CN105712897A - Tea polyphenol extracting and recycling method - Google Patents
Tea polyphenol extracting and recycling method Download PDFInfo
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- CN105712897A CN105712897A CN201610049481.4A CN201610049481A CN105712897A CN 105712897 A CN105712897 A CN 105712897A CN 201610049481 A CN201610049481 A CN 201610049481A CN 105712897 A CN105712897 A CN 105712897A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D473/00—Heterocyclic compounds containing purine ring systems
- C07D473/02—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
- C07D473/04—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms
- C07D473/06—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3
- C07D473/12—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3 with methyl radicals in positions 1, 3, and 7, e.g. caffeine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Tea And Coffee (AREA)
- Fertilizers (AREA)
Abstract
The invention relates to a tea polyphenol extracting and recycling method, comprising the steps: continuous countercurrent extraction: charging raw tea leaves that are subjected to picking and screening pretreatment into an extracting channel by a charging device, pushing the tea leaves to move along the channel by mechanical forces of scrapers and a screw, fully contacting a solvent for extracting, wringing at a discharge segment and discharging; after an extraction solvent enters the extracting channel and flows from high to low under the gravitational action, discharging tea leave extract from an overflow port to obtain catechin residue; separating and collecting theanine in the catechin residue by using an ultrafiltration membrane and a reverse osmosis membrane that are 3500 Da in molecular weight; subjecting the theanine separated in the former step to ultrafiltration and decoloring pretreatment, selecting an adsorbing process including pH 3.4, liquid concentration 3.0 mg/ml and flow speed 1.7 column-bed volume per hour, eluting with ammonia water 11.3 in pH to obtain the theanine; subjecting the catechin residue with the theanine separated to supercritical CO2 extraction to obtain caffeine and tea polyphenols, and freeze-drying to obtain a finished product. The tea polyphenols obtained by the method are high in purity and yield and are cyclically obtainable.
Description
Technical field
The present invention relates to tea polyphenol extract circulation utilization method.
Background technology
Extracting tea polyphenols effective component yield low, waste is big, and cost is high；Can not Appropriate application tea grounds, make theanine discard；Take off when washing caffeine without absorption affinity；Nutrient loss.
Summary of the invention
For the problems referred to above, the present invention provides a kind of tea polyphenol extract circulation utilization method, comprises the following steps:
(1) Continuous Countercurrent Extraction: the tea raw material through plucking, screen pretreatment is put into extraction tank by charging device, moves along groove, after being fully contacted extraction with solvent, be discharged after discharging section water squeezing under the mechanical force of scraper plate and spiral promotes；Extraction solvent flows after entering extraction tank under gravity from high to low, and tea extract is discharged from overfall, i.e. catechin slag.(2) tea grounds separation tea base acid, adopts the ultrafilter membrane of molecular weight 3500Da, reverse osmosis membrane to separate and collect the theanine in catechin slag..The ultrafilter membrane of molecular weight 3500Da, reverse osmosis membrane is adopted to separate and collect the theanine in catechin slag, comprehensive yield reaches 54.05%, product purity reaches 10%, tea grounds biological value is up to 55%, it it is the primary raw material of fertilizer, which enhance the comprehensive benefit that Folium Camelliae sinensis deep development utilizes, reduce further production cost.
(3) ion exchange column technique: ion exchange extracts theanine；Theanine step (2) separated is again through after ultrafiltration, decolouring pretreatment, and selected absorbing process condition is pH3.4, liquid concentration 3.0mg/ml, flow velocity 1.7 bed volume per hour, after the ammonia eluting of pH11.3, obtains theanine.Obtaining theanine content is 58%, and the theanine response rate is 82%, while obtaining benefit, decreases contaminated wastewater
(4) supercritical CO2Extraction process: the catechin slag after the theanine separate step (2) is through supercritical CO2Caffeine, tea polyphenols are obtained by extraction, after freeze-dried, obtain product.
Solvent in step (1) is any one in water, ethanol, acetone, it is preferred to water.
In step (1), tea raw material and solvent do reverse extraction, the contact surface of tea raw material and solvent is under concentration difference state all the time, after multistage vadose solution extracts, Folium Camelliae sinensis material slag is discharged, extracting solution is then penetrated into step by step by effective content of tea and becomes high concentration extracting solution, and flows out from opposite direction.
The mass concentration difference of the contact surface of tea raw material and solvent is 20%-30%, and extracting solution is then penetrated into step by step by effective content of tea and becomes high concentration extracting solution, and the mass concentration of its high concentration extracting solution is 70%-80%.
Supercritical extraction described in step (4) can also be extracted for algae, namely, catechin slag after the theanine separate step (2) is placed in algae, in dark, after stirring 10-12h, use alcoholic solution gradient elution, tea polyphenols after reclaiming ethanol fluidised bed spray drying, can be obtained.
Described algae is any one in chlorella, Nannochloropsis oceanica, very thin Euglena, spirulina maxim.The mass ratio of described catechin slag and algae is 10-15:1-3.
Algae has stronger absorption property, the present invention utilizes algae to be adsorbed under dark (light presents a note to the growth affecting chlorella) condition by the tea polyphenols in catechin slag, upon adsorption complete after, then in alcoholic solution, eluting is adsorbed with the algae of tea polyphenols, makes tea polyphenols purer.
In the present invention, Continuous Countercurrent Extraction, this technique is applied in tea comprehensive processing process, and Folium Camelliae sinensis and hot water do the motion of rightabout continuous flow upstream in extraction element simultaneously, realizing the continuous isolation operation of tea juice or extract in counter-current process, Folium Camelliae sinensis inclusions leaching rate is high.Compared with domestic intermittent extraction process commonly used at present, the advantage that Continuous Countercurrent Extraction has extract concentration height, effective component extraction rate is high, can improve tea raw material utilization rate.
This technique realizes the totally-enclosed operation of serialization, dynamic countercurrent extraction, plays and saves manpower, reduces solvent load, reduces production cost, improves the effect of production efficiency.It is made up of charging device, transportation sprocket assembly, transmission band, scraper plate, solvent inlet, extracting liquid outlet, slag-drip opening etc..First, the tea raw material through pretreatment is put into extraction tank by charging device, moves along groove, after being fully contacted extraction with water equal solvent, be discharged after discharging section water squeezing under the mechanical force of scraper plate and spiral promotes；The Extraction solvent such as water flow after entering extraction tank under gravity from high to low, and tea extract is discharged from overfall.The Extraction solvent such as tea raw material and water, both make reverse movement, contact interface is under concentration difference state all the time, after multistage vadose solution extracts, Folium Camelliae sinensis material slag is discharged, extracting solution then becomes high concentration extracting solution due to the infiltration step by step of effective content of tea, flows out from opposite direction, thus realizing the extraction to greatest extent of effective ingredient in Folium Camelliae sinensis.
Supercritical CO2In extraction process, CO2Being nonpolar molecule, caffeine is also nonpolar molecule, and catechin is polar molecule, so caffeine is easily by supercritical CO2Extract, and tea polyphenols is at supercritical CO2Middle dissolution rate is extremely low, thus can be used for extracting caffeine, purification tea polyphenols.Supercritical fluid is in more than critical temperature, critical pressure, the fluid between gas and liquid.Supercritical fluid extraction, it is simply that using a certain critical fluids (the such as CO as solvent2) contact with solid or liquid mixture, utilize balancing each other and transmission characteristic of their "abnormal", extract object, then decompression or the method heated up are adopted, reduce the density (dissolving power) of extraction phase, make solvent separate with extract again, utilize the balance each other difference of state of each component under different condition to separate.Compared with other extracting process, supercritical fluid extraction has that rate of extraction is fast, consumed energy is few, solvent-oil ratio is few, the not advantage such as residual.In the extraction of thermographic compound, can make to be extracted material and not go bad because of oxidation, decomposition, loss.Can have a lot as the material of supercritical fluid, wherein with CO2 better performances, 1) inexpensive, easily make high-purity gas.2) critical temperature is low, it is simple to operation, be suitable for heat-sensitive substance extract 3) nontoxic, tasteless, do not remain, nonflammable, free from environmental pollution.4) chemical inertness, it is to avoid tea polyphenols aoxidizes.
The present invention is also with lignocellulose adsorption column separation.Lignin and cellulose, hemicellulose are the main components of Plant fiber.Adopting the waste materials such as wood flour, in the material of the processing of soda acid, lignin and cellulose exist simultaneously, are called lignocellulose.Polyphenols in solution is had good adsorption effect by this material, but to caffeine without absorbability.Through lignocellulose post, tea polyphenols solution being removed caffeine, uses alcoholic solution gradient elution, reclaim ethanol, bed spray obtains polyphenol content after drying > 98%, catechin total amount 60-95%, EGCG content 60%-90%, caffeine content 0.5%-1%.Yield 10%-11%.
Vacuum lyophilization, vacuum freeze-drying, dry also known as molecule.Being applied to the processing with the Folium Camelliae sinensis extract of high added value, its operation principle is to be freezed by present-35 DEG C of tea extract, makes moisture become solid ice, then under higher vacuum, is directly distilled by ice and remove for gaseous form, make material dewatering dry.Low temperature, vacuum dry run, maintain the color of dried object, shape to greatest extent, and protect contained nutritional labeling.
Continuous Countercurrent Extraction has extract concentration height, effective component extraction rate height；
Adopt the ultrafilter membrane of molecular weight 3500Da, reverse osmosis membrane to separate and improve the comprehensive benefit that Folium Camelliae sinensis deep development utilizes, reduce further production cost；
Ion exchange extracts theanine, and obtaining theanine content is 58%, and the theanine response rate is 82%, while obtaining benefit, decreases contaminated wastewater；
Supercritical fluid extraction has that rate of extraction is fast, consumed energy is few, solvent-oil ratio is few, not residual.
Detailed description of the invention
Embodiment 1
A kind of tea polyphenol extract circulation utilization method, comprises the following steps:
(1) Continuous Countercurrent Extraction: the tea raw material through plucking, screen pretreatment is put into extraction tank by charging device, moves along groove, after being fully contacted extraction with water, be discharged after discharging section water squeezing under the mechanical force of scraper plate and spiral promotes；Extraction solvent flows after entering extraction tank under gravity from high to low, and tea extract is discharged from overfall, i.e. catechin slag；
Tea raw material and solvent do reverse extraction, the contact surface of tea raw material and solvent is under concentration difference state all the time, and after multistage vadose solution extracts, Folium Camelliae sinensis material slag is discharged, extracting solution is then penetrated into step by step by effective content of tea and becomes high concentration extracting solution, and flows out from opposite direction.The mass concentration difference of the contact surface of tea raw material and solvent is 25%, and extracting solution is then penetrated into step by step by effective content of tea and becomes high concentration extracting solution, and the mass concentration of its high concentration extracting solution is 74%.(2) tea grounds separation tea base acid, adopts the ultrafilter membrane of molecular weight 3500Da, reverse osmosis membrane to separate and collect the theanine in catechin slag；
(3) ion exchange column technique: ion exchange extracts theanine；
Theanine step (2) separated is again through after ultrafiltration, decolouring pretreatment, and selected absorbing process condition is pH3.4, liquid concentration 3.0mg/ml, flow velocity 1.7 bed volume per hour, after the ammonia eluting of pH11.3, obtains theanine；
(4) supercritical CO2Extraction process: the catechin slag after the theanine separate step (2) is through supercritical CO2Caffeine, tea polyphenols are obtained by extraction, after freeze-dried, obtain product.
The theanine content obtained is 58%, and the theanine response rate is 82%, polyphenol content > 99%, and catechin total amount is 81%, and EGCG content is 79.3%, and caffeine content is 0.74%.
Embodiment 2
A kind of tea polyphenol extract circulation utilization method, comprises the following steps:
(1) Continuous Countercurrent Extraction: the tea raw material through plucking, screen pretreatment is put into extraction tank by charging device, moves along groove, after being fully contacted extraction with water, be discharged after discharging section water squeezing under the mechanical force of scraper plate and spiral promotes；Extraction solvent flows after entering extraction tank under gravity from high to low, and tea extract is discharged from overfall, i.e. catechin slag；Tea raw material and solvent do reverse extraction, the contact surface of tea raw material and solvent is under concentration difference state all the time, after multistage vadose solution extracts, Folium Camelliae sinensis material slag is discharged, extracting solution is then penetrated into step by step by effective content of tea and becomes high concentration extracting solution, and flows out from opposite direction, and the mass concentration difference of the contact surface of tea raw material and solvent is 22%, extracting solution is then penetrated into step by step by effective content of tea and becomes high concentration extracting solution, and the mass concentration of its high concentration extracting solution is 80%.(2) tea grounds separation tea base acid, adopts the ultrafilter membrane of molecular weight 3500Da, reverse osmosis membrane to separate and collect the theanine in catechin slag；
(3) ion exchange column technique: ion exchange extracts theanine；
Theanine step (2) separated is again through after ultrafiltration, decolouring pretreatment, and selected absorbing process condition is pH3.4, liquid concentration 3.0mg/ml, flow velocity 1.7 bed volume per hour, after the ammonia eluting of pH11.3, obtains theanine；
(4) the catechin slag after theanine step (2) separated is placed in chlorella in (mass ratio of described catechin slag and algae is 10:1) dark, after stirring 10-12h, use alcoholic solution gradient elution, tea polyphenols after reclaiming ethanol fluidised bed spray drying, can be obtained.
The theanine content obtained is 58%, and the theanine response rate is 82%, polyphenol content > 99%, and catechin total amount is 96%, and EGCG content is 85%, and caffeine content is 0.88%.
Embodiment 3
Step leads to embodiment 2, enters chlorella and replaces with Nannochloropsis oceanica, and the mass ratio of catechin slag and algae is 12:1.6.The theanine content obtained is 58%, and the theanine response rate is 82%, polyphenol content > 99%, and catechin total amount is 94.5%, and EGCG content is 83.2%, and caffeine content is 0.7%.
Embodiment 4
Step leads to embodiment 2, enters chlorella and replaces with very thin Euglena, and the mass ratio of catechin slag and algae is 13:2.2.The theanine content obtained is 58%, and the theanine response rate is 82%, polyphenol content > 99%, and catechin total amount is 91.9%, and EGCG content is 86.7%, and caffeine content is 0.65%.
Embodiment 4
Step leads to embodiment 2, enters chlorella and replaces with spirulina maxim, and the mass ratio of catechin slag and algae is 14:3.The theanine content obtained is 58%, and the theanine response rate is 82%, polyphenol content > 99%, and catechin total amount is 95.5%, and EGCG content is 82.6%, and caffeine content is 0.72%.
Claims (7)
1. a tea polyphenol extract circulation utilization method, it is characterised in that comprise the following steps:
(1) Continuous Countercurrent Extraction: the tea raw material through plucking, screen pretreatment is put into extraction tank by charging device, moves along groove, after being fully contacted extraction with solvent, be discharged after discharging section water squeezing under the mechanical force of scraper plate and spiral promotes；Extraction solvent flows after entering extraction tank under gravity from high to low, and tea extract is discharged from overfall, i.e. catechin slag；
(2) tea grounds separation tea base acid, adopts the ultrafilter membrane of molecular weight 3500Da, reverse osmosis membrane to separate and collect the theanine in catechin slag；
(3) ion exchange column technique: ion exchange extracts theanine；
Theanine step (2) separated is again through after ultrafiltration, decolouring pretreatment, and selected absorbing process condition is pH3.4, liquid concentration 3.0mg/ml, flow velocity 1.7 bed volume per hour, after the ammonia eluting of pH11.3, obtains theanine；
(4) supercritical CO2Extraction process: the catechin slag after the theanine separate step (2) is through supercritical CO2Caffeine, tea polyphenols are obtained by extraction, after freeze-dried, obtain product.
2. the tea polyphenol extract circulation utilization method described in claim 1, it is characterised in that the solvent in step (1) is any one in water, ethanol, acetone, it is preferred to water.
3. the tea polyphenol extract circulation utilization method described in claim 1, it is characterized in that, in step (1), tea raw material and solvent do reverse extraction, the contact surface of tea raw material and solvent is under concentration difference state all the time, and after multistage vadose solution extracts, Folium Camelliae sinensis material slag is discharged, extracting solution is then penetrated into step by step by effective content of tea and becomes high concentration extracting solution, and flows out from opposite direction.
4. the tea polyphenol extract circulation utilization method described in claim 1, it is characterized in that, the mass concentration difference of the contact surface of tea raw material and solvent is 20%-30%, extracting solution is then penetrated into step by step by effective content of tea and becomes high concentration extracting solution, and the mass concentration of its high concentration extracting solution is 70%-80%.
5. the tea polyphenol extract circulation utilization method described in claim 1, it is characterized in that, supercritical extraction described in step (4) can also be extracted for algae, namely, catechin slag after the theanine separate step (2) is placed in algae, in dark, after stirring 10-12h, use alcoholic solution gradient elution, tea polyphenols after reclaiming ethanol fluidised bed spray drying, can be obtained.
6. the tea polyphenol extract circulation utilization method described in claim 5, it is characterised in that described algae is any one in chlorella, Nannochloropsis oceanica, very thin Euglena, spirulina maxim.
7. the tea polyphenol extract circulation utilization method described in claim 5, it is characterised in that the mass ratio of described catechin slag and algae is 10-15:1-3.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107712169A (en) * | 2017-11-20 | 2018-02-23 | 福建省农业科学院茶叶研究所 | A kind of tea Processing method |
| CN107913530A (en) * | 2017-11-24 | 2018-04-17 | 广西中港高科国宝金花茶产业有限公司 | A kind of CO2The method that supercritical methanol technology fluid extracts tea polyphenols from Camellia nitidissima |
| CN110437203A (en) * | 2019-07-15 | 2019-11-12 | 湖南鑫文天生物科技有限公司 | Scale Continuous Countercurrent Extraction and supercritical carbon dioxide extracting nicotine group technology |
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| CN110437203A (en) * | 2019-07-15 | 2019-11-12 | 湖南鑫文天生物科技有限公司 | Scale Continuous Countercurrent Extraction and supercritical carbon dioxide extracting nicotine group technology |
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