Process of separating acetylpropionic acid with active carbon

A technology of levulinic acid and activated carbon, which is applied in the field of adsorption and ion exchange separation and purification, can solve the problems of large consumption of extractant, high processing cost, and difficult separation of extracts, and achieve low production cost, easy industrialization, and high yield. high rate effect

Inactive Publication Date: 2007-08-22
ZHEJIANG UNIV
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  • Abstract
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Problems solved by technology

However, the solvent extraction method has the disadvantages of large consumption of extractant, difficulty in separating the extract,

Method used

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  • Process of separating acetylpropionic acid with active carbon

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 300ml of a mixture of formic acid and levulinic acid (1.04mg / ml formic acid, 5.20mg / ml levulinic acid) with a mass ratio of 0.2:1 through 100ml bed volume at a flow rate of 3BV / h at 20°C Granular activated carbon column: After heating to 50°C, fully rinse the bed with deionized water at a flow rate of 3BV / h to desorb all formic acid adsorbed on the activated carbon. Then at the same temperature and at the same flow rate, the levulinic acid adsorbed on the activated carbon is eluted with a 95% ethanol aqueous solution. The elution curve of the entire separation process is shown in Figure 2. The eluate is concentrated under reduced pressure to obtain pure levulinic acid The purity of the product was 99.1% by HPLC, and the spectrum showed no miscellaneous peaks. The total yield of levulinic acid was 94.1%.

Embodiment 2

[0022] 200ml of a mixture of formic acid and levulinic acid (63.5mg / ml formic acid, 12.7mg / ml levulinic acid) with a mass ratio of 5:1 through 100ml bed volume at a flow rate of 0.5BV / h at 40°C The granular activated carbon column; after heating to 80℃, fully rinse the bed with deionized water at a flow rate of 0.5BV / h to desorb all the formic acid adsorbed on the activated carbon; then use 30% of the formic acid at the same flow rate at the same temperature The ethanol aqueous solution eluted the levulinic acid adsorbed on the activated carbon, and the eluate was concentrated under reduced pressure to obtain the pure levulinic acid. Detected by HPLC, its purity is 98.8%, the spectrum has no other peaks, and the total yield of levulinic acid is 96.5%.

Embodiment 3

[0024] 90ml of a mixture of formic acid and levulinic acid with a mass ratio of 1:1 (51.1mg / ml formic acid and 51.1mg / ml levulinic acid) was passed through a bed volume of 100ml at a flow rate of 1BV / h at 30°C Granular activated carbon column; after heating to 60℃, fully rinse the bed with deionized water at a flow rate of 1BV / h to desorb all formic acid adsorbed on the activated carbon; then use 80% methanol aqueous solution at the same temperature and at the same flow rate The levulinic acid adsorbed on the activated carbon is eluted. The purity of the obtained pure levulinic acid detected by HPLC was 99.3%, the spectrum showed no miscellaneous peaks, and the total yield of levulinic acid was 96.8%.

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Abstract

The present invention is process of separating acetylpropionic acid with active carbon from the mixture solution of acetylpropionic acid and formic acid or acetylpropionic acid containing hydrolysate obtained through hydrolyzing sacchraide. The mixture solution or hydrolysate after being chromatographically separated in alkali cationic column and decolorized in macroporous resin is passed through adsorbing active carbon column to adsorb formic acid, acetylpropionic acid is eluted with water solution of alcohol, and the eluted solution is decompression concentrated to obtain high content acetylpropionic acid product. The present invention has complete separation of acetylpropionic acid from formic acid, high yield, low production cost, easy industrial application and other advantages.

Description

Technical field [0001] The invention relates to the technical field of adsorption and ion exchange separation and purification, in particular to a method for separating levulinic acid with activated carbon. Background technique [0002] Levulinic acid (Levulinic Acid, LA), also known as 4-oxovaleric acid, levonic acid or pentoxone acid. It has both the properties of carboxylic acid and ketone, so it has good chemical reactivity and can undergo various reactions such as esterification, redox, substitution, polymerization, etc., to synthesize many useful compounds and new polymer materials, including Resins, medicines, fragrances, solvents and inks, rubber and plastic additives, lubricant 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 by asymmetric reduction. Levulinic acid is also a biologically active molecule, as well as an intermediate of pesticides and dyes. In addition, methylt...

Claims

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Application Information

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IPC IPC(8): C07C51/47C07C59/185
Inventor 任其龙刘宝鉴苏宝根杨亦文
Owner ZHEJIANG UNIV
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