Water phase/organic phase two-phase extraction-chromatography purification method for gutta-percha

A purification method and organic phase technology, which is applied in the purification field of Eucommia gum aqueous phase/organic phase two-phase extraction-chromatography, which can solve the problems of large pollution of organic volatiles, failure to remove, and large consumption of solvents, etc.

Pending Publication Date: 2022-01-11
JISHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is easy to operate and can improve the purity to a certain extent, but it cannot remove impurities that can also be dissolved in the good solvent.
To achieve better purity, this process needs to be repeated many times, but the multiple recrystallization process is time-consuming, consumes a large amount of solvent, causes large pollution of organic volatiles, and high cost in industrial implementation, which is not an economical and environmentally friendly method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Filtration of Eucommia coarse glue solution:

[0025] Use a filter to filter out the residues visible to the naked eye from the extract obtained by extracting eucommia gum with petroleum ether, and let the glue-containing solution stand at 50°C for 6 hours, and then use a finer filter to remove finer residues to obtain light yellow Containing gum solution, as the next purification raw material.

[0026] 2. Aqueous-organic two-phase extraction:

[0027] Mix the aqueous phase containing 1% chelating agent EDTA and 1% ammonium salt with the Eucommia gum organic solvent obtained in the previous step, the aqueous phase: organic phase volume ratio is 0.5:1 (v / v), and stir at 30°C After 3 hours, let stand to separate the liquid, and take the upper organic phase for later use.

[0028] 3. Column purification:

[0029] The organic phase obtained above was pressurized and continuously flowed through the chromatographic equipment, and the flow rate of the organic phase was 1...

Embodiment 2

[0031] 1. Filtration of Eucommia coarse glue solution:

[0032] The extract obtained by extracting eucommia gum with toluene was filtered through a filter to remove visible residues, and the glue-containing liquid was left to stand at 55°C for 8 hours, and finer residues were filtered through a finer filter to obtain a light yellow Glue, as the next purification raw material.

[0033] 2. Aqueous-organic two-phase extraction:

[0034] Mix the aqueous phase containing 2% chelating agent citric acid and 2% NaOH with the Eucommia gum organic solvent obtained in the previous step, the aqueous phase: organic phase volume ratio is 1:1 (v / v), and stir at 60°C After 2 hours, let stand to separate the liquid, and take the upper organic phase for later use.

[0035] 3. Column purification:

[0036] The organic phase obtained above was pressurized and continuously flowed through the chromatographic equipment, and the flow rate of the organic phase was 3BV / h. The chromatography equipme...

Embodiment 3

[0038] 1. Filtration of Eucommia coarse glue solution:

[0039] The extract obtained by extracting eucommia gum with benzene was filtered through a filter to remove visible residues, and the glue-containing liquid was left to stand at 55°C for 7 hours, and finer residues were filtered through a finer filter to obtain a light yellow Glue, as the next purification raw material.

[0040] 2. Aqueous-organic two-phase extraction:

[0041]Mix the aqueous phase containing 3% chelating agent potassium sodium tartrate and 3% KOH with the Eucommia gum organic solvent obtained in the previous step, the aqueous phase: organic phase volume ratio is 1.5:1 (v / v), at 60 ° C Stir for 1 h, let stand for liquid separation, and take the upper organic phase for later use.

[0042] 3. Column purification:

[0043] The organic phase obtained above was pressurized and continuously flowed through the chromatographic equipment, and the flow rate of the organic phase was 2BV / h. The chromatography eq...

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Abstract

The invention provides a water phase / organic phase two-phase extraction-chromatography purification method for gutta-percha, and belongs to the technical field of gutta-percha purification. The method comprises the following steps: S1, obtaining a to-be-purified crude for gutta-percha solution; S2, performing water phase-organic phase two-phase extraction and purification; and S3, performing chromatographic column purification. According to the method, the eucommia ulmoides crude rubber is subjected to water phase / organic phase two-phase extraction and purification, and metal ions generated by hydrolysis in organic carboxylate are subjected to complexation reaction with a chelating agent in a water phase and exist in the water phase, so that the dissociation of the organic carboxylate is accelerated, and inorganic metal ions in the gutta-percha are more thoroughly removed; wherein organic lipids are hydrolyzed under the catalysis of alkali, and hydrolysate is transferred to a water phase, so that the impurities are removed, and the effective separation and purification of the gutta-percha are achieved. The primary column chromatography purification is carried out on the gutta-percha, and organic impurities such as proteins and phospholipids are effectively separated from the gutta-percha by utilizing polarity difference or an adsorption principle, so that the gutta-percha is purified.

Description

technical field [0001] The invention relates to the technical field of eucommia gum purification, in particular to a purification method of eucommia gum aqueous phase / organic phase two-phase extraction-chromatography. Background technique [0002] Eucommia ulmoides Olive (Eucommia ulmoides Olive) is a deciduous tree belonging to Eucommia ulmoides. , that is, trans polyisoprene. Eucommia gum belongs to hard rubber. Through vulcanization modification or blending with other materials and deep processing, Eucommia gum can develop a series of new functional materials and industrial materials, especially in rubber products and tire industries. Existing studies have shown that the tensile strength, modulus, Shore hardness, and elongation at break of Eucommia gum and natural rubber blends have almost no change before the blending ratio is 1:1. Eucommia gum has the excellent characteristic of low dynamic mechanical loss. The dynamic mechanical loss is only 1 / 5 of that of butadiene ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/00C08L7/00
CPCC08J3/00C08J2307/00
Inventor 陈上王东慧李佑稷韩张英
Owner JISHOU UNIVERSITY
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