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Method for separating glycol and 1,2-butanediol

A technology of ethylene glycol and butanediol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as high reflux ratio and theoretical plate number, unsatisfactory separation effect, and harsh separation conditions. Achieve the effect of reducing the number of theoretical plates and reflux ratio, reducing losses, and reducing equipment and operating costs

Inactive Publication Date: 2014-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] What the present invention is to solve is that when the prior art separates and purifies the stream containing ethylene glycol and 1,2-butanediol, the use of ordinary rectification requires a high reflux ratio and the number of theoretical plates, resulting in large investment and high energy consumption. The technical problem of harsh separation conditions or unsatisfactory separation effect by ordinary azeotropic distillation method provides a new reaction-azeotropic distillation method for separating streams containing ethylene glycol and 1,2-butanediol

Method used

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  • Method for separating glycol and 1,2-butanediol
  • Method for separating glycol and 1,2-butanediol
  • Method for separating glycol and 1,2-butanediol

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Reaction - The theoretical plate number of the azeotropic rectification column is 30, and the reaction does not contain a catalyst. The weight percentage composition is dimethyl oxalate less than 100ppm, 1,2-propanediol 1.26%, 1,2-butanediol 3.54%, ethylene glycol 94.39%, diethylene glycol and other heavy components 0.80% of raw materials from the reaction- The 8th theoretical plate of the azeotropic distillation column enters, and the reactant I-1 (substituent R 1 , R 2 Respectively: -CH 3 , (CH 2 ) 2 CH(CH 3 ) 2) enters from the 20th theoretical plate of the tower, the initial molar ratio of ethylene glycol in the reactant to the raw material is 0.6:1, the operating pressure of the reaction-azeotropic rectification tower is normal pressure, the reflux ratio is 2, and the tower top temperature It is 166°C, and the temperature of the tower bottom is 198°C. Ethylene glycol and the entrainer generated by the reaction form an azeotrope, which is evaporated from the ...

Embodiment 2

[0028] Reaction - The number of theoretical plates of the azeotropic distillation tower is 8, and the catalyst for the reaction is YJ-1 acid resin catalyst, which is loaded on 4~6 theoretical plates of the rectification tower. The weight percentage is composed of 20% ethylene glycol, 75% 1,2-butanediol and 5% 1,2-propylene glycol. The mixed solution enters from the 4th theoretical plate of the reaction-azeotropic distillation column, and the reactant I-1 Enter from the 6th theoretical plate of the tower, the initial molar ratio of ethylene glycol in the reactant and the raw material is 0.8:1, the consumption of the catalyst is 5% of the mixed mass mole fraction of the raw material and the reactant, the reaction-azeotropic rectification column The operating pressure is 10KPa in absolute pressure, the reflux ratio is 10, the temperature at the top of the tower is 125°C, and the temperature at the bottom of the tower is 149°C. Ethylene glycol and the entrainer generated by the re...

Embodiment 3

[0031] Reaction-The theoretical plate number of the azeotropic rectification column is 15, and the catalyst of the reaction is p-toluenesulfonic acid. The weight percent composition is 0.23% methanol, 1.83% 1,2-propanediol, 0.42% 1,2-butanediol and 95.22% ethylene glycol oxalate hydrogenation product and catalyst from the fifth reaction-azeotropic distillation column Block theory board enters, reactant I-2 (substituent R 1 , R 2 Respectively: -CH 2 CH 3 ,-(CH 2 ) 2 CH 3 ) enters from the 10th theoretical plate of the tower, the initial molar ratio of ethylene glycol in the reactant to the raw material is 1:1, the amount of the catalyst is 2.5% of the mixed mass mole fraction of the raw material and the reactant, reaction-azeotropic distillation The operating pressure of the tower is 30KPa in absolute pressure, the reflux ratio is 5, the temperature at the top of the tower is 136°C, and the temperature at the bottom of the tower is 162°C. Ethylene glycol and the entraine...

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Abstract

The invention relates to a method for separating glycol and 1,2-butanediol, which mainly solves the problems of high investment and energy consumption due to the fact that a very high reflux ratio and very high number of theoretical plates are required when a common rectification method is employed to separate and purify a material flow containing glycol and 1,2-butanediol, and severe separation conditions or a non-ideal separation effect when a common azeotropic rectification method is employed. The method better solves the problem by employing the technical scheme that the material flow containing glycol and 1,2-butanediol and a reactor enters from the upper part and the lower part of a reaction-azeotrope rectification tower respectively, a generated reaction product forms an azeotrope with glycol at the same time, a tower kettle obtains a material flow containing 1,2-butanediol, and after the azeotrope distilled from the tower top is subjected to condensation phase splitting, a glycol-rich phase at the lower layer is further refined to form a glycol product. The method can be used for industrial production of separating the material flow containing glycol and 1,2-butanediol.

Description

technical field [0001] The invention relates to a reaction-azeotropic distillation method for separating streams containing ethylene glycol and 1,2-butanediol, which can be used to separate and purify ethylene glycol from oxalate hydrogenation liquid phase products, and can also be used for other streams containing ethylene glycol The separation of ethylene glycol and 1,2-butanediol streams can also be used to prepare and separate and purify the entrainer used for separating ethylene glycol and 1,2-butanediol streams by reactive distillation technology. Background technique [0002] Ethylene glycol is an important basic organic chemical raw material, mainly used for copolymerization with terephthalic acid to produce polyethylene terephthalate (PET). In addition, ethylene glycol can also be used in the production of antifreeze, lubricants, plasticizers, non-ionic surfactants and explosives, etc., and has a wide range of uses. my country is a big consumer of ethylene glycol. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/82
CPCC07C29/82
Inventor 郭艳姿肖剑
Owner CHINA PETROLEUM & CHEM CORP
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