Method for separating alcohol-salt mixture by supercritical carbon dioxide extraction

A carbon dioxide, supercritical technology, applied in the preparation of organic compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the problems of difficult separation, corrosion of equipment, low separation efficiency, etc., to improve the total yield and high efficiency. separation effect

Inactive Publication Date: 2017-07-25
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation process of this method is very long, the unit operation is complicated, the polyol and the organic acid will also azeotrope, the separation efficiency is low, the separation is difficult, and the organic acid is corrosive to the equipment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Extraction of Polyols from Sorbitol Hydrocracking Rectification Alcohol Mixture

[0039]Add 500g sorbitol hydrocracking rectification alkoxide mixture in 1000ml extraction tank, each component content of alkoxide mixture is respectively: organic acid salt 30wt%, dibasic alcohol 55wt%, polyhydric alcohol dehydration product 15% (based on alkoxide The total mass of the mixture, the same below), wherein the total mass of polyols is 350g, seal the extraction tank, introduce carbon dioxide gas and pressurize to 10MPa, gradually raise the temperature of the extraction tank to 120 ° C, start timing, and stop after 8 hours of extraction Heating, gradually release the pressure of the supercritical carbon dioxide dissolved with polyols to the first-stage separation tank, detect and calculate the total amount of polyols in carbon dioxide to be 315g, keep the pressure of the first-stage separation tank at 8MPa, and keep the temperature at 50°C. After standing still for 3 hours, the...

Embodiment 2

[0041] Extraction of Polyols from Glucose Hydrocracking Rectification Alcohol Mixture

[0042] Add 500g of glucose hydrocracking rectification alkoxide mixture in 1000ml extraction tank, organic acid salt 20wt% in alkoxide mixture, dibasic alcohol 62wt%, polyhydric alcohol dehydration product 18wt%, wherein the total mass of polyhydric alcohol is 400g, seal The extraction tank is fed with carbon dioxide gas and pressurized to 12MPa. When the temperature of the extraction tank is gradually raised to 60°C, the timing is started. After 5 hours of extraction, the heating is stopped, and the pressure release of the supercritical carbon dioxide dissolved in polyols is gradually transferred to the primary separation. In the tank, detect and calculate the total amount of polyalcohols in carbon dioxide to be 380g, keep the pressure of the primary separation tank at 9MPa, keep the temperature at 40°C, and after standing for 1 hour, transfer the carbon dioxide to a place where 2% of the m...

Embodiment 3

[0044] Extraction of Polyols from Xylitol Hydrocracking Rectification Alcohol Mixture

[0045] Add 500g xylitol hydrocracking rectification alkoxide mixture in 1000ml extraction tank, organic acid salt 25wt% in the alkoxide mixture, glycol 70wt%, polyol dehydration product 5wt%, wherein the total mass of polyol is 375g , seal the extraction tank, feed carbon dioxide gas and pressurize to 18MPa, gradually raise the temperature of the extraction tank to 160°C, start timing, stop heating after 12 hours of extraction, and gradually release the pressure of supercritical carbon dioxide dissolved in polyols to a In the first-stage separation tank, detect and calculate the total amount of polyols in the carbon dioxide to be 363.75g, keep the pressure of the first-stage separation tank at 12MPa, and keep the temperature at 70°C. After standing for 5 hours, transfer the carbon dioxide to the mass of the alkoxide mixture added in advance. In the secondary separation tank of 0.5% polyoxye...

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PUM

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Abstract

The invention provides a method for separating an alcohol-salt mixture by supercritical carbon dioxide extraction. The method comprises a) feeding supercritical carbon dioxide into an extraction tank, extracting polyol in an alcohol-salt mixture and transferring the polyol into a primary separation tank, b) reducing the temperature and pressure in the primary separation tank, keeping a carbon dioxide supercritical state, separating the extracted polyol from carbon dioxide and feeding the supercritical carbon dioxide containing a small amount of polyol into a secondary separation tank, and c) pre-adding a defoamer into the secondary separation tank, reducing pressure so that the supercritical state of the carbon dioxide is changed into a common gaseous state and further separating polyol so that polyol in the alcohol-salt mixture can be completely separated.

Description

technical field [0001] The invention relates to a method for extracting and separating alkoxide mixtures by supercritical carbon dioxide, in particular to a method for separating polyols and organic acid salts by using supercritical carbon dioxide, and belongs to the technical field of bio-based polyol production. Background technique [0002] Bioenergy is a renewable energy source on the earth. Sugar and sugar alcohol compounds can provide energy for living organisms to survive, and the source of this type of substance is mostly plants, such as starch. Glucose, xylose, sucrose, maltose, fructose, sorbitol, xylitol, mannitol, isosorbide, etc. can be prepared through hydrolysis and other multi-step reactions through the most primary and original starch and other substances. These sugar alcohols are structurally The common feature of these substances is that they have more than five carbon atoms and more than four hydroxyl groups. These substances can often be used as food or ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/84C07C31/20
CPCC07C29/84C07C31/202C07C31/205C07C31/207Y02P20/54
Inventor 张鑫陈海波吕兵
Owner WANHUA CHEM GRP CO LTD
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