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Adsorption separation method of polyhydric alcohol mixture with similar boiling points

A boiling point approach, adsorption separation technology, applied in the separation/purification of hydroxyl compounds, organic chemistry and other directions, can solve the problem of high energy consumption of rectification towers, achieve mature preparation technology, reduce environmental pollution and energy consumption, and low cost. Effect

Active Publication Date: 2017-06-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
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  • Description
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Problems solved by technology

During this process, ethylene glycol will react with methanol and ethanol to generate 1,2-propanediol and 1,2-butanediol respectively, and these two impurities are generally separated by rectification, but The energy consumption of the rectification column is also very large

Method used

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  • Adsorption separation method of polyhydric alcohol mixture with similar boiling points
  • Adsorption separation method of polyhydric alcohol mixture with similar boiling points

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Such as figure 1 As shown, valves 1, 3, and 6 are open, and valves 2, 4, 5, and 7 are closed. Adsorption columns 1 and 2 are both equipped with 20 grams of fully dried Hβ molecular sieve adsorbent with a silicon-aluminum ratio of 25. Heat the adsorption column 1 to 30°C, and the adsorption column 2 is eluted and regenerated with pure water at 80°C for 1.5 hours. 1mL / min. Use a plunger pump to pass the ethylene glycol crude product containing 10% mass fraction of 1,2-butanediol into the adsorption column at a flow rate of 3mL / min, and extract the refined product of ethylene glycol at the outlet of the adsorption column. The mass fraction of ethylene glycol is as high as 99.6%. The 1,2-butanediol contained in the bed of adsorption column 2 is completely eluted by water, heat the bed to evaporate all the pure water contained in it, and the regeneration of the adsorbent in adsorption column 2 is completed, heat the adsorption column to 2 to 30°C .

[0029] When the mass...

Embodiment 2

[0031] Such as figure 2 As shown, valves 1 and 3 are open and valves 2 and 4 are closed. Adsorption columns 1 and 2 are both equipped with 40 grams of fully dry acidic alumina, heating adsorption column 1 to 40 ° C, adsorption column 2 is heated to 500 ° C in air and calcined for 4 hours, and the regeneration of the adsorbent in adsorption column 2 is completed. With a gear pump, the ethylene glycol crude product containing 30% 1,2-pentanediol is passed into the adsorption column at a flow rate of 4mL / min, and the refined product of ethylene glycol is extracted at the outlet of the adsorption column. The mass fraction of ethylene glycol is as high as 99%. Heat the adsorption column from 2 to 40 °C.

[0032] When the mass fraction of 1,2-pentanediol in the ethylene glycol at the outlet of the adsorption column 1 exceeds 1%, open valves 2 and 4 and close valves 1 and 3 . The raw material stream was switched to the adsorption column 2 to continue adsorption and purification, ...

Embodiment 3

[0034] For gas phase adsorption separation, the system needs to be vacuumed and decompressed. Such as figure 1 As shown, open valves 1, 3, 6 and close valves 2, 4, 5, 7. Adsorption columns 1 and 2 were both equipped with 30 grams of fully dried sulfonated activated carbon, and adsorption column 1 was heated to 130°C, and adsorption column 2 was eluted and regenerated with ethanol at normal temperature and pressure for 2 hours, with a flow rate of 1.2mL / min. The adsorption column 1 is decompressed to an absolute pressure of 7kPa with a vacuum pump, and the crude product of ethylene glycol containing 27% 1,2-hexanediol is vaporized and passed into the adsorption column at a gas velocity of 3g / min. Ethylene glycol vapor is discharged at the outlet of the adsorption column and condensed into a product, and the mass fraction of ethylene glycol in the product is as high as 99.2%. The 1,2-hexanediol contained in the bed layer of the adsorption column 2 is completely eluted by ethan...

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Abstract

The invention discloses an adsorption separation method of a polyhydric alcohol mixture with similar boiling points. Ethylene glycol containing one or several kinds of binary or ternary fusel (including 1,2-propanediol, 1,3-propanediol, 1,2-butanediol, 1,3-butanediol, 2,3-butanediol, 1,4-butanediol, 1,2-pentanediol, 1,2-hexanediol and glycerol) is used as raw materials; in an adsorption device, binary or ternary fusel is adsorbed and immobilized by solid protonic acids such as hydrogen molecular sieves, hydrogen type resin and sulfonated activated carbon; the ethylene glycol basically does not generate adsorption and is directly produced into products. The solid acids after the adsorption saturation can be regenerated by a sintering method or a solvent elution method. The whole technical process conditions are mild; adsorption agents can be easily regenerated; high adsorption selectivity is particularly realized on 1,2-butanediol and 1,2-pentanediol which are difficult to be recovered through conventional rectification. The method provided by the invention belongs to an efficient and energy-saving process for separating difficult-to-separate ethylene glycol coarse products into high-purity ethylene glycol and dihydric alcohol byproducts.

Description

technical field [0001] The invention relates to an adsorption separation method for polyol mixtures with close boiling points, and belongs to the technical field of chemical separation. Background technique [0002] Ethylene glycol is a colorless, odorless, sweet liquid chemical raw material, mainly used to produce polyester fiber (polyester), bottle grade PET (mineral water bottle), solvent, antifreeze, plasticizer, hygroscopic Among them, the ethylene glycol consumed by the polyester industry accounts for more than 90% of the total consumption. Although my country's ethylene glycol production capacity and output have grown rapidly, it still cannot meet the growing market demand for domestic polyester. China's ethylene glycol imports account for more than 70% of the demand, and the demand It has increased every year, and the huge market gap has caused an upsurge in the construction of ethylene glycol plants in China. [0003] The traditional ethylene glycol synthesis metho...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/76
CPCC07C29/76C07C31/202C07C31/205C07C31/207C07C31/20C07C31/225
Inventor 艾硕郑明远张涛王爱琴王晓东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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