Preparation method of p-bromoethoxybenzene

A technology of bromophenethyl ether and p-bromophenol, which is applied in the field of organic compound preparation, can solve problems such as difficulty in reducing costs, unfavorable economic benefits, and low production efficiency, and achieve the effects of reducing production costs, reducing material input, and convenient operation

Inactive Publication Date: 2010-11-24
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The usual production method of p-bromophenethyl ether is a diazotization reaction. Because the diazotization reaction needs to be carried out at low temperature, low-temperature freezing equipment is needed. The problems in this type of preparation method: 1. Because the diazotization reaction step needs to use expensive It can only be realized with a high-quality refrigeration pump. Therefore, this method has the problems of many production equipment and high cost, so it is difficult to reduce the cost.
2. Since the diazotization reaction step is an essential and very time-consuming and energy-consuming production step in the production of p-bromophenetole, this method has the problems of long production time and low production efficiency, which is not conducive to the economic benefits of enterprises improvement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of p-bromophenetole, comprising the following steps:

[0019] (1) Etherification reaction step: 10 moles of p-bromophenol, 200 moles of water, and 5.5 moles of diethyl sulfate are successively dropped into a 50-liter reactor with heating device, electric stirring, and thermometer, and heated to 35 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.

[0020] (2) Water washing step: put 800 moles of water in the mixed solution obtained after the etherification reaction, stir evenly, let stand to separate layers, and separate the oil layer.

[0021] (3) Rectification step: the oil layer is carried out the rectification of high-efficiency rectification tower, and this rectification tower is 10 grades of high-efficiency separation rectification towers, uses Type network packing, the product that obtai...

Embodiment 2

[0023] A preparation method of p-bromophenetole, comprising the following steps:

[0024] (1) Etherification reaction step: drop into 10 moles of p-bromophenol, 200 moles of water, and 5.5 moles of diethyl sulfate successively in a 50-liter reactor with a heating device, electric stirring, and a thermometer, and heat to 40 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.

[0025] (2) Water washing step: put 800 moles of water in the mixed solution obtained after the etherification reaction, stir evenly, let stand to separate layers, and separate the oil layer.

[0026] (3) Rectification step: the oil layer is carried out the rectification of high-efficiency rectification tower, and this rectification tower is 10 grades of high-efficiency separation rectification towers, uses Type network packing, th...

Embodiment 3

[0028] A preparation method of p-bromophenetole, comprising the following steps:

[0029] (1) Etherification reaction step: 10 moles of p-bromophenol, 200 moles of water, and 5.5 moles of diethyl sulfate are successively dropped into a 50-liter reactor with heating device, electric stirring, and thermometer, and heated to 45 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.

[0030] (2) Water washing step: put 800 moles of water in the mixed solution obtained after the etherification reaction, stir evenly, leave to stand for stratification, and separate the oil layer.

[0031] (3) Rectification step: the oil layer is carried out the rectification of high-efficiency rectification tower, and this rectification tower is 10 grades of high-efficiency separation rectification towers, uses Type network packing, the product that ...

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PUM

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Abstract

The invention relates to a preparation method of p-bromoethoxybenzene, comprising the following steps: (1) etherification reaction: throwing p-bromophenol and diethyl sulfate into a reaction kettle, stirring, heating, distributing and adding sodium hydroxide to react; (2) washing: adding water to a mixture after etherification reaction, evenly stirring, standing and layering to separate out oily liquid; and (3) rectification: rectifying an oil layer by an efficient rectification tower to obtain the finished product. In the preparation method, the efficient rectification tower is used for rectification instead of the original distillation operation, thus reducing the usage amount of diethyl sulfate and water, keeping the reaction temperature at 30-50 DEG C, saving energy, obtaining high-quality and high-content p-bromoethoxybenzene, achieving high content of p-bromoethoxybenzene up to 99.5% and enhancing the market competitiveness of the product.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a preparation method of 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-bromophenethyl ether is a diazotization reaction. Because the diazotization reaction needs to be carried out at low temperature, low-temperature freezing equipment is needed. The problems in this type of preparation method: 1. Because the diazotization reaction step needs to use expensive Therefore, this method has the problems of many production equipments and high cost, so it is difficult to reduce the cost. 2. Since the diazotization reaction step is an essential and very time-consuming and energy-consuming production step in the production of p-bromophenetole, this method has the problems of long production time and low product...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/225C07C41/16
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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