CN100387591C - Removal of caffeine from polyhydric phenol by supercritical carbon dioxide process - Google Patents
Removal of caffeine from polyhydric phenol by supercritical carbon dioxide process Download PDFInfo
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- CN100387591C CN100387591C CNB2004100540097A CN200410054009A CN100387591C CN 100387591 C CN100387591 C CN 100387591C CN B2004100540097 A CNB2004100540097 A CN B2004100540097A CN 200410054009 A CN200410054009 A CN 200410054009A CN 100387591 C CN100387591 C CN 100387591C
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The present invention relates to a removal method of caffeine from tea polyphenol by supercritical carbon dioxide. Food-grade CO2 is adopted; the food-grade CO2 is converted into supercritical CO2 by pressurization and is used as an extraction solvent. Firstly, raw material tea polyphenol is placed into a supercritical extraction kettle; after CO2 is driven into the supercritical extraction kettle, the raw materials are sufficiently soaked under the condition of high voltage CO2; then, extraction is carried out by a continuous extraction way; the caffeine is selectively extracted by selecting technical parameters, such as temperature, pressure, time, etc., according to the theory that polyphenol substances, such as catechin in the tea polyphenol, etc., and the caffeine have different dissolvability in the supercritical CO2. Accordingly, tea polyphenol products which do not have residual solvent and have a low caffeine content can be obtained. Accordingly, the caffeine from tea polyphenol can be used for the aspects, such as high-grade food antioxidants, health foods, medicines, etc.
Description
Technical field
The present invention relates to a kind of method that removes caffeine in the tea-polyphenol, relate in particular to and a kind ofly remove the method for caffeine in the tea-polyphenol, adopt supercritical CO with supercritical co
2Be solvent, remove the caffeine in the tea-polyphenol, obtain the tea-polyphenol product of low caffeine content.Belong to tea products deep processing field.
Background technology
Tea-polyphenol (Tea polyhenols) is a kind of polyphenolic compound that extracts from tealeaves.Nearest studies show that, that tea-polyphenol has is anticancer, radioprotective, anti-ageing, anti-inflammatory, effect such as antibacterial, has important use to be worth at protective foods, aspect medical.Yet directly the tea-polyphenol product that extraction obtains from tealeaves generally contains the caffeine about 2%～10%.Excessive caffeine may influence the physiological system of human body, shows lather, insomnia, easily wakes up, diarrhoea, headache and cardio palmus shape.Medicines and health protection with the tea-polyphenol product in requiring product, must not detect hazardous solvent residual, special requirement content of caffeine＜1% also.At present, the method for acquisition low caffeine content tea-polyphenol mainly contains ion precipitation method, absorption method and supercritical fluid extraction.(Hubei chemical industry such as Yuan Hua, the third phase in 2000,12-14) utilize the ion precipitation method to prepare the tea-polyphenol of low caffeine content, according to tea-polyphenol can be with the metal ion co-precipitation not with the character of caffeine co-precipitation, in the water extract of tealeaves, add metal ion, form tea-polyphenol-precipitation by metallic ion thing, filtration obtains throw out, add acid dissolving, use the organic solvent extraction tea-polyphenol, obtain content of caffeine after the precipitation drying less than 1% tea-polyphenol product.This method operation is loaded down with trivial details, and product exists organic solvent and the residual problem that exceeds standard of metal ion; United States Patent (USP) (5,702,747) adopts the caffeine in the activated carbon fiber absorption removal green tea water crude extract, but caffeine is resolved relatively difficulty again from activated carbon fiber, make the utilization ratio of carbon fiber not high, and the products production cost increases.Patent (86103112) " is removed the method for caffeine in the tealeaves " and is adopted supercritical CO
2Directly caffeine is removed in extraction from tealeaves, is raw material but do not relate to the tea-polyphenol, removes wherein caffeine.
Summary of the invention
The objective of the invention is at above-mentioned the deficiencies in the prior art, provide a kind of and remove the method for caffeine in the tea-polyphenol with supercritical co, obtain the tea-polyphenol product of noresidue solvent, low caffeine content, technical process is simple, is suitable for suitability for industrialized production.
For realizing such purpose, the present invention adopts food-class CO
2, be converted into supercritical CO by pressurization
2As extraction solvent.Earlier tea polyphenol raw materials is put into supercritical extraction reactor, squeeze into CO
2Make raw material at high pressure CO
2Down fully dipping extracts in the continuous extraction mode then, by selecting processing parameters such as temperature, pressure, time, according to polyphenol substance such as catechin in the tea-polyphenol and caffeine at supercritical CO
2The principle of different solubility, selectively caffeine is extracted, obtain the product of low caffeine content.
Method of the present invention comprises raw material dipping and circulation two steps of extraction, and is specific as follows:
(1) raw material dipping: tea polyphenol raw materials is put into supercritical extraction reactor, squeeze into CO with high-pressure pump
2Press 8～30MPa to still, the still temperature is made as 32-55 ℃, closes high-pressure pump, pressurize, makes raw material at high pressure CO
2Middle static dipping 0.5-2 hour.
(2) circulation is extracted: open the extraction kettle terminal valve, start high-pressure pump, keep still pressure, temperature-resistant, CO
2Flow velocity be made as 10～40kg/h, the temperature of separator is made as 40-50 ℃, pressure 4-7MPa, continuous cycling extraction raw material in extraction kettle-separator-extraction kettle extraction loop, after 1～4 hour, collect the tea-polyphenol product that obtains low caffeine content at extraction kettle.
Caffeine is at supercritical CO
2In solubleness bigger than polyphenol substances such as catechins, thereby at first be extracted out, enter separator because separator pressure is lower, caffeine is precipitated out in separator, is enriched in the separator bottom, CO
2Then become gas again and turn back to the extraction that extraction kettle carries out next round; Polyphenol substances such as the catechin in the tea-polyphenol are still stayed in the extraction kettle.After the extraction, can collect the tea-polyphenol product that obtains low caffeine content from extraction kettle.
Tea-polyphenol of the present invention refers to the green tea water crude extract of different catechin content.
The CO that the present invention adopts
2After can becoming liquid through refrigeration earlier, inject extraction kettle by high-pressure pump again.
Adopt method products obtained therefrom content of caffeine of the present invention 0.3%～1%.This product noresidue solvent can be used for aspects such as gourmet food antioxidant, protective foods, medicine.Technology of the present invention is simple, and compliance with environmental protection requirements is suitable for suitability for industrialized production.
Embodiment
Below by specific embodiment technical scheme of the present invention and the effect that reaches thereof are further described.
Embodiment 1:
Take by weighing 100 gram tea polyphenol raw materials, wherein catechin content is 80.0%, and content of caffeine 3% is put into supercritical extraction reactor, injects CO with high-pressure pump
2Press 8MPa to still, the still temperature is made as 32 ℃, closes the extraction kettle terminal valve, closes high-pressure pump, pressurize, static dipping raw material 0.5 hour.Open the extraction kettle terminal valve, start high-pressure pump, the maintenance still is pressed, the still temperature is constant, CO
2Flow velocity be made as 10kg/h, the temperature of separator is made as 40 ℃, pressure is 4MPa, cycling extraction raw material continuously in extraction kettle-separator one extraction kettle extraction loop.
Caffeine is at supercritical CO
2In solubleness bigger than polyphenol substances such as catechins, thereby at first be extracted out, enter separator because separator pressure is lower, coffee precipitates in separator, is enriched in the separator bottom, CO
2Then become gas again again and get back to the extraction that extraction kettle carries out next round; Polyphenol substances such as the catechin in the tea-polyphenol are still stayed in the extraction kettle.
After 1 hour, stop extraction, release, open extraction kettle, collect the tea-polyphenol product that obtains low caffeine content, wherein catechin content is 80.3%, content of caffeine 1.0%.
Embodiment 2:
Take by weighing 100 gram tea polyphenol raw materials, wherein catechin content is 90.0%, and content of caffeine 2% is put into supercritical extraction reactor, injects CO with high-pressure pump
2Press 15MPa to still, the still temperature is made as 40 ℃, closes the extraction kettle terminal valve, closes high-pressure pump, pressurize, static dipping raw material 1 hour.Open the extraction kettle terminal valve, start high-pressure pump, the maintenance still is pressed, the still temperature is constant, CO
2Flow velocity be made as 20kg/h, the temperature of separator is made as 45 ℃, pressure is 5MPa, cycling extraction raw material continuously in extraction kettle-separator-extraction kettle extraction loop.After 3 hours, stop extraction, release, open extraction kettle, collect the tea-polyphenol product that obtains low caffeine content, wherein catechin content is 90.0%, content of caffeine 0.8%.
Embodiment 3:
Take by weighing 100 gram tea polyphenol raw materials, wherein catechin content is 93.0%, and content of caffeine 2.8% is put into supercritical extraction reactor, injects CO with high-pressure pump
2Press 30MPa to still, the still temperature is made as 55 ℃, closes the extraction kettle terminal valve, closes high-pressure pump, pressurize, static dipping raw material 2 hours.Open the extraction kettle terminal valve, start high-pressure pump, the maintenance still is pressed, the still temperature is constant, CO
2Flow velocity be made as 40kg/h, the temperature of separator is made as 50 ℃, pressure 7MPa, cycling extraction raw material continuously in extraction kettle-separator-extraction kettle extraction loop.After 4 hours, stop extraction, release, open extraction kettle, collect the tea-polyphenol product that obtains low caffeine content, wherein catechin content is 92.0%, content of caffeine 0.3%.
Claims (3)
1. one kind removes the method for caffeine in the tea-polyphenol with supercritical co, it is characterized in that adopting supercritical CO
2As extraction solvent, divide following two steps to carry out:
1) raw material dipping: tea polyphenol raw materials is put into supercritical extraction reactor, squeeze into CO with high-pressure pump
2Press 8～30MPa to still, the still temperature is made as 32-55 ℃, closes high-pressure pump, pressurize, makes raw material at high pressure CO
2Middle static dipping 0.5-2 hour;
2) circulation is extracted: open the extraction kettle terminal valve, start high-pressure pump, keep still pressure, temperature-resistant, CO
2Flow velocity be made as 10～40kg/h, the temperature of separator is made as 40-50 ℃, and pressure is 4-7MPa, continuous cycling extraction raw material in extraction kettle-separator-extraction kettle extraction loop, after 1～4 hour, collect the tea-polyphenol product that obtains low caffeine content at extraction kettle.
2. as claimed in claim 1ly remove the method for caffeine in the tea-polyphenol, it is characterized in that described CO with supercritical co
2After becoming liquid through refrigeration earlier, inject extraction kettle by high-pressure pump again.
3. as claimed in claim 1ly remove the method for caffeine in the tea-polyphenol, it is characterized in that described tea-polyphenol refers to the green tea water crude extract of different catechin content with supercritical co.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100540097A CN100387591C (en) | 2004-08-26 | 2004-08-26 | Removal of caffeine from polyhydric phenol by supercritical carbon dioxide process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100540097A CN100387591C (en) | 2004-08-26 | 2004-08-26 | Removal of caffeine from polyhydric phenol by supercritical carbon dioxide process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1613855A CN1613855A (en) | 2005-05-11 |
| CN100387591C true CN100387591C (en) | 2008-05-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2004100540097A Expired - Fee Related CN100387591C (en) | 2004-08-26 | 2004-08-26 | Removal of caffeine from polyhydric phenol by supercritical carbon dioxide process |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100411528C (en) * | 2005-07-25 | 2008-08-20 | 美晨集团股份有限公司 | Technique for removing caffeine in tea through supercritical carbon dioxide extraction method |
| CN100379732C (en) * | 2006-02-28 | 2008-04-09 | 浙江大学 | Method for removing caffeine from theapolyphenol coarse extract |
| CN102924453A (en) * | 2010-08-02 | 2013-02-13 | 张海 | Process method for extracting theine from teas |
| CN102504954B (en) * | 2011-10-26 | 2014-01-15 | 四川中测科技投资有限公司 | Method for extracting essences from tea leaves |
| CN103300182A (en) * | 2013-04-15 | 2013-09-18 | 杭州艾菲曼普香精香料有限公司 | Method for extracting aromatic substances and tea polyphenols from tea leaves step by step |
| CN104757220B (en) * | 2015-05-06 | 2016-05-25 | 美町宝植物科技(中国)有限公司 | Decaffeination production technology of oolong |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1008507B (en) * | 1985-05-02 | 1990-06-27 | Skw特罗斯特贝格股份公司 | Process for decaffeination of tea |
| CN1253940A (en) * | 1998-11-12 | 2000-05-24 | 无锡轻工大学 | Method for extracting tea-polyphenol from tea |
| CN1482126A (en) * | 2003-07-21 | 2004-03-17 | 红河唐人生物发展有限公司 | Tea polyphenols extracting process |
-
2004
- 2004-08-26 CN CNB2004100540097A patent/CN100387591C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1008507B (en) * | 1985-05-02 | 1990-06-27 | Skw特罗斯特贝格股份公司 | Process for decaffeination of tea |
| CN1253940A (en) * | 1998-11-12 | 2000-05-24 | 无锡轻工大学 | Method for extracting tea-polyphenol from tea |
| CN1482126A (en) * | 2003-07-21 | 2004-03-17 | 红河唐人生物发展有限公司 | Tea polyphenols extracting process |
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| CN1613855A (en) | 2005-05-11 |
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