CN100413858C - Method for producing high pure tea polyphenol with low caffeine - Google Patents
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- CN100413858C CN100413858C CNB2004100524041A CN200410052404A CN100413858C CN 100413858 C CN100413858 C CN 100413858C CN B2004100524041 A CNB2004100524041 A CN B2004100524041A CN 200410052404 A CN200410052404 A CN 200410052404A CN 100413858 C CN100413858 C CN 100413858C
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Abstract
The present invention discloses a method for producing high pure tea polyphenol, which comprises the working procedures: the leaching of tea leaves, ultrahigh-speed centrifugation of leaching liquid, ultrafiltration and purification of centrifugate, the adsorption of ultrafiltrate macroporous resin, the graded elution and separation of caffeine and tea polyphenol, and the sodium filtration or the reverse osmosis condensation of tea polyphenol eluent. After the tea polyphenol concentrated liquid is sprayed and dried, the high pure tea polyphenol is obtained. The method has the characteristics that in the production process of the tea polyphenol, organic solvent, such as chloroform, ethyl acetate, etc., is not used; the condensation of tea polyphenol extract does not need depressurization, condensation, etc. (which are frequently used). The method can not only avoid the residue of the organic solvent, but also save energy, increase the degree of production automation, greatly reduce the production cost of the tea polyphenol, and increase the quality and the safety of the products. The tea polyphenol produced by the method has the efficiency of resisting oxidation, aging, etc. Accordingly, the method is particularly suitable for the production of foods, beverages, health products and daily chemicals.
Description
Technical field
The present invention relates to a kind of production method of natural organic-compound, particularly relate to a kind of production method of high-purity tea polyphenol, it belongs to the deep processing field of biochemical industry and agricultural-food.
Background technology
Tea-polyphenol is the many alkyl phenolic substance that is rich in the green tea, main ingredient is poly-flavanol compound, it is made up of about six kinds monomer, be D, L-catechin (D, L-G), L-l-Epicatechol (L-EC), L-epigallocatechin (L-EGC), D, L-l-Epigallocatechol (D, L-GC), L-table catechu tea-polyphenol is the many alkyl phenolic substance that is rich in the tealeaves, and main ingredient is poly-flavanol compound, and it is made up of about six kinds monomer, be D, L-catechin (D, L-G), L-l-Epicatechol (L-EC), L-epigallocatechin (L--EGC), D, L-l-Epigallocatechol (D, L-GC), the L-l-Epicatechol is not eaten ester acid esters (L-ECG), L----NVP-XAA 723 (L-EGCG), wherein, most of ester catechin that belongs to.Catechin is not only the main body chemical substance that constitutes the tealeaves color, and have many-sided effects such as radical in anti-oxidant, the retention mass, reducing blood-fat, anti-ageing, radioprotective, fat-reducing, anti-cancer, sterilization anti-inflammatory, anti-dental caries, deodorizing, be with a wide range of applications in fields such as food, medicine, daily use chemicals and greases.In recent years, both at home and abroad, particularly China and Japan were to exploring new tea-polyphenol extraction and separation process growing interest.Except that traditional method, developed some again and new must get isolation technique, as supercritical extraction (SFE), high speed adverse current chromatogram partition method (HSCCC) etc.
Method that conclude to extract tea-polyphenol generally was divided into for two steps: at first from tea not extraction contain the tea-polyphenol crude product solution of caffeine; Separate then concentrate, purify the high-content tea-polyphenol.
The extraction process of tea-polyphenol is divided into four types in the tealeaves.
1) solvent extration:
This is at present domesticly to make that its patent of one of method is also a lot of the most widely, has left more than ten kind of solvent extration.This ratio juris is to utilize the dissolubility difference of tea-polyphenol in different solvents to carry out extraction separation, and its operational path is as follows: tea raw material, and---solvent extraction---is filtered---decon------separation---spraying drying---tea-polyphenol crude product of extraction mutually.The solvent that extraction is used has water, ethanol, methyl alcohol, acetone, ethyl acetate etc.,, adopt refluxing extraction more, there are Fujian big Fujian food and Jiangxi Lv Kang two enterprises to adopt countercurrent extraction.Impurity elimination commonly used is that method has chloroform decaffeinated, decolorizing with activated carbon, sherwood oil depigmentation or passes through stand at low temperature decon, chlorophyll, polysaccharide etc.; The choice solvent of extraction is an ethyl acetate, and tea-polyphenol is separated from aqueous phase.
Solvent extration extracts tea-polyphenol and remains many having much room for improvement and perfect link as can be seen, mainly is a metallization processes, reduces cost and improve effective component content and extraction yield.
2) precipitator method:
This method is another method comparatively commonly used, the beanstalk principle is to utilize tea-polyphenol can form complex compound and sedimentary character with the metal ion in some mineral alkali, the salt under certain condition, separate with components such as caffeine in the water solvent, monose, amino acid, tea-polyphenol is extracted in enrichment.Its operational path is as follows:
Tea raw material → boiling water extraction → filtration → precipitation → commentaries on classics is molten → extraction → concentrate → drying → tea-polyphenol finished product.
This method need not be used a large amount of organic solvents, and as toxic substances such as chloroforms, cost is low.But different have a weak point, needs strict controlling acidity when changeing molten as precipitation, and the pH value not only influences the solubleness of tea-polyphenol complex precipitate, also influences the stability of tea-polyphenol.The fluctuation of pH value very easily causes the oxidation of polyphenols to destroy greatly, and finished color is deepened.
3) adsorpting column chromatogram method:
This method mainly be utilize sorbent material and eluent adsorb → desorb makes catechin and other separating substances in the tealeaves vat liquor.General technology route tealeaves → hot water lixiviate → filtration → adsorption-desorption---concentrates---spraying drying---tea-polyphenol finished product.The boiling water vat liquor of a usefulness tealeaves is crossed the MC adsorption column of pH=2 in the bamboo tail, then with behind 70% the alcohol desorption, concentrates, vacuum-drying, obtains purity and be 68% catechin.
Macroporous adsorbent resin is the novel non-ionic type molecular adsorbent of a class, has shown the centrifugation of its uniqueness, and existing reporting for work is applied to the extraction separation of tea-polyphenol.This method is to utilize the molecular sieve and the adsorption property of polymeric adsorbent, and catechin is adsorbed on polymeric adsorbent---desorb and other separating substances, and reach the separation and purification purpose.Its key is to select a kind of loading capacity big, is easy to the polymeric adsorbent of desorb again, and the nonpolar macroporous adsorption resin effect of reporting for work at present is better.This domestic series products is a lot, and 92-2 and 92-3 polymeric adsorbent fully can the substituting import one products, as the Amberlite XAD of the U.S. and the Kiaion HP series of Japan etc.Adsorption resin method is easy and simple to handle, and resin is also renewable to be used repeatedly, and stability is high, and cost is low, just progressively moves towards the industrialization.Through examination, this method is applied in the tea-polyphenol production of violent hole, Guzhang, Hunan river vegetable products company limited.
4) supercritical carbon dioxide extraction method:
Supercritical extraction (SFE) is a kind of new separation technology that developed recently gets up.It utilizes the fluid under the supercritical state to make solvent, extracts under the zone that exceeds critical temperature and pressure, uses supercritical carbon dioxide fluid as the more apparent advantage of solvent.Because the threshold value of carbonic acid gas is low, pressure all can cause the amplitude change of fluid density with a less variation with temperature, and very easily is penetrated in the raw material matrix, makes extracted component fully dissolving by distributing diffusion, thereby reaches the purpose of extraction.
Domestic existing research report with SFE method extraction tea-polyphenol.This method has been selected the temperature and pressure condition of 80 degree Celsius and 21Mpa, directly extracts tea-polyphenol with SFE from tealeaves, and purity is 95.45%, but extraction efficiency is not high.Therefore, with SFE directly from tealeaves the extraction tea-polyphenol in industrial production and inadvisable.But the caffeine that can utilize the CO2SFE method to remove in the tea-polyphenol is feasible.
Although it is many to produce the technology of tea-polyphenol both at home and abroad, the technology of macroporous resin adsorption separating tea multi-phenol also begins to be used for industrial production.But, also there is following defective:
1, green tea extractive liquor contains more impurity without (surpassing) high speed centrifugation and uf processing, causes the efficient of macroporous resin adsorption not high, and the product purity of production is not enough.
2, the macroporous resin model of selecting for use is not ideal enough, and not high enough to the selectivity of tea-polyphenol absorption, tea-polyphenol is thorough inadequately with separating of caffeine, causes catechin content (about 75%) on the low side in the product, content of caffeine higher (about 0.5%).
3, liquid concentration often adopts concentrating under reduced pressure or scraper plate to concentrate energy consumption height in the production process.
Summary of the invention
The objective of the invention is to develop the production method of a kind of quality product height, safer, lower-cost high-purity tea polyphenol.
For achieving the above object, technical solution of the present invention is:
The present invention is after the extraction and separation method of the character of green tea composition and tea-polyphenol, caffeine is furtherd investigate, and realizes by following operational path and processing condition:
1, operational path:
Green tea → lixiviate coarse filtration → high speed centrifugation → ultrafiltration → macroporous resin adsorption → desorb → nanofiltration concentrates → distillation → spraying drying packing → tea-polyphenol finished product
2, operation steps and processing condition:
2.1 starting material are selected
The main raw material of producing tea-polyphenol is green tea or green tea end, should be from sense index, physical and chemical index and the strict control in three aspects of sanitary index raw materials quality.Particularly want pesticide residue and heavy metal content in the strict control sanitary index, in the middle of just can not be when having an index defective as raw materials for production.When the buying raw material, emphasis to detect the following index of control:
(1), sense index: color, smell and taste are normal, nothing is gone mouldy.The material 〉=40 orders
(2) physical and chemical index:
I, polyphenol content 〉=18%
Ii, catechin total amount 〉=10%
iii、EGCG≥6％
Iv, moisture content≤8%
(3) sanitary index:
I, pesticide residue (mgmg/kgkg)≤10
Ii, heavy metal (mgmg/kgkg)≤20
2.2 lixiviate coarse filtration
Raw material is measured in the extraction equipment of pack into band heating and whipping appts, add the pure water of raw material 9-10 times weight for the first time, be heated to 75-85 ℃, stir (rotating speed 15r/min) extraction 35min, carry out the second time after the filtration and extract.Extract the pure water that adds the heavy 5-6 times of weight of raw material for the second time, be heated to 75-85 ℃, stir and extract 35min, filter.Twice filtrate is cooled to 35-40 ℃ through heat exchange, goes into extracting solution basin (survey solid content).
2.3 high speed centrifugation
Extracting solution is pumped into tubular-bowl centrifuge continuously centrifuged under 10000-12000r/min separate, get clarifying green tea extractive liquor, go into clear liquor basin (survey solid content).Its objective is the suspended substance of removing extracting solution, reduce pollution and the increase membrane flux of impurity ultra-filtration membrane.
2.4 ultrafiltration
Centrifugal green tea clear liquor pumped into carries out ultrafiltration in the ultrafiltration apparatus, remove tea polysaccharide, pectin or the like impurity (in existing fractionation by adsorption tea-polyphenol technology green tea extractive liquor without the ultrafiltration impurity elimination, thereby cause: 1, the purity of product is lower; 2, impurity is bigger to the pollution of resin), ultrafiltrated is gone into jar.The ultra-filtration membrane of selecting for use is the polyvinylidene fluoride film of molecular weight cut-off 40000-50000, (as flat sheet membrane such as UF605-2, the UF610 of the U.S. and suntar2272 rolled film etc.).The ultrafiltration technology condition is: room temperature to 40 ℃, entrance pressure 4-6bar goes out to press 1bar.The ultrafiltrated yield is 92.5-95.5%.
2.5 macroporous resin adsorption
The green tea extractive liquor of ultrafiltration impurity elimination is used macroporous resin adsorption at normal temperatures and pressures.The macroporous resin of selecting for use is polystyrene copolymerization body or polyethylene interpolymer, and its aperture is 32-
Specific surface area 400-650m
2/ g.Flow velocity is decided on post height, post footpath.
2.6 desorb
With the macroporous resin that is adsorbed with tea-polyphenol and caffeine under normal temperature and pressure conditions, earlier with the 35-45% neutral alcohol take off wash no caffeine after, use alkaline ethanol (with ammoniacal liquor accent PH=8-8.5) the wash-out tea-polyphenol of 65-70% instead, take off washing lotion and store in the basin.The utilization macroreticular resin absorbing method separates caffeine and tea-polyphenol, and separates caffeine and tea-polyphenol without chloroform, ethyl acetate extraction, has both avoided the pollution of organic solvents such as chloroform, ethyl acetate, has reduced cost again.
2.7 nanofiltration (or reverse osmosis) concentrates
The tea-polyphenol elutriant pumped at normal temperatures and pressures carry out nanofiltration (or reverse osmosis) in nanofiltration (or reverse osmosis) equipment and concentrate, its processing condition are: entrance pressure 32-35bar goes out to press 30bar.Cycles of concentration is 6-7 times, and concentrated solution content is 7.5-8%.The nanofiltration of selecting for use (or reverse osmosis) film is a polyethers phenol composite membrane.And need not currently adopt concentrating under reduced pressure both at home and abroad more, and can save the energy in a large number, reduce cost.
2.8 distillation
The nanofiltration concentrated solution of tea-polyphenol is pumped in the distillation axe, heats up, 78-79 ℃ down distillation reclaim ethanol, the tea-polyphenol concentrated solution of solid content 25-30%.Its objective is the residual ethanol after the further recovery nanofiltration.
2.9 spraying drying
The tea-polyphenol concentrated solution of distillation gained is got tea-polyphenol through centrifugal spray drying.Its processing condition are: inlet temperature 145-220 ℃, air outlet temperature 70-85 ℃, time of drying 30s.
2.10 packing
With the tea-polyphenol of spraying drying gained through mix, sieve, product examine qualified after, by packing instructions pack the tea-polyphenol finished product.
After adopting such scheme, because present method uses ethanol as elutriant wash-out tea-polyphenol in the production process of tea-polyphenol, and do not use organic solvents such as chloroform, ethyl acetate, the tea-polyphenol extracting solution concentrates characteristics such as need not (using) concentrating under reduced pressure always, both avoid organic solvent residual, saved energy consumption again, improved production automation degree, greatly reduce the production cost of tea-polyphenol, improved the quality and the security of product.The purity of the tea-polyphenol that present method is produced is greater than 98%, and wherein catechin is greater than 90%, and caffeine is less than 0.1%, and the product yield is greater than 10%.Many-sided effects such as that the product that the present invention produces has is anti-oxidant, anti-ageing, reducing blood-fat, fat-reducing, anti-cancer, sterilization anti-inflammatory are specially adapted to the production of food, beverage, healthcare products, household chemicals.
Embodiment
Embodiment 1:
The present invention adopts low-grade green tea or green tea end for the production method of the high-purity tea polyphenol of raw material, comprises the steps:
1, starting material are selected:
The main raw material of producing tea-polyphenol is green tea or green tea end, should be from sense index, physical and chemical index and the strict control in three aspects of sanitary index raw materials quality.Particularly want pesticide residue and heavy metal content in the strict control sanitary index, in the middle of just can not be when having an index defective as raw materials for production.
2, lixiviate coarse filtration:
With 200kg green tea pack into (the multipotency extractor of 3000L) in the extraction equipment of band heating and whipping appts, the pure water that adds for the first time 1900kg, close charging opening, start and stir, the breakdown steam valve, be heated to 75-85 ℃, stir (rotating speed 15r/min) and extract 35min, carry out the second time after the filtration and extract.Extract the pure water that adds 1000kg for the second time, be heated to 75 ℃, stir and extract 35min, filter.Twice filtrate is cooled to 35 ℃ through heat exchange, goes into the extracting solution basin (surveying solid content 〉=1.2%) of 4000L.
3, high speed centrifugation:
With extracting solution at normal temperatures and pressures, pump into tubular-bowl centrifuge continuously centrifuged under 10000r/min by the flow velocity of 33L/min and separate, clarifying green tea extractive liquor, go into the clear liquor basin of 4000L.
4, ultrafiltration:
Centrifugal green tea clear liquor is gone into to carry out ultrafiltration in the ultrafiltration equipment by the flow pump of 33L/min, remove tea polysaccharide, pectin or the like impurity, ultrafiltrated is gone into the 4000L basin.The ultra-filtration membrane of selecting for use is molecular weight cut-off 40000 vinylidene fluoride films, (as flat sheet membrane such as UF605-2, the UF610 of the U.S. and suntar2272 rolled film etc.).The ultrafiltration technology condition is: room temperature, entrance pressure 6bar goes out to press 1bar.The exit velocity of ultrafiltrated is 30L/min.
5, macroporous resin adsorption:
At normal temperatures and pressures, the green tea extractive liquor of the ultrafiltration impurity elimination flow velocity by 30L/min is pumped in the high level tank of macroporous resin adsorption tower.Breakdown and adjusting feed valve, the flow velocity that the green tea extractive liquor of macroporous resin adsorption tower is advanced in control is 30L/min.The macroporous resin of selecting for use is polystyrene copolymerization body or polyethylene interpolymer, its mean pore size is 〉=
Specific surface area 〉=400m
2/ g.Macroporous resin adsorption tower height 3m, tower diameter 350mm.
6, desorb:
To be adsorbed with the macroporous resin of tea-polyphenol and caffeine under normal temperature and pressure conditions, take off with 35% neutral alcohol earlier and wash (flow velocity 15L/min) after the no caffeine of detection, using 65% alkaline ethanol (transferring PH=8 with ammoniacal liquor) instead is 13L/min wash-out tea-polyphenol with the flow velocity, takes off washing lotion and stores in the basin.
7, nanofiltration (or reverse osmosis) concentrates:
At normal temperatures and pressures, the tea-polyphenol elutriant is pumped into the flow velocity of 13L/min carry out nanofiltration in the tubular type nanofiltration equipment and concentrate.Its processing condition are: entrance pressure 35bar goes out to press 30bar.The concentrated solution take-off rate is 2.2L/min, and the concentrated solution solid content is 7.5%.The nanofiltration of selecting for use (or reverse osmosis) film is the polyamide (PA) composite membrane, and molecular weight cut-off is 200.
8, distillation:
The nanofiltration concentrated solution 300L of tea-polyphenol is pumped in the distillation axe of 700L (ZQN700 type), heat up, distill down at 78 ℃ and reclaim ethanol, get the tea-polyphenol concentrated solution 96L of solid content 25%.
9, spraying drying:
The 96L tea-polyphenol concentrated solution of distillation gained is got tea-polyphenol 20.85kg through LPG-100 type centrifugal spray drying, and yield is 10.4%.Its processing condition are: 145 ℃ of inlet temperature, 70 ℃ of air outlet temperatures, time of drying 30s.
10, packing:
With the 20.85kg tea-polyphenol of spraying drying gained through mix, sieve, inspection by sampling, the content of tea-polyphenol is 99.2%, the content of catechin is 91%, EGCG content is 73%, moisture content≤3%, and coffee is because 0.07%, pesticide residue do not detect, heavy metal≤2PPM, and quality product is qualified.By packing instructions pack the tea-polyphenol finished product.
Embodiment 2:
1, starting material are selected identical with embodiment 1.
2, lixiviate coarse filtration:
200kg green tea is packed into (the multipotency extractor of 3000L) in the extraction equipment of band heating and whipping appts, and add the pure water of 1800kg the first time, closes charging opening, start and stir, the breakdown steam valve is heated to 85 ℃, stir (rotating speed 15r/min) and extract 35min, carry out the second time after the filtration and extract.Extract the pure water of adding 1000 for the second time, be heated to 85 ℃, stir and extract 35min, filter.Twice filtrate is cooled to 40 ℃ through heat exchange, goes into the extracting solution basin (surveying solid content=1.4%) of 4000L.
3, high speed centrifugation:
With extracting solution at normal temperatures and pressures, pump into tubular-bowl centrifuge continuously centrifuged under 12000r/min by the flow velocity of 35L/min and separate, clarifying green tea extractive liquor, go into the clear liquor basin of 4000L.
4, ultrafiltration:
Centrifugal green tea clear liquor is gone into to carry out ultrafiltration in the ultrafiltration equipment by the flow pump of 35L/min, remove tea polysaccharide, pectin or the like impurity, ultrafiltrated is gone into the 4000L basin.The ultra-filtration membrane of selecting for use is the polyvinylidene fluoride film of molecular weight cut-off 60000.The ultrafiltration technology condition is: room temperature, entrance pressure 6bar goes out to press 1bar.The exit velocity of ultrafiltrated is 33L/min.
5, macroporous resin adsorption:
At normal temperatures and pressures, the green tea extractive liquor of the ultrafiltration impurity elimination flow velocity by 33L/min is pumped in the high level tank of macroporous resin adsorption tower.Breakdown and adjusting feed valve, the flow velocity that the green tea extractive liquor of macroporous resin adsorption tower is advanced in control is 33L/min.The macroporous resin of selecting for use is polystyrene copolymerization body or polyethylene interpolymer, and its mean pore size is
Specific surface area 650m
2/ g.Macroporous resin adsorption tower height 4m, tower diameter 350mm.
6, desorb:
To be adsorbed with the macroporous resin of tea-polyphenol and caffeine under normal temperature and pressure conditions, take off with 40% neutral alcohol earlier and wash (flow velocity 15L/min) after the no caffeine of detection, using 70% alkaline ethanol (transferring PH=8.5 with ammoniacal liquor) instead is 15L/min wash-out tea-polyphenol with the flow velocity, takes off washing lotion and stores in the basin.
7, nanofiltration (or reverse osmosis) concentrates:
At normal temperatures and pressures, the tea-polyphenol elutriant is pumped into the flow velocity of 15L/min carry out nanofiltration in the tubular type nanofiltration equipment and concentrate.Its processing condition are: entrance pressure 35bar goes out to press 30bar.The concentrated solution take-off rate is 2.5L/min, and the concentrated solution solid content is 8%.The nanofiltration of selecting for use (or reverse osmosis) film is the polyamide (PA) composite membrane, and molecular weight cut-off is 200.
8, distillation:
The nanofiltration concentrated solution 300L of tea-polyphenol is pumped in the distillation axe of 700L (ZQN700 type), heat up, distill down at 79 ℃ and reclaim ethanol, get the tea-polyphenol concentrated solution 96L of solid content 30%.
9, spraying drying:
The 96L tea-polyphenol concentrated solution of distillation gained is got tea-polyphenol 20.85kg through LPG-100 type centrifugal spray drying, and yield is 10.4%.Its processing condition are: 220 ℃ of inlet temperature, 85 ℃ of air outlet temperatures, time of drying 30s.
10, packing is identical with embodiment 1
Embodiment 3:
1, starting material are identical with embodiment 1.
2, lixiviate coarse filtration:
200 green tea are packed in the extraction equipment of band heating and whipping appts, add 2000 pure water for the first time, close charging opening, start and stir, the breakdown steam valve is heated to 70 ℃, stirs (rotating speed 15r/min) and extracts 35min, carries out the extraction second time after the filtration.Extract the pure water that adds 1200kg for the second time, be heated to 80 ℃, stir and extract 35min, filter.Twice filtrate is cooled to 38 ℃ through heat exchange, goes into the extracting solution basin (surveying solid content=1.35) of 4000L.
3, high speed centrifugation:
With extracting solution at normal temperatures and pressures, pump into tubular-bowl centrifuge continuously centrifuged under 13000r/min by the flow velocity of 34L/min and separate, clarifying green tea extractive liquor, go into the clear liquor basin of 4000L.
4, ultrafiltration:
Centrifugal green tea clear liquor is gone into to carry out ultrafiltration in the ultrafiltration equipment by the flow pump of 34L/min, remove tea polysaccharide, pectin or the like impurity, ultrafiltrated is gone into the 4000L basin.The ultra-filtration membrane of selecting for use is the polyvinylidene fluoride film of molecular weight cut-off 50000.The ultrafiltration technology condition is: room temperature, entrance pressure 6bar goes out to press 1bar.The exit velocity of ultrafiltrated is 32L/min.
5, macroporous resin adsorption:
At normal temperatures and pressures, the green tea extractive liquor of the ultrafiltration impurity elimination flow velocity by 34L/min is pumped in the high level tank of macroporous resin adsorption tower.Breakdown and adjusting feed valve, the flow velocity that the green tea extractive liquor of macroporous resin adsorption tower is advanced in control is 34L/min.The macroporous resin of selecting for use is polystyrene copolymerization body or polyethylene interpolymer, and its mean pore size is
Specific surface area 500m
2/ g.Macroporous resin adsorption tower height 3.5m, tower diameter 350mm.
6, desorb:
To be adsorbed with the macroporous resin of tea-polyphenol and caffeine under normal temperature and pressure conditions, take off with 45% neutral alcohol earlier and wash (flow velocity 15L/min) after the no caffeine of detection, using 68% alkaline ethanol (transferring PH=8.2 with ammoniacal liquor) instead is 14L/min wash-out tea-polyphenol with the flow velocity, takes off washing lotion and stores in the basin.
7, nanofiltration (or reverse osmosis) concentrates:
At normal temperatures and pressures, the tea-polyphenol elutriant is pumped into the flow velocity of 14L/min carry out nanofiltration in the tubular type nanofiltration equipment and concentrate.Its processing condition are: entrance pressure 35bar goes out to press 30bar.The concentrated solution take-off rate is 2.4L/min, and the concentrated solution solid content is 7.8%.
8, distillation:
The nanofiltration concentrated solution 300L of tea-polyphenol is pumped in the distillation axe of 700L (ZQN700 type), heat up, distill down at 78 ℃ and reclaim ethanol, get the tea-polyphenol concentrated solution 96L of solid content 28%.
9, spraying drying:
The 96L tea-polyphenol concentrated solution of distillation gained is got tea-polyphenol 20.85kg through centrifugal spray drying, and yield is 10.4%.Its processing condition are: 200 ℃ of inlet temperature, 78 ℃ of air outlet temperatures, time of drying 30s.
10, packing is identical with embodiment.
Claims (3)
1. the production method of the high-purity tea polyphenol of a low-caffeine, comprise the steps: that (1) pack green tea metering in the extraction equipment of band heating and whipping appts into, add the pure water of raw material 9-10 times weight the first time, is heated to 75-85 ℃, stir and extract 35min, carry out the second time after the filtration and extract, extract the pure water that adds 5-6 times of weight of raw material for the second time, be heated to 75-85 ℃, stir and extract 35min, filter extracting solution, twice filtrate is cooled to 35-40 ℃ through heat exchange, goes into the extracting solution basin; (2) extracting solution is centrifugal through tubular-bowl centrifuge is that the ultra-filtration membrane ultrafiltration of 30000-50000 removes impurity such as tea polysaccharide, pectin with molecular weight cut-off after continuously centrifuged under the 10000-12000r/min separates, and obtains clarifying green tea clear liquor; (3) the clear liquor via hole diameter is
Specific surface area 400-650m
2/ g polystyrene copolymerization body or polyethylene interpolymer macroporous resin are from handing over bed Adsorption of Tea Polyphenols and caffeine; (4) resin that will be adsorbed with tea-polyphenol and caffeine carries out the classification wash-out; (5) the tea-polyphenol elutriant concentrates or reverse osmosis concentration through the polyamide composite film nanofiltration of molecular weight cut-off 200, gets the tea-polyphenol concentrated solution, and concentrated solution reclaims ethanol through distillation, makes its solid content be increased to solid content more than 25%; (6) the concentrated solution spraying drying get content of caffeine less than 0.01%, polyphenol content greater than 98%, catechin content is greater than 90% tea-polyphenol.
2. the production method of the high-purity tea polyphenol of low-caffeine according to claim 1, it is characterized in that: the ultra-filtration membrane that the ultrafiltration of step (2) is selected for use is a polyvinylidene fluoride (PVDF) ultrafiltration membrane.
3. the production method of the high-purity tea polyphenol of low-caffeine according to claim 1, it is characterized in that: it is under normal temperature and pressure conditions that the described resin that will be adsorbed with tea-polyphenol and caffeine of step (4) carries out the classification wash-out, earlier with the 35-45% neutral alcohol take off wash no caffeine after, the pH value of using 60-80% instead is a 8-8.5 alkaline ethanol wash-out tea-polyphenol.
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