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Deep purification method of high-purity glycerol

A purification method, glycerin technology, applied in the separation/purification of hydroxyl compounds, organic chemistry, etc., to achieve the effects of reduced separation cost, short production cycle, and convenient operation

Active Publication Date: 2020-11-10
SICHUAN SIPO CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, although this technology has been applied in some fields, it is still blank in the separation and purification of impurities such as fatty acids, aldehydes, and polyglycerols in glycerin. Therefore, the exploration of raw materials, solvent systems, and separation and purification conditions under this system is of great importance. The industrial development of high-purity glycerol is crucial

Method used

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  • Deep purification method of high-purity glycerol
  • Deep purification method of high-purity glycerol
  • Deep purification method of high-purity glycerol

Examples

Experimental program
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Effect test

Embodiment 1

[0034] The solvent used in high-speed countercurrent chromatography in this example is a mixed solution of n-heptane-isopropanol-water, and the ratio by volume is n-heptane:isopropanol:water=6:6:2, oscillate evenly, and stand to separate To obtain a two-phase mixed solution, collect the upper phase solvent and the lower phase solvent separately, and place them in an ultrasonic oscillator for ultrasonic degassing treatment; the lower phase solvent is used as the mobile phase, and the upper and upper phase solvents are used as the stationary phase; the high-speed countercurrent chromatograph After preheating for 30 minutes, pump the stationary phase at a flow rate of 60 mL / min, and when the liquid pumped out of the waste liquid bottle reaches 30-50) mL, start the main engine, adjust the speed to 400 rpm, and pump the mobile phase at a flow rate of 10 mL / min; When the mobile phase and the stationary phase in the waste liquid bottle are clearly separated, open the injection valve, ...

Embodiment 2

[0045] The solvent used in the high-speed countercurrent chromatography in this example is petroleum ether-ethanol-ethyl acetate mixed solution, and the volume ratio is petroleum ether:ethanol:ethyl acetate=6:3:1. The upper and lower phase solvents were collected separately, and placed in an ultrasonic oscillator for ultrasonic degassing. The lower phase of the solvent is used as the mobile phase, and the upper phase of the solvent is used as the stationary phase. After preheating the high-speed countercurrent chromatograph for 30 minutes, pump the stationary phase at a flow rate of 50mL / min; when the liquid pumped out of the waste liquid bottle reaches 30-50mL, start the main engine, adjust the speed to 500rpm, and pump the liquid at a flow rate of 15mL / min. When the mobile phase and the stationary phase in the waste liquid bottle are clearly separated, open the injection valve, inject 80 g of the sample raw material solution (glycerin raw material 2#) at 15 mL / min, collect t...

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Abstract

The invention discloses a deep purification method of high-purity glycerol, and the method comprises the following steps: carrying out high-speed counter-current chromatography separation on a glycerol raw material, collecting eluent in different time periods, and collecting glycerol eluent; and carrying out low-temperature reduced pressure distillation on the collected glycerol eluent to recoverthe solvent, thereby obtaining the high-purity glycerol. The invention provides a deep purification method of high-purity glycerol, which ensures effective separation of glycerol from glyceraldehyde,formaldehyde and other reducing substances, fatty acid and dipolyglycerol in the glycerol crude product, thereby obtaining high-purity glycerol, and ensuring that the total amount of miscellaneous peaks in the final glycerol product is less than or equal to 0.01%, the content of aldehyde and reducing substances is less than or equal to 0.5 ppm, and the content of fatty acid and ester is less thanor equal to 0.1 mL. Since the stationary phase and fluidity of the high-speed counter-current chromatography are both liquids and can be recycled, compared with the conventional chromatographic separation, the process has the advantages of no solid carrier adsorption loss and high sample recovery rate; no stationary phase consumables are consumed, and the separation cost is reduced. Compared witha conventional process, the process has the advantages of being convenient to operate, short in production period and high in yield.

Description

technical field [0001] The invention relates to the technical field of separation and purification, in particular to a deep purification method of high-purity glycerin. Background technique [0002] Glycerin, also known as glycerin, is derived from the by-product of oil hydrolysis, non-toxic, colorless, non-irritating, and good chemical stability, because of its special physical properties and chemical structure (such as Figure 5 ), can be used as synthetic raw materials or directly used in industry, medicine and daily life, and has a wide range of uses. Glycerin has more than 2,000 uses, mainly used in medicine, food, cosmetics, alkyd resin, ester products, tobacco, explosives, cellophane, textile printing and dyeing industry, paper industry, rubber industry, etc. [0003] In the prior art, the purification of crude glycerol is mostly carried out by vacuum distillation, activated carbon adsorption, ion exchange and other methods. Although the glycerin purified by the exis...

Claims

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Application Information

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IPC IPC(8): C07C29/76C07C31/22
CPCC07C29/76C07C31/225
Inventor 秦一别冯自伟徐守斌罗金安刘天婷
Owner SICHUAN SIPO CHEMICAL CO LTD
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