Separating method for ethylene-glycol and 1,2-butanediol

A separation method, ethylene glycol technology, 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, harsh separation conditions, etc., to achieve The effect of reducing losses, reducing investment and energy consumption, and reducing the number of theoretical boards

Active 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

[0006] The technical problem to be solved by the present invention is that when the prior art separates 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 problem of harsh separation conditions or unsatisfactory separation effect of azeotropic distillation provides a new separation method of ethylene glycol and 1,2-butanediol

Method used

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  • Separating method for ethylene-glycol and 1,2-butanediol

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Experimental program
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Effect test

Embodiment 1

[0021] The theoretical plate number of the azeotropic distillation column is 30. The weight percent composition is a mixed solution of dimethyl oxalate less than 100ppm, 1.26% of 1,2-propanediol, 3.54% of 1,2-butanediol, 94.39% of ethylene glycol, 0.80% of diethylene glycol and other heavy components. The 20th theoretical plate of the boiling rectification column enters, and the entrainer AZ1 (substituent R 1 , R 2 , R 3 and R 4 Respectively: -H, -H, -CH 3 ,-(CH 2 ) 4 CH 3 ) enters from the top of the tower, the molar ratio of entrainer to ethylene glycol in the raw material is 1.5:1, the operating pressure of the azeotropic distillation column is normal pressure, the reflux ratio is 0.5, the temperature at the top of the tower is 166°C, and the temperature of the bottom of the tower is The temperature is 198°C. The azeotrope formed by ethylene glycol and entrainer is evaporated from the top of the tower. After the azeotrope is condensed and phase-separated, the volume ...

Embodiment 2

[0024] The number of theoretical plates in the azeotropic distillation column is 8. 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 6th theoretical plate of the azeotropic distillation column, and the entrainer AZ1 (substituent R 1 , R 2 , R 3 and R 4 Respectively: -H, -H, -CH 3 ,-(CH 2 ) 4 CH 3 ) enters from the top of the tower, the molar ratio of entrainer to ethylene glycol in the raw material is 2:1, the operating pressure of the azeotropic distillation column is 10KPa in absolute pressure, the reflux ratio is 10, and the temperature at the top of the tower is 125°C, The temperature of the tower kettle is 149°C, the volume ratio of the upper and lower layers of the top azeotrope after condensation and phase separation is 3.5:1, and the lower ethylene glycol-rich phase does not contain 1,2-butanediol, the weight percentage of ethylene glycol The composition is: 86.98%, and ...

Embodiment 3

[0027]The number of theoretical plates in the azeotropic distillation column is 15. A mixed solution composed of 0.23% methanol, 1.83% 1,2-propanediol, 0.42% 1,2-butanediol and 95.22% ethylene glycol enters from the 10th theoretical plate of the azeotropic distillation column, and the entrainer AZ2 (substituent R 1 , R 2 , R 3 and R 4 Respectively: -H, -H, -CH 2 CH 3 ,-(CH 2 ) 2 CH 3 ) from the top of the tower, the molar ratio of the entrainer to the ethylene glycol in the raw material is 3:1, the operating pressure of the azeotropic distillation column is 30KPa in absolute pressure, the reflux ratio is 5, and the temperature at the top of the tower is 136°C, The temperature of the tower kettle is 162°C, the volume ratio of the upper and lower layers of the top azeotrope after condensation and phase separation is 7.4:1, and the lower ethylene glycol-rich phase does not contain 1,2-butanediol, the weight percentage of ethylene glycol The composition is: 88.33%, and th...

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Abstract

The invention relates to a separating method for ethylene-glycol and 1,2-butanediol and mainly solves the problems that when the ethylene-glycol and the 1,2-butanediol are separated and purified in the prior art, a common precise distillation method requires very high reflux ratio and theoretical plate number, resulting in large investment and high energy consumption; an azeotropic distillation method is harsh in separation condition and undesirable in separating effect. According to the method adopting the technical scheme that material flow containing the ethylene-glycol and the 1,2-butanediol enters into an azeotropic rectification column from the lower part and an azeotropic agent enters the azeotropic rectification column from the top to obtain an azeotrope of the ethylene-glycol and the azeotropic agent at the top, the material flow containing the 1,2-butanediol is obtained in a tower kettle; after the azeotrope is subjected to condensation and phase-splitting, the azeotropic agent-rich phase at the upper layer returns to the azeotropic rectification column and continues performing azeotropic reaction while an ethylene-glycol-rich phase at the lower layer is subjected to refining to obtain the ethylene-glycol product, and the problems are well solved. Therefore, the method can be used for industrial production for separating the ethylene-glycol and the 1,2-butanediol.

Description

technical field [0001] The invention relates to a method for separating and purifying a stream containing ethylene glycol and 1,2-butanediol, which can be used for separating and purifying ethylene glycol from oxalate ester hydrogenation liquid phase products, and can also be used for other streams containing ethylene glycol and 1,2-butanediol - Separation of the butanediol stream. 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. In recent years, with the completion and operation of a number of large-scale PET plants, the demand for ethylene glycol has increased rapidly. The current domestic ethylene g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/82
CPCC07C29/82C07C31/202C07C31/207
Inventor 肖剑郭艳姿
Owner CHINA PETROLEUM & CHEM CORP
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