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Bromol production method

A technology of tribromophenol and phenol, which is applied in the field of preparation of tribromophenol, can solve the problems of not specifying the post-treatment method of tribromophenol, reduce the safety of the reaction process, increase the cost of the product, etc., and achieve simple and easy post-treatment procedures. Industrial production, easy to remove effect

Active Publication Date: 2008-07-16
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, this paper does not specifically clarify the aftertreatment method of tribromophenol, the concentration of ethanol in the solvent is as high as 67wt%, and ethanol is easy to volatilize and makes loss big, causes the pollution to environment and reduces recovery, increases the cost of product, in addition because ethanol is easily It is flammable and explosive, which reduces the safety of the reaction process; at the same time, bromine is a highly toxic and highly corrosive drug, which is easy to overflow, and there are also great potential safety hazards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of preparation method of tribromophenol is to add respectively 48.8g (0.5186mol) phenol, 140g dehydrated alcohol, 203.2g30wt% ( That is, the concentration of weight percentage) (1.7929mol) of hydrogen peroxide aqueous solution, the temperature is raised to 30-40°C, under stirring, 320.8g of 40wt% (1.5862mol) of hydrogen bromide aqueous solution is added dropwise, and after about 1.5h, the hydrogen bromide aqueous solution is dripped After the addition, keep the reactant at about 37°C for 10-20 minutes, raise the temperature to 50-60°C, and keep the temperature for 1.5h. Sodium aqueous solution, 5wt% sodium bisulfite aqueous solution and distilled water soak and wash the filter cake, and the filter cake is dried in a vacuum oven at 55°C to obtain tribromophenol (TBP) white needle-like powder with a yield of 98.5% and a melting point of 90-93 ℃.

Embodiment 2

[0023] Change absolute ethanol to 160g, and others are the same as in Example 1, and obtain TBP white needle-like powder with a yield of 96.7%.

Embodiment 3

[0025] Add alkaline substances (such as sodium hydroxide or sodium carbonate, etc.) to the filtrate collected in Example 1 and Example 2 to adjust to PH=7~9, then distill to collect the ethanol fraction between 75~85°C; Add 36.6g (0.3889mol) of phenol, 105g of 64wt% recovered ethanol, and 152.4g of 30wt% (1.3447mol) of hydrogen peroxide solution in the bottle, raise the temperature to 30-40°C, and add dropwise 240.6g of 40wt% hydrogen bromide solution under stirring. (1.1896 mol). Others are the same as in Example 1, and the TBP white powder is obtained with a yield of 98.3%.

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Abstract

The invention discloses a method for preparing a tribromophenol, which is characterized in that bromine is generated by the hydrogen peroxide reaction between a hydrogen bromide and an oxidant, and then the bromine continues to react with a phenol to synthesize a tribromophenol, and the method can be finished with no middle steps. A crude product passes through water, a sodium bicarbonate liquor and a sodium bisulfite liquor, then after the simple treatments of water washing, impurity removal and filtration, the product can be got. The method has the advantages of simple and convenient process, easy operation, high reaction safety, less pollution and simple post processing. The yield ratio can reach to more than 96 percent. The product has a high purity, is easy to realize industrial production and has a strong practicality.

Description

technical field [0001] The invention belongs to a compound having at least one hydroxyl group connected to a carbon atom of a six-membered aromatic ring, and relates to a preparation method of tribromophenol. Background technique [0002] Tribromophenol is an important fine chemical intermediate. With the rapid development of the synthetic materials industry, the demand for flame retardants synthesized from tribromophenol is increasing rapidly, and the domestic and foreign markets are very optimistic. It is one of the fine chemical intermediates with considerable development potential and prospects. The process route of synthesizing tribromophenol by traditional phenol-bromine water oxidation method is long, the yield is low, the reaction has great potential safety hazards, and the pollution is serious. The phenol solvent method developed in recent years, that is, adding a certain solvent during the phenol-bromine oxidation reaction process can improve the safety of the rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/27C07C37/62
Inventor 吴学明黄杰叶伦学唐安斌范盈
Owner SICHUAN DONGFANG INSULATING MATERIAL
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