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Synthesis method of 2, 4, 6-tribromophenol

A synthesis method, the technology of tribromophenol, applied in the field of compound synthesis, can solve problems such as difficult transportation and storage, potential safety hazards in production, and easy corrosion of metals, and achieve the effects of low production cost, high safety, and low pollution

Pending Publication Date: 2021-12-10
北京盈诺维科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional method of synthesizing tribromophenol is the bromination reaction between phenol and bromine. Bromine is a highly volatile poisonous and highly corrosive liquid, which is not easy to transport and store, and there are great safety hazards in production.
This process uses organic solvents such as ethanol, and hydrobromic acid is highly corrosive and easily corrodes metals. Its strong reducing property causes it to gradually turn yellowish brown due to free bromine in the air and sunlight, which is not conducive to long-term production. storage of time

Method used

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  • Synthesis method of 2, 4, 6-tribromophenol
  • Synthesis method of 2, 4, 6-tribromophenol
  • Synthesis method of 2, 4, 6-tribromophenol

Examples

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Effect test

Embodiment 1

[0043] This embodiment is a kind of synthetic method of 2,4,6-tribromophenol, such as figure 1 Shown, this synthetic method comprises the steps:

[0044] (a) phenol and metal bromide are dissolved in water to obtain a mixed solution of phenol and metal bromide, which is denoted as the first mixed solution, wherein the concentration of phenol in the mixed solution of phenol and metal bromide is 1mmol / ml, and the metal bromide The concentration of compound is 2mmol / ml; Metal bromide is sodium bromide;

[0045] (b) Under stirring conditions, add bromate solution and hydrochloric acid dropwise into the first mixed solution and react at 20-45°C for 3h, wherein the volume ratio of bromate solution, hydrochloric acid and the first mixed solution is 5:3:10; bromate solution concentration is 2mmol / ml; hydrochloric acid concentration is 36%; bromate is sodium bromate;

[0046] (c) After the reaction is completed, add sodium sulfite to the reaction solution until the light brown color ...

Embodiment 2

[0057] The present embodiment is a synthetic method of 2,4,6-tribromophenol, and the synthetic method comprises the following steps:

[0058] (a) dissolve phenol and metal bromide in water to obtain a mixed solution of phenol and metal bromide, denoted as the first mixed solution, wherein the concentration of phenol in the mixed solution of phenol and metal bromide is 1.2 mmol / ml, and the metal The concentration of bromide is 2.4mmol / ml; the metal bromide is potassium bromide;

[0059] (b) under stirring conditions, add bromate solution and hydrochloric acid dropwise to the first mixed solution and react at 20 to 45 ° C for 2 h, wherein the volume ratio of bromate solution, hydrochloric acid and first mixed solution is 5:2:12; bromate solution concentration is 2.2mmol / ml; hydrochloric acid concentration is 30%; bromate is potassium bromate;

[0060] (c) treat that reaction finishes, in reaction solution, add sodium sulfite to light brown color disappears completely in reactio...

Embodiment 3

[0065] The present embodiment is a synthetic method of 2,4,6-tribromophenol, and the synthetic method comprises the following steps:

[0066] (a) dissolving phenol and metal bromide in water to obtain a mixed solution of phenol and metal bromide, denoted as the first mixed solution, wherein the concentration of phenol in the mixed solution of phenol and metal bromide is 0.8 mmol / ml, and the metal The concentration of bromide is 1.6mmol / ml; the metal bromide is sodium bromide;

[0067] (b) under stirring conditions, add bromate solution and hydrochloric acid dropwise to the first mixed solution and react at 20~45°C for 4h, wherein the volume ratio of bromate solution, hydrochloric acid and first mixed solution is 5:4:8; bromate solution concentration is 1.8mmol / ml; hydrochloric acid concentration is 40%; bromate is sodium bromate;

[0068] (c) treat that reaction finishes, in reaction solution, add sodium sulfite to light brown color disappears completely in reaction solution,...

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Abstract

The invention discloses a synthesis method of 2, 4, 6-tribromophenol, which comprises the following steps: dissolving phenol and metal bromide in water to obtain a mixed solution of phenol and metal bromide, and recording the mixed solution as a first mixed solution; dropwise adding a bromate solution and hydrochloric acid into the first mixed solution for reaction; and after the reaction is finished, adding sodium sulfite into the reaction liquid until the light brown color in the reaction liquid completely disappears, filtering, washing and drying to obtain the 2, 4, 6-tribromophenol. According to the synthesis method disclosed by the invention, the bromide salt is used as a bromine source, so that available resources are fully utilized, and the use of an organic solvent is avoided; after the reaction is finished, a crude product is separated out in a water phase, and a product with enough purity is obtained after simple filtering treatment; according to the process method, the production cost is greatly reduced, meanwhile, potential safety hazards in transportation and production are reduced, and the working environment is improved.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a synthesis method of 2,4,6-tribromophenol. Background technique [0002] 2,4,6-Tribromophenol (TBP) is obtained by bromination of phenol. It is used for flame retardant modification of engineering plastics used in electronics, electrical appliances, textiles, automobiles and other fields. It can be used as epoxy resin and polyurethane polycarbonate , Reactive flame retardants for adhesives and sealants such as phenolic resins, intermediates of new high-performance flame retardants such as brominated polyphenylene ethers, phosphites, phosphates, etc., can be used as preservatives for wood, paper, etc. It can also be used as a component of compound flame retardant in other resins. Tribromophenol is also an important fine chemical intermediate and an upstream raw material for the preparation of tris(2,4,6-tribromophenoxy)-s-triazine and the like. In addition, tribromop...

Claims

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Application Information

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IPC IPC(8): C07C37/62C07C39/27
CPCC07C37/62C07C39/27
Inventor 孙宏伟孙刚张玉芬张立山
Owner 北京盈诺维科技有限公司
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