solvent by distillation, and the remaining product is tribromophenol; g After the reaction is complete, the ethanol solution of tribromophenol sodium salt is obtained.

[0028] 2) Synthesis of 2,4,6-tribromophenyl allyl ether:

[0029] Add 0.94 g of dispersant p-octylphenol polyoxyethylene ether and 1.88 g of catalyst II tetramethylammonium chloride to the ethanol solution of tribro...

Embodiment 2

[0031] A kind of synthetic method of 2,4,6-tribromophenyl allyl ether, it comprises the following steps successively:

[0032] 1) Synthesis of the ethanol solution of tribromophenol sodium salt:

[0033] Add 94g of phenol, 940g of ethylene dichloride as the organic solvent, 4.7g of catalyst I tin powder, and control the reaction temperature at 20°C (control the reaction temperature not to exceed 20°C) and add the brominating agent bromine chloride to the four-neck flask After 357.7g, heat up to 30°C and keep warm for 5h, then filter to remove catalyst Ⅰ, distill and recover organic solvent, and the remaining product is tribromophenol; g After the reaction is complete, the ethanol solution of tribromophenol sodium salt is obtained.

[0034] 2) Synthesis of 2,4,6-tribromophenyl allyl ether:

[0035] In the ethanolic solution of tribromophenol sodium salt that step 1) makes, add dispersant sodium dodecylsulfonate 4.7g and catalyzer II tetraethylammonium bromide 9.4g, first be w...

Embodiment 3

[0037] A kind of synthetic method of 2,4,6-tribromophenyl allyl ether, it comprises the following steps successively:

[0038] 1) Synthesis of the ethanol solution of tribromophenol sodium salt:

[0039] Add 94g of phenol, 705g of chloroform as the organic solvent, 2.4g of antimony powder as the catalyst I, and control the reaction temperature at 16°C (control the reaction temperature not to exceed 20°C), add brominating agent to chlorinate After 346.2g of bromine, heat up to 26°C and keep it warm for 5 hours, then filter to remove catalyst Ⅰ, distill and recover the organic solvent, and the remaining product is tribromophenol; then add tribromophenol to the ethanol solution with a mass concentration of 15% sodium ethoxide After 527.4 g of the reaction was completed, an ethanol solution of tribromophenol sodium salt was obtained.

[0040] 2) Synthesis of 2,4,6-tribromophenyl allyl ether:

[0041] Add 2.1 g of dispersing agent sodium dodecylbenzenesulfonate and 3.2 g of catal...

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Abstract

The invention relates to a synthesis method of 2,4,6-tribromophenyl allyl ether, which solves the problem of complex synthesis process, slow process of etherification reaction, serious hydrolysis of allyl chloride, low product yield and dark product color in the prior art , Low purity affects the technical problem of flame retardant performance. The present invention provides a kind of synthetic method of 2,4,6-tribromophenyl allyl ether, it comprises the following steps successively: 1) the synthesis of the ethanol solution of tribromophenol sodium salt: add catalyst in the organic solvent of phenol 1. Add brominating agent at 15-20°C, then raise the temperature to 25-30°C and keep warm to react to obtain tribromophenol; then add tribromophenol to the ethanol solution of sodium ethoxide to obtain the ethanol solution of tribromophenol sodium salt; 2) Synthesis of 2,4,6-tribromophenyl allyl ether: add dispersant and catalyst II to the ethanol solution of tribromophenol sodium salt prepared in step 1), and drop the ethanol solution of allyl chloride , keep warm until the end of the reaction to get 2,4,6-tribromophenyl allyl ether. 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 synthesis method of 2,4,6-tribromophenyl allyl ether. Background technique [0002] There are many kinds of flame retardants with different properties, and they are usually classified according to the method of use and chemical composition. According to different usage methods, flame retardants can be divided into two types: additive type and reactive type. Additive flame retardants are used in polymer processing and are mostly used in thermoplastics. They are characterized by convenient use and wide application, but they may affect the processing performance and mechanical and physical properties of products. Reactive flame retardants have reactive functional groups in their molecules, which are bonded to their molecular chains during polymer synthesis. They are mainly used in thermosetting plastic products. The advantages are that they have little impact on the mecha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/16C07C43/225C07C37/62C07C39/26
CPCC07C37/62C07C41/16C07C43/225C07C39/26
Inventor 吴多坤王东全秦善宝张君营杨丽丽
Owner WEIFANG YUCHENG CHEM
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