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Method for separating acetylpropionic acid from mono saccharide hydrolyzate

A technology of levulinic acid and hydrolyzate, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of high processing costs, large consumption of extractants, and difficult separation of extracts, and achieve low production costs , easy industrialization, and simple technological process

Inactive Publication Date: 2006-05-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solvent extraction method has the disadvantages of large consumption of extractant, difficulty in separating the extract, and high processing costs. There are limitations in the industrial separation and purification of levulinic acid by solvent extraction.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1) A mixed hydrolyzate containing 17.2 mg / ml of glucose, 19.6 mg / ml of formic acid and 18.4 mg / ml of levulinic acid was used as the starting material for chromatographic separation.

[0018] 2) The column size is 12×500mm, filled with 335 gel-type porous epoxy weak base anion exchange resin (20-50 mesh), and the bed height is 48.5cm (about 55ml bed volume BV). 140ml of the above-mentioned hydrolyzate was passed into the chromatography column at a flow rate of 1BV / h (resin bed volume / hour), and the temperature was controlled at 30°C. After the feeding is completed, wash the chromatography column with 156ml of deionized water at a flow rate of 1BV / h to wash away neutral impurities such as sugar. Then use 0.5mol / l hydrochloric acid aqueous solution to elute the levulinic acid and formic acid adsorbed on the resin, the flow rate is 0.5BV / h, and collect the eluent in sections until all the adsorbed levulinic acid and formic acid are eluted .

[0019] 3) Use HPLC to detect...

Embodiment 2

[0021] 1) A mixed hydrolyzate containing 12.5 mg / ml of glucose, 6.5 mg / ml of fructose, 6.1 mg / ml of formic acid and 15.3 mg / ml of levulinic acid was used as the starting material for chromatographic separation.

[0022] 2) The column size is 12×500mm, filled with 335 gel-type porous epoxy weak base anion exchange resin (20-50 mesh), and the bed height is 48.5cm (about 55ml bed volume BV). 140ml of the above-mentioned hydrolyzate was passed into the chromatography column at a flow rate of 3.0BV / h (resin bed volume / hour), and the temperature was controlled at 40°C. After the feeding is completed, first wash the chromatography column with 156ml of deionized water at a flow rate of 0.5BV / h to wash away neutral impurities such as sugar. Then use 1.0mol / l hydrochloric acid aqueous solution to elute the levulinic acid and formic acid adsorbed on the resin, the flow rate is 2.0BV / h, and collect the eluent in sections until all the adsorbed levulinic acid and formic acid are eluted ....

Embodiment 3

[0025] 1) A mixed hydrolyzate containing 12.5 mg / ml of glucose, 15.3 mg / ml of levulinic acid, and 9.2 mg / ml of formic acid was used as the starting material for chromatographic separation.

[0026] 2) The column size is 12×500mm, filled with 335 gel-type porous epoxy weak base anion exchange resin (20-50 mesh), and the bed height is 48.5cm (about 55ml bed volume BV). 200ml of the above-mentioned hydrolyzate was passed into the chromatography column at a flow rate of 0.5BV / h (resin bed volume / hour), and the temperature was controlled at 20°C. After the feed is completed, first wash the chromatography column with 156ml of deionized water at a flow rate of 3.0BV / h to wash away neutral impurities such as sugar. Then use 0.1mol / l hydrochloric acid aqueous solution to elute the levulinic acid and formic acid adsorbed on the resin, the flow rate is 0.3BV / h, and collect the eluent in sections until all the adsorbed levulinic acid and formic acid are eluted .

[0027] 3) Use HPLC to...

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PUM

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Abstract

The invention relates to the resin absorbing separation and purification technique, relating to a method for separating acetyl propionic acid from monosaccharide hydrolyzate, passing the acetyl propionic acid hydrolyzate containing residual sugar and other impurities such as neutral matter and formic acid through weakly basic anion exchange resin column, firstly washing off unabsorbable impurities such as sugar with the deionized water, then eluting acetyl propionic acid and formic acid from the resin with acid water solution, and the acetyl propionic acid eluting solution is concentrated at normal pressure and vacuum-distilled to be able to obtain high-content acetyl propionic acid whose purity is up to 98.5% and whose total yield can be above 85%. The method has the advantages of simple processing flow, low production cost and being easy to industrialize.

Description

technical field [0001] The invention relates to a resin adsorption separation and purification technology, in particular to a method for separating levulinic acid from a monosaccharide hydrolyzate. Background technique [0002] Levulinic acid (Levulinic Acid, LA), also known as 4-oxovaleric acid, levotranic acid or valeric acid. It has both the nature of carboxylic acid and the nature of ketone, so it has good chemical reactivity, and can carry out various reactions such as esterification, redox, substitution, polymerization, etc., and synthesize many useful compounds and new polymer materials, including Resins, medicines, spices, solvents and inks, rubber and plastic additives, lubricating oil additives, surfactants, etc. At the same time, the carbonyl group at the 4-position is a latent chiral group, and chiral compounds can be obtained through asymmetric reduction. Levulinic acid is also a biologically active molecule and an intermediate for pesticides and dyes. In add...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C59/185
Inventor 任其龙刘宝鉴杨亦文吕秀阳陈丰秋詹晓力黄梅苏宝根魏作君
Owner ZHEJIANG UNIV
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