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Preparation method of shikimic acid

A technology of shikimic acid and ultrafiltration membrane, which is applied in the field of shikimic acid extraction and purification technology, can solve the problems of inability to concentrate shikimic acid crystal concentration, low enrichment degree of molecular substances, corrosion of stainless steel concentrator, etc., and achieve short cycle and low cost , The effect of less dissolution of impurities

Inactive Publication Date: 2010-06-30
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are a lot of oil and proteoglycan in star anise, which cannot be removed only through general filtration or clarifying agent treatment, resulting in a small amount of resin adsorption and low yield. Shikimic acid is concentrated at high temperature. The higher the concentration, the stronger the acidity, which will seriously corrode the stainless steel concentrator. , at the same time there are a large number of metal ions in the concentrate, it is difficult to achieve crystallization
Simple membrane separation can only remove macromolecular substances. The degree of enrichment is low, and the number of purifications increases. The solubility of shikimic acid in water is 18g / ml. The existing membrane concentration equipment cannot concentrate the concentration of shikimic acid crystals at all.

Method used

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  • Preparation method of shikimic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Take 100kg star anise (shikimic acid content 9%), grind it into 40 mesh, add 500L water, heat to 50°C, stir and extract for 1 hour, extract twice, combine the extracts, filter, add microfiltration membrane system to filter and then pass through the interception The ultrafiltration membrane with a molecular weight of 1000-3000 collects the permeate. The permeate was added to 20L D201 ion exchange resin column for adsorption, first washed with deionized water until neutral, then 100L 5% sodium hydroxide aqueous solution was used to elute shikimic acid, the collected shikimic acid eluate was desalted through 001×7 cationic resin column, The collected column liquid was concentrated under reduced pressure with a graphite concentrator to a density of 1.5, and left to crystallize for 10 hours. The crystals were filtered to obtain 10 kg of crude crystals, which were refluxed with 90% methanol to dissolve, the methanol was recovered to 50 L under reduced pressure, left to crysta...

Embodiment 2

[0029] Take 100kg star anise (shikimic acid content 10%), crush it into 60 mesh, add 600L water, heat to 40°C, stir and extract for 2 hours, extract twice, combine the extracts, filter, add microfiltration membrane system to filter and then pass through the retention The ultrafiltration membrane with a molecular weight of 1000-3000 collects the permeate. The permeate was added to 20L 201×7 ion exchange resin column for adsorption, first washed with deionized water until neutral, then 80L 6% sodium hydroxide aqueous solution was used to elute shikimic acid, and the shikimic acid eluate was collected. 001×8 cation resin column for desalination, collect the column liquid and concentrate it to a density of 1.6 under reduced pressure with a graphite concentrator, and leave it to crystallize for 15 hours. The crystals were filtered to obtain 10.5 kg of crude crystals, which were refluxed with 99% methanol to dissolve, the methanol was recovered to 63 L under reduced pressure, left t...

Embodiment 3

[0031] Take 100kg star anise (shikimic acid content 9%), crush it to 50 mesh, add 550 g of water, heat to 40°C, stir and extract for 1 hour, extract three times, combine the extracts, filter, add microfiltration membrane system to filter and then pass through molecular weight cut off For 1000-3000 ultrafiltration membrane, collect the permeate. The permeate was added to 20L 201×7 ion exchange resin column for adsorption, first washed with deionized water until neutral, then 90L 5% sodium hydroxide aqueous solution was used to elute shikimic acid, and the shikimic acid eluate was collected through 001×7 cationic resin column for desalting, the collected column liquid was concentrated to a density of 1.5 under reduced pressure with a graphite concentrator, and left to crystallize for 16 hours. The crystals were filtered to obtain 10.3 kg of crude crystals, which were refluxed with 95% methanol to dissolve, the methanol was recovered to 60 L under reduced pressure, left to crysta...

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Abstract

The invention relates to a method for purifying shikimic acid by water extraction, membrane separation, ion exchange resin absorption enrichment, graphite concentrator concentration and recrystallization. The method solves the problems of excessive sorts and difficult recycling of organic reagent, small resin exchange capacity, low concentration capacity of glass concentrators and easy erosion of stainless steel concentrators. The method has the advantages of short cycle, high yield and low cost when used in shikimic acid production, and easily realizes industrialization.

Description

Technical field: [0001] The invention relates to an extraction and purification process of shikimic acid, in particular to a method for separating and purifying shikimic acid using membrane technology and ion exchange resin enrichment. Background technique: [0002] Molecular formula and molecular weight of shikimic acid: C7H10O5 (174.15) [0003] [0004] Physical and chemical properties: White fine powder, easily soluble in water, methanol, ethanol, the solubility in water is 18g / 100ml, insoluble in chloroform, benzene and petroleum ether. The melting point is 185°C~191°C, the optical rotation is -180°, and the smell is bitter. [0005] Shikimic acid exists in the dry ripe fruits of Magnoliaceae star anise (Illicium verum Hook.f.). Star anise is a bulk export product, also known as fennel and aniseed. According to Chinese Pharmacopoeia, star anise has the effects of warming yang and dispelling cold, regulating qi and relieving pain. Its fruit, skin and leaves are rich...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C62/32C07C51/42
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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