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Preparation method of curcumin with low solvent residue

A low-solvent residue, curcumin technology, applied in the separation/purification of carbonyl compounds, organic chemistry and other directions, can solve problems such as increasing production costs, many extraction steps, and no solvent, so as to improve production efficiency and safety, reduce The amount and type of use, the effect of avoiding cumbersome processes

Active Publication Date: 2020-01-24
CHENGUANG BIOTECH GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Exist in the prior art the extraction of many curcumin, the method for separating and purifying, wherein also relate to the preparation technology of low soluble curcumin, as, CN107805193A discloses a kind of production method of low soluble curcumin crystal, by adding emulsifier and essence Reagents such as preparations to obtain low residual curcumin, but this process uses a large amount of organic solvents and surfactants, the addition of reagents not only increases the production cost but also increases the risk of introducing new impurities
CN106866397A discloses a low-cost and high-efficiency curcumin extraction method. Dried turmeric is extracted with ethanol, the extract is concentrated, extracted with petroleum ether, concentrated again, dissolved in sodium hydroxide and extracted with ethyl acetate to obtain the initial extract. The initial extract is dissolved in ethanol, and then adsorbed and separated with special tools to obtain high-purity curcumin. This method has many extraction steps, uses a variety of reagents, and requires special separation tools, which is not universally applicable.
CN101831199A discloses a method for extracting curcumin with fast extraction speed. Turmeric is ground into powder and then steamed for granulation. Gained turmeric granules are extracted with leaching after granulation. Although this method is relatively fast, the purity of the extract is not high. High, and did not solve the problem of solvent residue in the extracted product
There is a literature (Chen Lingtong, cooling crystallization separation and purification of curcumin, Zhejiang Chemical Industry, 2019, 50(5):25-27) to investigate the influence of cooling speed, stirring method, and whether to add crystal seeds on the crystallization yield and crystal purity of curcumin, Although this document discloses that curcumin crystals of higher purity are obtained by cooling, stirring, and adding crystal seeds, the crystallization process still needs to use an organic solvent as a crystallization agent, which increases production costs and steps, and does not give a solution to the problem of solvents. residue issues

Method used

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  • Preparation method of curcumin with low solvent residue
  • Preparation method of curcumin with low solvent residue
  • Preparation method of curcumin with low solvent residue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Prepare turmeric extract: get 300g of turmeric raw material and pulverize it, extract with 1.8L ethyl acetate, filter after extraction, and obtain curcumin extract;

[0036] (2) Concentration of the extract: take the extract of step (1) and concentrate it by rotary evaporation until the solid content is 45%;

[0037](3) Primary crystallization: heat the turmeric concentrate in step (2) in a water bath at 25° C., stir and crystallize, and filter after no more crystals are precipitated. The obtained filter cake is independently processed and sold as an intermediate product;

[0038] (4) Desolventization of the mother liquor: take the mother liquor obtained by filtration in step (3) and remove the residual solvent at -0.05±0.01MPa at 60°C;

[0039] (5) Secondary crystallization: Add 0.01g of curcumin crystal nuclei with dissolved residue<10ppm to the low dissolved residue mother liquor obtained in step (4), cool to 55°C and keep warm, stir at 60r / min until the crystals...

Embodiment 2

[0043] (1) Prepare turmeric extract: get 0.5kg of turmeric raw material to pulverize, extract with a mixed solution of 3L acetone, and suction filter after extraction to obtain curcumin extract;

[0044] (2) Concentration of the extract: take the extract of step (1) and concentrate it by rotary evaporation until the solid content is 60%;

[0045] (3) Primary crystallization: heat the turmeric concentrate in step (2) in a water bath at 20° C., stir and crystallize, and filter after no more crystals are precipitated. The obtained filter cake is independently processed and sold as an intermediate product;

[0046] (4) Desolventization of mother liquor: take the mother liquor obtained by filtration in step (3) and remove residual solvent at -0.06±0.01MPa at 50°C;

[0047] (5) Secondary crystallization: Add 0.19g of curcumin with a residual <10ppm in the low-dissolved mother liquor obtained in step (4) as a crystal nucleus, cool to 40°C and keep warm, stir at a speed of 30r / min, un...

Embodiment 3

[0051] (1) Prepare turmeric extract: get 2 kg of turmeric raw materials and pulverize, extract with a mixed solution of 12L ethanol, and suction filter after extraction to obtain curcumin extract;

[0052] (2) Concentration of the extract: take the extract of step (1) and concentrate it by rotary evaporation until the solid content is 50%;

[0053] (3) Primary crystallization: heat the turmeric concentrate in step (2) in a 50°C water bath, stir and crystallize, and filter after no more crystals are precipitated, and the obtained filter cake is independently processed and sold as an intermediate product;

[0054] (4) Mother liquor desolvation residue: take the mother liquor obtained by filtration in step (3) and remove the residual solvent at 50° C. at -0.05±0.01MPa;

[0055] (5) Secondary crystallization: Add 0.92g of curcumin with residual <10ppm to the mother liquor with low dissolved residue obtained in step (4) as crystal nuclei, cool to 60°C and keep warm, stir at 30r / min...

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Abstract

The invention discloses a preparation method of curcumin with low solvent residue. The method comprises the following process steps: extracting a turmeric raw material with a solvent, concentrating the obtained extract to a certain extent, carrying out heat-insulation stirring for primary crystallization, separating obtained crystals to obtain common curcumin, removing the solvent residue from a crystallized mother liquor, and carrying out secondary crystallization on the low-solvent-residue mother liquor to produce curcumin with low solvent residue. The method obtains the finished curcumin with the low solvent residue by controlling the crystallization procedure and parameters without adding a crystallizing agent, so the solvent raw material is saved, and the working procedure is simplified.

Description

technical field [0001] The invention belongs to the field of preparation of natural extracts, and relates to a preparation method suitable for industrial production and efficiently obtaining curcumin with low solvent residue. Background technique [0002] Curcuminoids are natural yellow phenolic compounds extracted from plants of the genus Curcuma (Curcuma, Zingiberaceae) such as turmeric, zedoary, and turmeric. The content of curcuminoids in turmeric rhizomes is relatively high. Curcumin is currently widely used in medicine, food, feed and dyeing industries. Curcumin is a kind of natural food pigment, which can dye protein, and the dyeing effect is strong; curcumin has strong anti-corrosion ability and will not produce side effects. In the process of food production at home and abroad, curcumin is often used as a natural color. food additives. [0003] my country's current curcumin extraction process mainly uses solvent extraction, and the extraction solvent includes ethy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/78C07C49/255C07C45/81
CPCC07C45/78C07C45/81C07C49/255
Inventor 齐立军彭静维高伟褚延伟黄利勇
Owner CHENGUANG BIOTECH GRP CO LTD