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Method for preparing parabromo-phenetole

A technology of bromophenethyl ether and p-bromophenol, applied in the field of organic compound preparation, can solve problems such as low production efficiency, long production time, and many production equipment, and achieve the advantages of improving market competitiveness, avoiding equipment investment, and reducing production costs. Effect

Inactive Publication Date: 2010-12-01
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problems in the existing preparation method are: 1, because the diazotization reaction step needs to use expensive refrigeration pumps to realize, therefore, this method has many production equipment and high cost problems, so it is difficult to reduce the cost; 2, Because the diazotization reaction is an indispensable step in the production process of p-bromophenethyl ether, it is very time-consuming and energy-consuming. Therefore, this method has the problems of long production time and low production efficiency, which is not conducive to the improvement of economic benefits of enterprises.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A preparation method of p-bromophenetole, comprising the following steps:

[0016] (1) Etherification reaction step: in a 50-liter reaction kettle with a heating device, electric stirring, and a thermometer, 10 moles of p-bromophenol, 200 moles of water, and 6.5 moles of diethyl sulfate are successively dropped into, and heated to 55 React at ±2°C, keep this temperature, add 11 moles of sodium hydroxide continuously, keep the reaction for 1 hour after adding sodium hydroxide, stop heating, and the etherification reaction is terminated.

[0017] (2) Water washing step: put 1000 moles of water into the mixed solution obtained after the etherification reaction, stir evenly, leave to stand for stratification, and separate the oil layer.

[0018] (3) Distillation step: the oil layer is distilled to obtain p-bromophenetole product, the content of the bromophenetole product is 96.5%, and the color is less than No. 50 (platinum-cobalt colorimetric).

Embodiment 2

[0020] A preparation method of p-bromophenetole, comprising the following steps:

[0021] (1) Etherification reaction step: drop into 10 moles of p-bromophenol successively, 200 moles of water, 6.5 moles of diethyl sulfate in a 50-liter reaction kettle with a heating device, electric stirring, and a thermometer, and heat to 70 moles while stirring. React at ±2°C, keep this temperature, add 11 moles of sodium hydroxide continuously, keep the reaction for 1 hour after adding sodium hydroxide, stop heating, and the etherification reaction is terminated.

[0022] (2) Water washing step: put 1000 moles of water into the mixed solution obtained after the etherification reaction, stir evenly, leave to stand for stratification, and separate the oil layer.

[0023] (3) Distillation step: the oil layer is distilled to obtain p-bromophenetole product, the content of the bromophenetole product is 96.5%, and the color is less than No. 50 (platinum-cobalt colorimetric).

Embodiment 3

[0025] A preparation method of p-bromophenetole, comprising the following steps:

[0026] (1) Etherification reaction step: drop into 10 moles of p-bromophenol successively, 200 moles of water, 6.5 moles of diethyl sulfate in a 50-liter reaction kettle with a heating device, electric stirring, and a thermometer, and heat to 80 moles simultaneously under stirring. React at ±2°C, keep this temperature, add 11 moles of sodium hydroxide continuously, keep the reaction for 1 hour after adding sodium hydroxide, stop heating, and the etherification reaction is terminated.

[0027] (2) Water washing step: put 1000 moles of water into the mixed solution obtained after the etherification reaction, stir evenly, leave to stand for stratification, and separate the oil layer.

[0028] (3) Distillation step: the oil layer is distilled to obtain p-bromophenetole product, the content of the bromophenetole product is 96.5%, and the color is less than No. 50 (platinum-cobalt colorimetric).

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PUM

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Abstract

The invention relates to a method for preparing parabromo-phenetole. The method comprises the following steps of: (1) etherification reaction: putting parabromo-phenol and diethyl sulfate into a reaction kettle, stirring and heating the mixture, and adding sodium hydroxide by distributing for the reaction; (2) washing: adding water into the mixture after the etherification reaction, uniformly stirring the mixture, standing the mixture to delaminate, and separating produced oily liquid; and (3) distillation: distilling the washed mixture to obtain a parabromo-phenetole product. The preparation method uses the direct etherification reaction to replace a diazotization reaction in a synthesizing step, does not need low-temperature freezing diazotization treatment, and avoids the investment of freezing pump equipment, and thus, the method saves equipment investment, reduces production cost and improves market competitiveness of products, and the quality of the prepared products completely meets the requirements of technical index.

Description

technical field [0001] The invention belongs to the field of preparation of organic compounds, in particular to a method for preparing p-bromophenetole. Background technique [0002] In the industrial production of chemiluminescent light, p-bromophenetole is more and more widely used as an important organic compound. The usual production method of p-bromophenetole is the diazotization reaction. Since the diazotization reaction needs to be carried out at low temperature, cryogenic refrigeration equipment is required. The problems in the existing preparation method are: 1, because the diazotization reaction step needs to use expensive refrigeration pumps to realize, therefore, this method has many production equipment and high cost problems, so it is difficult to reduce the cost; 2, Because the diazotization reaction is an indispensable step in the production process of p-bromophenethyl ether, it is very time-consuming and energy-consuming. Therefore, this method has the prob...

Claims

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Application Information

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IPC IPC(8): C07C43/225C07C41/16
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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