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O-ethoxyl phenol refining process

A technology for o-ethoxyphenol and ethoxyphenol, which is applied in the refining field of synthesizing o-ethoxyphenol by a catechol method, can solve problems such as being difficult to separate, achieve high product purity, reduce production costs, and improve The effect of productivity

Inactive Publication Date: 2005-12-14
CNPC JILIN CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of synthesizing o-ethoxyphenol, the boiling points of o-ethoxyphenol product and by-product o-diethoxyphenol obtained at the same time are only 1°C apart, so it is difficult to separate them

Method used

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  • O-ethoxyl phenol refining process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 1090g of the above-mentioned condensed liquid oil phase, divide it into two equal parts, and determine it as the first and second batches, and carry out the following steps respectively: wash with 960g of 5% sodium hydroxide solution for 30 minutes, and then separate the liquids; Add 31% hydrochloric acid to neutralize until the pH value is 1, then add 600 g of toluene to fully extract, separate the layers, and collect the oil phase. Then add the extracted oil phase into the distillation flask, install the condenser, tail pipe, receiver and thermometer, and heat to 140°C with an oil bath for distillation. When the column temperature is between 110°C and 120°C, distillates begin to flow out from the top of the column, and the effluent at this time is mainly toluene and contains a small amount of water. When the toluene is almost evaporated, the column temperature begins to drop, and when the column temperature is 30°C to 40°C, the atmospheric distillation ends. Aft...

Embodiment 2

[0030] Take 1090g of the above-mentioned condensed liquid oil phase, divide it into two equal parts, and determine it as the 3rd and 4th batches, and carry out the following steps respectively: wash with 480g of 10% sodium hydroxide solution for 30 minutes, and then separate the liquids; Add 31% hydrochloric acid to neutralize until the pH value is 2, then add 600 g of toluene to fully extract and separate the layers. Collect the oily phase. Then add the extracted oil phase into the distillation flask, install the condenser, tail pipe, receiver and thermometer, and heat to 140°C with an oil bath for distillation. When the column temperature is between 110°C and 120°C, distillates begin to flow out from the top of the column, and the effluent at this time is mainly toluene and contains a small amount of water. When the toluene is almost evaporated, the column temperature begins to drop, and when the column temperature is 30°C to 40°C, the atmospheric distillation ends. After ...

Embodiment 3

[0032] Take 1090g of the above-mentioned condensed liquid oil phase, divide it into two equal parts, and determine it as the 5th and 6th batches, and carry out the following steps respectively: wash with 20% sodium hydroxide solution 480g alkali for 30 minutes, then separate the liquids; take the water after alkali washing Add 31% hydrochloric acid to neutralize until the pH value is 4, then add 600 g of toluene to fully extract and separate the layers. Collect the oily phase. Then add the extracted oil phase into the distillation flask, install the condenser, tail pipe, receiver and thermometer, and heat to 140°C with an oil bath for distillation. When the column temperature is between 110°C and 120°C, distillates begin to flow out from the top of the column, and the effluent at this time is mainly toluene and contains a small amount of water. When the toluene is almost evaporated, the column temperature begins to drop, and when the column temperature is 30°C to 40°C, the at...

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Abstract

The o-ethoxyl phenol refining process includes the following steps: alkali washing condensated o-ethoxyl phenol oil phase or o-ethoxyl phenol product obtained through catechol process with 5-20 % sodium hydroxide solution for 30 min and separating liquid; regulating pH value of the water phase after alkali washing with hydrochloric acid to 1-4, extracting with toluene, and separating liquid to collect oil phase; distilling the oil phase at 110-120 deg.c to recover toluene, lowering the temperature to 30-40 deg.c for decompression rectification to obtain o-ethoxyl phenol of purity not lower than 99.2 %, with the recovered toluene being reused. The present invention can raise the production capacity of industrial apparatus and lower production cost.

Description

technical field [0001] The invention relates to a refining method of catechol, in particular to a refining method for synthesizing o-ethoxyphenol by a catechol method. Background technique [0002] O-ethoxyphenol, also known as o-hydroxyphenethyl ether and ethyl guaiacol, is the most important raw material for the synthesis of ethyl vanillin and an indispensable pharmaceutical intermediate in the pharmaceutical industry. [0003] The main synthesis methods of o-ethoxyphenol are o-aminophenethyl ether method and catechol method. Among them, the catechol method is divided into catechol, ethanol method, catechol, diethyl sulfate method and catechol, ethyl chloride method. The synthesis of o-ethoxyphenol by catechol and ethyl chloride method is to use catechol and ethyl chloride as raw materials, and under the action of a catalyst, it is prepared through steps such as condensation and post-treatment, and its chemical reaction formula as follows: [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/253
Inventor 苑冰郭双龙陈继新盛光王芳黄文焕石占崇黄晓东
Owner CNPC JILIN CHEM GROUP CORP
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