Separation method of polyol mixture

A separation method and mixture technology, which are applied in the preparation of organic compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., to achieve the effects of reducing vacuum degree, reducing high performance requirements, reducing the number of trays and energy consumption

Active Publication Date: 2017-06-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The extractant performs extraction in the form of gas

Method used

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  • Separation method of polyol mixture
  • Separation method of polyol mixture
  • Separation method of polyol mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Such as figure 1 As shown, add 200mL of a mixture of 1,2-propanediol and ethylene glycol to the bottom of the batch distillation column, wherein the mass fraction of 1,2-propanediol is 22%, and the mass fraction of ethylene glycol is 78%. The absolute pressure of the gas phase at the top of the rectification tower is maintained at 13kPa, and the liquid phase temperature in the tower kettle is 120°C. The rectification column uses triangular spiral packing, and the number of theoretical plates is 55. Adjust the temperature of condenser 1 to 100°C and the temperature of condenser 2 to 10°C. Total reflux for 0.5h to stabilize the system;

[0030]Set the reflux ratio to 10:1. Inject ethyl butyrate from the storage tank at a flow rate of 0.78 mL / min into the evaporation tube with an inner surface temperature of 105 °C, and the ethyl butyrate is completely vaporized in the evaporation tube. The gaseous extractant enters the distillation column where it contacts the descend...

Embodiment 2

[0032] Such as figure 1 As shown, add 200mL of a mixture of 1,2-butanediol and ethylene glycol to the bottom of the batch distillation column, wherein the mass fraction of 1,2-butanediol is 10%, and the mass fraction of ethylene glycol is 90%. The absolute pressure of the gas phase at the top of the rectification tower is kept at 14.5kPa, and the temperature of the liquid phase in the tower kettle is 110°C. The rectification column uses Pall ring packing, and the number of theoretical plates is 60. Adjust the temperature of condenser 1 to 90°C and the temperature of condenser 2 to 3°C. Full reflux for 0.5h to stabilize the system;

[0033] Set the reflux ratio to 10:1. Inject propyl ether from the storage tank at a flow rate of 1.1 mL / min into the evaporating tube with an inner surface temperature of 95°C. Most of the propyl ether is vaporized in the evaporating tube, and a small amount is vaporized at the bottom of the tower. The gaseous extractant enters the distillatio...

Embodiment 3

[0035] Such as figure 1 As shown, add 200mL of a mixture of 1,2-propanediol and ethylene glycol to the bottom of the batch distillation column, wherein the mass fraction of 1,2-propanediol is 50%, and the mass fraction of ethylene glycol is 50%. The absolute pressure of the gas phase at the top of the rectification tower is maintained at 19.8kPa, and the temperature of the liquid phase in the tower kettle is 150°C. The rectification column uses Raschig ring packing, and the number of theoretical plates is 83. Adjust the temperature of condenser 1 to 137°C and the temperature of condenser 2 to 20°C. Total reflux for 0.7h to stabilize the system;

[0036] Set the reflux ratio to 8.5:1. From the storage tank, inject isobutanol into the evaporation tube with an inner surface temperature of 143 °C at a flow rate of 1 mL / min. Most of the isobutanol is vaporized in the evaporation tube, and a small amount is vaporized at the bottom of the tower. The gaseous extractant enters the ...

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Abstract

The invention discloses a separation method of a mixture of polyols with similar boiling points. Glycol containing dihydric fusels (1,2-butylene glycol and 1,2-butylene glycol) is adopted as the feedstock of a reduced pressure rectifying tower, and a weakly polar gaseous extraction agent is introduced to the bottom of the tower, so relative volatility between the 1,2-butylene glycol and 1,2-butylene glycol which have the same weak polarity and the glycol with strong polarity is improved, and the separation efficiency of rectification is improved. The invention provides a novel rectification method of the dihydric fusels from the glycol. The boiling point of the gaseous extraction agent is far lower than that of the dihydric alcohols, and the gaseous extraction agent is easy to separate and can be recycled, so the material consumption and the energy consumption in the separation process are reduced. The method allows the 1,2-butylene glycol and 1,2-butylene glycol to be separated from the glycol, and allows highly pure glycol and concentrated 1,2-butylene glycol and 1,2-butylene glycol byproducts to be obtained.

Description

technical field [0001] The invention relates to a chemical separation technology for removing 1,2-propanediol and 1,2-butanediol from ethylene glycol. Background technique [0002] Ethylene glycol is a basic chemical raw material for mass production, which can be used to produce polyester fiber (polyester), polyethylene terephthalate, explosives, solvents, antifreeze agents, plasticizers, hygroscopic agents, etc. At present, the industry mainly uses ethylene as raw material to produce ethylene glycol through ethylene oxide hydration method, which needs to consume a large amount of non-renewable oil and natural gas resources. Since 2002, China's ethylene glycol imports accounted for more than 70% of the demand. Among them, the ethylene glycol consumed by the polyester industry accounts for more than 80%. Biomass raw materials rich in cellulose are cheap and easy to obtain. Producing ethylene glycol from renewable biomass can not only reduce dependence on oil and coal, but a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/84C07C31/20
CPCC07C29/84C07C31/202C07C31/205C07C31/207
Inventor 艾硕郑明远张涛庞纪峰王爱琴王晓东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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