CN102863476A - Method for preparing tea polyphenols with rotating disc tower countercurrent extractor - Google Patents
Method for preparing tea polyphenols with rotating disc tower countercurrent extractor Download PDFInfo
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Abstract
The invention discloses a method for preparing tea polyphenols with a rotating disc tower countercurrent extractor. The method comprises the following steps: removing the impurities out of tea, leaching tea with a mixture of water and alcohol to obtain tea polyphenol leach liquor, performing rotary evaporation to remove the alcohol out of the leach liquor to obtain a tea polyphenol concentrated solution, diluting the concentrated solution with a buffer solution to obtain tea polyphenol dope; pumping the tea polyphenol dope used as the raw material and an extractant into an extraction tower in a countercurrent mode to complete the extraction process, wherein the heavy phase stands still at the tower bottom and the light phase stands still at the tower top at the end; with a buffer solution as the back-extractant, pumping the extract phase and the back-extractant into a back extraction tower in the countercurrent mode, wherein two-phase fluids fully contact with each other under the rotation of the rotating disc and the back extraction process is completed; performing vacuum drying on the back extraction phase separated by the back extraction tower to obtain pure tea polyphenols; and separating to obtain the back raffinate phase which can be used as an extractant for cyclic utilization after rinsing or rotary evaporation. By adopting the method for preparing tea polyphenols with the rotating disc tower countercurrent extractor, the continuous mass production of tea polyphenols can be realized and the high-value utilization of the low-value tea can also be realized.
Description
Technical field
The present invention relates to a kind of chemical separating method, be specifically related to a kind of method of utilizing the rotating disc contactor countercurrent extraction device to prepare tea-polyphenol.
Background technology
Tea-polyphenol is the general name of Polyphenols in the tealeaves, mainly is comprised of flavanol compound, anthocyan, anthoxanthins, carboxylic acid and carboxylic phenolic acids.That tea-polyphenol has is anti-oxidant, antibiotic, anticancer, eliminate the biological activity such as free radical, and the diseases such as cardiovascular disorder, tumour are had preferably preventive and therapeutic action, has been widely used in the industries such as food, medicine, light industry and chemical industry.Scale is used in continuous expansion in the market of tea-polyphenol, shows according to " Chinese food newspaper ", and be about 2000 tons to the demand of tea-polyphenol both at home and abroad, its market scale can reach tens00000000 yuan.The raw materials for production of tealeaves are mainly tender leaf and the bud of tea tree in spring since ancient times, but the tealeaves except tender leaf is not fully utilized.In addition, the summer autumn tea is because nutritive value is lower than spring tea, and taste is pained, causes the market utilization ratio of summer autumn tea very low.These tealeaves all are referred to as " low value tealeaves ".According to statistics, have approximately in China's tea yield at present 70% be low value tealeaves, do not obtain utilizing.In addition, tea-enterprise has 2%～4% by product approximately in the Tea Processing process also be low value tealeaves, obtains utilizing at all.Therefore, utilize these low value tealeaves to produce tea-polyphenol for raw material, on the one hand so that the low value tea resources obtains adequately and reasonably high-valuedly, also improved on the other hand the output of tea-polyphenol to satisfy the growing market requirement.
About the extraction of tea-polyphenol, a large amount of papers and patent report have been arranged both at home and abroad.Domestic disclosed production tea-polyphenol patent mainly comprises following methods: patent CN1386731A and discloses a kind of processing method of extracting tea-polyphenol, mainly is to adsorb impurity with acetone, uses organic solvent extraction again, obtains the method for tea-polyphenol crude product finally by drying; Patent CN1104621A discloses a kind of extraction of theophenol---and the ion precipitation method, the mixed precipitant that forms with the muriate such as Ca, Mg and oxyhydroxide first makes the tea-polyphenol Precipitation, re-uses HCl and H
2SO
4Turn molten precipitation agent and realize obtaining the tea-polyphenol crude product finally by extraction, drying separating of tea-polyphenol and precipitation agent Deng answering of consisting of of acid solvent; Patent CN1253940A discloses a kind of method for preparing tea-polyphenol from tealeaves, first with ethanol or hot water lixiviate, and the concentrated and CO through ethyl acetate extraction
2Supercritical extraction obtains the tea-polyphenol powder; Patent CN1546485A discloses a kind of separation method of tea-polyphenol mixture, mainly is to utilize resin absorption, and then the separation method of wash-out.External disclosed production polyphenols patent has following several method: patent JP63158453 to disclose a kind of production method of polyphenols, starting material are stem or the unleavened tealeaves of tealeaves or the tea tree that does, first with organic solvent or hot water lixiviate starting material, the ultrafiltration vat liquor, obtain containing again the powder of 30% polyphenols through concentrate drying, the purity of the tea-polyphenol that with sorbent material or activated carbon treatment powder is at last is improved; Patent US4,396,757 disclose a kind of production method of polyphenol, mainly are to produce polyphenol by oxypolymerization phenol; Patent US7,820,866B2 disclose a kind of production process of polyphenol, and starting material are polyphenol complex, such as bis-phenol, produce tea-polyphenol by enzyme-catalyzed change.
Above-mentioned domestic and international extracting method about tea-polyphenol can be summarized as following Four types: solvent-extraction process, ion precipitation method, carbon dioxide supercritical extraction method and post partition method, wherein ion precipitation method extraction tea-polyphenol step is more loaded down with trivial details, need through precipitation, dissolving, extraction and dry four programs, and in the product of preparation a large amount of heavy-metal residuals is arranged; The tea-polyphenol purity of post partition method preparation is higher, however need a large amount of eluents so that, production cost is high; The carbon dioxide supercritical extraction method advanced technology, however cost of investment is high, and the tea-polyphenol of production is ' gram magnitude '.External also have this method of oxypolymerization phenol production polyphenol, yet this is inconsistent with original intention of the present invention.Therefore the preparation method of above-mentioned tea-polyphenol all has its limitation separately, in the urgent need to developing a kind of good operation performance, job costs are low, product purity is high tea-polyphenol novel preparation method.
Although disclose the solvent extraction process of a large amount of tea-polyphenol, the report that utilizes the rotating disc contactor countercurrent extraction device to prepare the tea-polyphenol related process never arranged.This patent utilizes the solvent extraction principle, uses homemade rotating disc contactor continuous countercurrent extraction device, sets up the novel process of a cover efficient preparation tea-polyphenol from low value tealeaves, for the industrial production of tea-polyphenol provides a kind of practicable method.
Summary of the invention
The technical problem that solves: the present invention is directed to above technical problem, a kind of method of utilizing the rotating disc contactor countercurrent extraction device to prepare tea-polyphenol is provided, and this technique is that the solvent extration of tea-polyphenol and rotating disc contactor countercurrent extraction device are combined in an a kind of method of producing continuously tea-polyphenol.The method can realize the serialization scale operation of tea-polyphenol, can realize the higher value application of low value tealeaves.
Technical scheme: utilize the rotating disc contactor countercurrent extraction device to prepare the method for tea-polyphenol, described rotating disc contactor countercurrent extraction device comprises extraction tower and stripping column, described extraction tower is identical with the stripping column structure, be provided with successively motor from top to bottom, on the section of leaving standstill, the body of the tower section, under the section of leaving standstill, the section of leaving standstill top is provided with the top discharge mouth on described, the bottom is provided with charging opening, described body of the tower section is coated with the recirculated water chuck, the section of leaving standstill top is provided with lower charging opening under described, the bottom is provided with lower discharge port, on the section of leaving standstill with under be equipped with glass spring in the section of leaving standstill, motor is provided with rotating shaft, described rotating shaft by on the section of leaving standstill be through to the body of the tower section, the rotating shaft in the body of the tower section is provided with rotating disk; Charging opening links to each other with the first storage tank on the extraction tower, extraction tower top discharge mouth links to each other with the second storage tank, charging opening links to each other with the second storage tank under the extraction tower, the extraction tower lower discharge port links to each other with charging opening on the stripping column, charging opening links to each other with the 3rd storage tank under the stripping column, the stripping column lower discharge port links to each other with the 4th storage tank, stripping column top discharge mouth links to each other with the 5th storage tank, it is characterized in that comprising the steps: that a. removes impurity with tealeaves, the water-alcohol mixture that with volume ratio is 5: 1～3: 1 obtains the tea-polyphenol vat liquor at 60～90 ℃ of lower lixiviate 0.5～1.5h, and then the alcohol that rotary evaporation is removed in the vat liquor obtains the tea-polyphenol concentrated solution, and with pH damping fluid dilution concentrated solution between 1～6, obtain concentration between 8～15g/L, the tea-polyphenol stoste of pH between 1～6; B. take tea-polyphenol stoste as raw material, take propyl carbinol, vanay, ethyl acetate, butylacetate or primary isoamyl alcohol as extraction agent, 2: 1 by volume～1: 2 with stoste and extraction agent respectively adverse current pump in the extraction tower, what relative density was little is entered by column bottoms pump, what relative density was large is pumped into by cat head, and two-phase liquid is fully contact under the rotation of rotating disk, finishes extraction process, last heavy phase leaves standstill at the bottom of tower, gently leaves standstill at cat head; C. take the damping fluid of pH as 4～12 as strippant, 2: 1 by volume～1: 2 with extraction phase and strippant respectively adverse current pump in the stripping column, what relative density was little among both is entered by column bottoms pump, what relative density was large is pumped into by cat head, two-phase liquid is fully contact under dial rotation, finishes the back extraction process, and last heavy phase leaves standstill at the bottom of tower, gently leave standstill at cat head, whole process extraction phase is continuous extraction and the operation 0.5～5h that strips in two rotating disc contactors; D. after stripping column separated, stripping obtained the tea-polyphenol sterling after vacuum-drying; E. separate the anti-extracting phase that obtains, can be as the extraction agent recycle behind washing or rotary evaporation.
The described starting material that are used for cooking vat liquor are tealeaves, and the pH of tea-polyphenol stoste is between 2～5, and the pH of strippant is between 4～11.
Extraction process turntable rotating speed is 50～350r/min, and the body of the tower temperature is controlled at 5～50 ℃.
Back extraction process turntable rotating speed is 50～350r/min, and the body of the tower temperature is controlled at 20～90 ℃.
Damping fluid among the described step a is: Repone K-hydrochloride buffer pH 1-2 or Sodium phosphate dibasic-citrate buffer solution pH2-7.
The described rotating disk center of circle is provided with shaft hole, and average mark is furnished with one group of diameter less than the through hole of shaft hole around the shaft hole.
Damping fluid among the described step c is Sodium phosphate dibasic-citrate buffer solution pH 4-7, Tris-hydrochloride buffer pH 8-9 or sodium bicarbonate-sodium hydrate buffer solution pH 10-11.
Extraction phase continuous extraction and the operation 0.5～5h that strips in two towers among the described step c.
Beneficial effect:
1. this technique prepares tea-polyphenol in conjunction with the rotating disc contactor countercurrent extraction device, can serialization production, and simple to operate, production energy consumption is low, can reduce the production cost of enterprise, improves the economic benefit of enterprise.
2. this technique is on starting material are selected, select low value tealeaves as raw material, the utilization ratio of low value tealeaves and the added value of tea place tea tree have been improved on the one hand, increased tea grower's income, enlarged on the other hand tea-polyphenol raw material sources, improved the output of tea-polyphenol, this behave is having important meaning aspect economic benefit and the social benefit two.
3. in the preparation process of tea-polyphenol, do not use any toxic agent, and extraction and back-extraction got be combined in one, quality product has had good assurance, enables to be applied to better each food, medicine, light industry and other relevant industries.
4. only use a kind of organic solvent as extraction agent in the process of production tea-polyphenol, this organic solvent good stability, toxicity is low, effect of extracting is outstanding, through can recycle after the washing, do not pollute the environment when reducing production costs, belong to environmentally friendly technique.
Description of drawings
Fig. 1: the rotating disc contactor countercurrent extraction device prepares the process flow diagram (taking vanay as example as extraction agent) of tea-polyphenol; 1: thermostatical circulating water; 2: upper charging opening; 3: lower charging opening; 4: the top discharge mouth; 5: lower discharge port; 6: electric motor; 7: on the section of leaving standstill; 8: the lower section of leaving standstill; 9: glass spring; 10: rotating shaft; 11: rotating disk; 12 recirculated water chucks; 13: the first storage tanks (vanay storage tank); 14: the second storage tanks (the former liquid storage tank of tea-polyphenol); 15: the three storage tanks (strippant storage tank); 17: the five storage tanks (reextraction phase storage tank) of 16: the four storage tanks (vanay pond for recovering); 18: extraction tower; 19: stripping column; 1 ': the stripping column thermostatical circulating water; 2 ': charging opening on the stripping column; 3 ': charging opening under the stripping column; 4 ': stripping column top discharge mouth; 5 ': the stripping column lower discharge port; 6 ': the stripping column electric motor; 7 ': the section of leaving standstill on the stripping column; 8 ': the section of leaving standstill under the stripping column; 9 ': the stripping column glass spring.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Among the embodiment of the present invention, the tea-polyphenol yield y(% that obtains of extraction) represent, i.e. the ratio of the mass M of tea-polyphenol in the quality m of tea-polyphenol and the tea-polyphenol stoste in the extraction phase, its calculating formula is:
y＝m/M×100％
The tea-polyphenol that back extraction obtains rate of recovery Y(%) expression, namely strip mutually in the ratio of the mass M of tea-polyphenol in the quality n of tea-polyphenol and the tea-polyphenol stoste, its calculating formula is:
Y＝n/M×100％
The detection method of tea-polyphenol: referring to the GB detection method, GB/T 8313-2008.
The technological step of finishing above invention task is: a kind of rotating disc contactor continuous countercurrent extraction is produced the technique of tea-polyphenol, comprises the steps:
1. summer autumn tea (or discarded tealeaves, fresh tea leaf in its, low-grade tea and useless time tea) is removed dust impurity, water and alcohol mixt be the lixiviate appropriate time at a certain temperature, rotary evaporation is removed alcohol, and with the damping fluid of proper acidity or alkalinity concentrated solution is diluted to certain concentration.
2. the screening of extraction agent take useless tealeaves vat liquor as raw material, take 12 kinds of organic solvents commonly used as extraction agent, is investigated respectively the effect of extracting of 12 kinds of organic solvents.
3. take the vat liquor of useless tealeaves as raw material, take propyl carbinol, vanay, ethyl acetate, butylacetate or primary isoamyl alcohol as extraction agent, with a certain proportion of vat liquor and extraction agent respectively adverse current pump in the rotating disc contactor (gently to be entered by column bottoms pump, heavy phase is pumped into by cat head), two-phase liquid is fully contact under the rotation of rotating disk, finish extraction process, wherein heavy phase leaves standstill at the bottom of tower, gently leaves standstill at cat head.
4. take the damping fluid of pH as 4～11 as strippant, with a certain proportion of extraction phase and strippant respectively adverse current pump in another rotating disc contactor (gently to be entered by column bottoms pump, heavy phase is pumped into by cat head), two-phase liquid is fully contact under the rotation of rotating disk, finish the back extraction process, wherein gently leave standstill at cat head, heavy phase leaves standstill at the bottom of tower.
5. after rotating disc contactor separated, the reextraction of leaving standstill at the bottom of cat head or the tower obtained the tea-polyphenol sterling after vacuum-drying.
6. at the bottom of the tower or the anti-extracting phase of cat head, i.e. propyl carbinol, vanay, ethyl acetate, butylacetate, trichloromethane or primary isoamyl alcohol solution can recycles behind washing or rotary evaporation.
Described tea-polyphenol quantity-produced technique is characterized in that used starting material are summer autumn tea (or discarded tealeaves, fresh tea leaf in its, low-grade tea and useless time tea).
Described tea-polyphenol quantity-produced technique is characterized in that the pH of vat liquor between 2～5, and damping fluid is Repone K-hydrochloride buffer (pH 1-2) or Sodium phosphate dibasic-citrate buffer solution (pH 2-7).
Described tea-polyphenol quantity-produced technique is characterized in that described extraction agent is propyl carbinol, vanay, ethyl acetate, butylacetate or primary isoamyl alcohol.
Described tea-polyphenol quantity-produced technique, it is characterized in that the pH of described strippant between 4～11, damping fluid is Sodium phosphate dibasic-citrate buffer solution (pH 4-7) or Tris-hydrochloride buffer (pH 8-9) or sodium bicarbonate-sodium hydrate buffer solution (pH 10-11).
Described tea-polyphenol quantity-produced technique is characterized in that having used the rotating disc contactor countercurrent extraction device in the preparation process of tea-polyphenol.
Described tea-polyphenol quantity-produced technique, the processing parameter of extraction process is: the rotating speed of rotating disc contactor I is controlled between 50～350r/min, and the tower body temperature is controlled between 5～50 ℃.
Described tea-polyphenol quantity-produced technique, the processing parameter of reextraction process is: the rotating speed of rotating disc contactor II is controlled between 50～350r/min, and the tower body temperature is controlled between 20～90 ℃.
The technique of described rotating disc contactor counter-current extraction tea-polyphenol, extraction phase is continuous extraction and the operation 0.5～5h that strips in two rotating disc contactors.
Embodiment 1:
Time tealeaves that will give up is removed dust impurity, obtain the tea-polyphenol vat liquor with 5: 1 water-alcohol mixture of volume ratio at 60 ℃ of lower lixiviate 0.5h, the alcohol that distillation is removed in the vat liquor obtains the tea-polyphenol concentrated solution, and with the Sodium phosphate dibasic of pH=6.0-citrate buffer solution dilution concentrated solution, obtaining concentration is that 8g/L, pH are 5.8 tea-polyphenol stoste.2: 1 by volume with tea-polyphenol stoste (2L) and ethyl acetate (1L) respectively by at the bottom of the tower and the cat head adverse current pump in the extraction tower, the tower body temperature is controlled at 50 ℃, rotary speed is controlled at 50r/min.Extracting phase leaves standstill at the bottom of tower after the balance, and extraction phase leaves standstill at cat head, is introduced into stripping column.By back extraction phase and 2: 1 Tris-hydrochloride buffers (2L) at stripping column adding pH=8.0 of extraction phase volume ratio, the tower body temperature is controlled at 40 ℃, and rotary speed is controlled at 50r/min, and extraction phase leaves standstill at cat head after the balance, and back extraction is left standstill at the bottom of tower.Whole process extraction phase is continuous extraction and the operation of stripping in two rotating disc contactors, finishes extracting-back extraction process behind the 2h, and the rate of recovery of tea-polyphenol is 13.84% as calculated.
Embodiment 2:
Tea dust is removed dust impurity, obtain the tea-polyphenol vat liquor with 4: 1 water-alcohol mixture of volume ratio at 90 ℃ of lower lixiviate 1h, the alcohol removed in the vat liquor of distillation obtains the tea-polyphenol concentrated solution, and diluting concentrated solution with the Repone K of pH=1.0-hydrochloride buffer, to obtain concentration be that 12g/L, pH are 1.2 tea-polyphenol stoste.1: 1 by volume with tea-polyphenol stoste (1L) and butylacetate (1L) respectively by at the bottom of the tower and cat head pump in the extraction tower, the tower body temperature is controlled at 10 ℃, rotary speed is controlled at 200r/min.Extracting phase leaves standstill at the bottom of tower after the balance, and extraction phase leaves standstill at cat head, is introduced into stripping column.Sodium phosphate dibasic-the citrate buffer solution (1L) that at stripping column adds pH=4.0 by back extraction phase and extraction phase volume ratio at 1: 1, the tower body temperature is controlled at 80 ℃, rotary speed is controlled at 200r/min, and back extraction is left standstill at cat head after the balance, and extraction phase leaves standstill at the bottom of tower.Whole process extraction phase is continuous extraction and the operation of stripping in two rotating disc contactors, finishes extracting-back extraction process behind the 1h, and the rate of recovery of tea-polyphenol is 6.10% as calculated.
Embodiment 3:
With summer and autumn tealeaves remove dust impurity, obtain the tea-polyphenol vat liquor with 3: 1 water-alcohol mixture of volume ratio at 80 ℃ of lower lixiviate 1.5h, the alcohol removed in the vat liquor of distillation obtains the tea-polyphenol concentrated solution, and diluting concentrated solution with the Sodium phosphate dibasic of pH=4.2-citrate buffer solution, to obtain concentration be that 15g/L, pH are 4.3 tea-polyphenol stoste.1: 2 by volume with tea-polyphenol stoste (1L) and primary isoamyl alcohol (2L) respectively by at the bottom of the tower and the cat head adverse current pump in the extraction tower, the tower body temperature is controlled at 30 ℃, rotary speed is controlled at 350r/min.Extracting phase leaves standstill at the bottom of tower after the balance, and extraction phase leaves standstill at cat head, is introduced into stripping column.Sodium bicarbonate-the sodium hydrate buffer solution (1L) that at stripping column adds pH=10.0 by back extraction phase and extraction phase volume ratio at 1: 2, the tower body temperature is controlled at 90 ℃, rotary speed is controlled at 350r/min, and back extraction is left standstill at the bottom of tower after the balance, and extraction phase leaves standstill at cat head.Whole process extraction phase is continuous extraction and the operation of stripping in two rotating disc contactors, finishes extracting-back extraction process behind the 5h, and the rate of recovery of tea-polyphenol is 15.85% as calculated.
Embodiment 4:
Low-grade tea is removed dust impurity, obtain the tea-polyphenol vat liquor with 4: 1 water-alcohol mixture of volume ratio at 90 ℃ of lower lixiviate 1h, the alcohol removed in the vat liquor of distillation obtains the tea-polyphenol concentrated solution, and diluting concentrated solution with the Sodium phosphate dibasic of pH=3.1-citrate buffer solution, to obtain concentration be that 10g/L, pH are 3.2 tea-polyphenol stoste.1: 1 by volume with tea-polyphenol stoste (1L) and acetin (1L) respectively by at the bottom of the tower and cat head pump in the extraction tower, the tower body temperature is controlled at 10 ℃, rotary speed is controlled at 200r/min.Extracting phase leaves standstill at cat head after the balance, and extraction phase leaves standstill at the bottom of tower, is introduced into stripping column.By back extraction phase and 1: 1 Tris-hydrochloride buffer (1L) at stripping column adding pH=9.0 of extraction phase volume ratio, the tower body temperature is controlled at 80 ℃, and rotary speed is controlled at 200r/min, and back extraction is left standstill at cat head after the balance, and extraction phase leaves standstill at the bottom of tower.Whole process extraction phase is continuous extraction and the operation of stripping in two rotating disc contactors, finishes extracting-back extraction process behind the 4h, and the rate of recovery of tea-polyphenol is 18.90% as calculated.
Embodiment 5:
Utilize the rotating disc contactor countercurrent extraction device to prepare the method for tea-polyphenol, as shown in Figure 1, above embodiment equipment used is the rotating disc contactor countercurrent extraction device, comprise extraction tower and stripping column, described extraction tower is identical with the stripping column structure, be provided with successively motor 6 from top to bottom, on the section of leaving standstill 7, the body of the tower section, under the section of leaving standstill 8, the section of leaving standstill 7 tops are provided with top discharge mouth 4 on described, the bottom is provided with charging opening 2, described body of the tower section is coated with recirculated water chuck 12, the section of leaving standstill 8 tops are provided with lower charging opening 3 under described, the bottom is provided with lower discharge port 5, on the section of leaving standstill with under be equipped with glass spring in the section of leaving standstill, motor is provided with rotating shaft 10, described rotating shaft by on the section of leaving standstill be through to the body of the tower section, the rotating shaft in the body of the tower section is provided with rotating disk 11; Charging opening links to each other with the first storage tank on the extraction tower, extraction tower top discharge mouth links to each other with the second storage tank, charging opening links to each other with the second storage tank under the extraction tower, the extraction tower lower discharge port links to each other with charging opening on the stripping column, charging opening links to each other with the 3rd storage tank under the stripping column, the stripping column lower discharge port links to each other with the 4th storage tank, and stripping column top discharge mouth links to each other with the 5th storage tank.The described rotating disk center of circle is provided with shaft hole, and average mark is furnished with one group of diameter less than the through hole of shaft hole around the shaft hole, and concrete steps are:
A. tealeaves is removed impurity, the water-alcohol mixture that with volume ratio is 5: 1～3: 1 obtains the tea-polyphenol vat liquor at 60～90 ℃ of lower lixiviate 0.5～1.5h, and then the alcohol that rotary evaporation is removed in the vat liquor obtains the tea-polyphenol concentrated solution, and with pH damping fluid dilution concentrated solution between 1～6, obtain concentration between 8～15g/L, the pH tea-polyphenol stoste between 1～6;
B. take tea-polyphenol stoste as raw material, take propyl carbinol, vanay, ethyl acetate, butylacetate or primary isoamyl alcohol as extraction agent, 2: 1 by volume～1: 2 with stoste and extraction agent respectively adverse current pump in the extraction tower, the phase that relative density is little (light phase) is entered by column bottoms pump, the phase that relative density is large (heavy phase) is pumped into by cat head, and two-phase liquid is fully contact under the rotation of rotating disk, finishes extraction process, last heavy phase leaves standstill at the bottom of tower, gently leaves standstill at cat head;
C. take the damping fluid of pH as 4～12 as strippant, 2: 1 by volume～1: 2 with extraction phase and strippant respectively adverse current pump in the stripping column, the phase that relative density is little among both (light phase) is entered by column bottoms pump, the phase that relative density is large (heavy phase) is pumped into by cat head, two-phase liquid is fully contact under dial rotation, finishes the back extraction process, and last heavy phase leaves standstill at the bottom of tower, gently leave standstill at cat head, whole process extraction phase is continuous extraction and the operation 0.5～5h that strips in two rotating disc contactors;
D. after stripping column separated, stripping obtained the tea-polyphenol sterling after vacuum-drying;
E. separate the anti-extracting phase (propyl carbinol, vanay, ethyl acetate, butylacetate or primary isoamyl alcohol) that obtains, can be as the extraction agent recycle behind washing or rotary evaporation.
The described starting material that are used for cooking vat liquor are tealeaves, and the pH of tea-polyphenol stoste is between 2～5, and the pH of strippant is between 4～11.Extraction process turntable rotating speed is 50～350r/min, and the body of the tower temperature is controlled at 5～50 ℃.Back extraction process turntable rotating speed is 50～350r/min, and the body of the tower temperature is controlled at 20～90 ℃.Damping fluid among the described step a is: Repone K-hydrochloride buffer pH 1-2 or Sodium phosphate dibasic-citrate buffer solution pH 2-7.Damping fluid among the described step c is Sodium phosphate dibasic-citrate buffer solution pH 4-7, Tris-hydrochloride buffer pH 8-9 or sodium bicarbonate-sodium hydrate buffer solution pH 10-11.Extraction phase continuous extraction and the operation 0.5～5h that strips in two towers among the described step c.
Claims (8)
1. utilize the rotating disc contactor countercurrent extraction device to prepare the method for tea-polyphenol, described rotating disc contactor countercurrent extraction device comprises extraction tower and stripping column, described extraction tower is identical with the stripping column structure, be provided with successively motor (6) from top to bottom, on the section of leaving standstill (7), the body of the tower section, under the section of leaving standstill (8), the section of leaving standstill on described (7) top is provided with top discharge mouth (4), the bottom is provided with charging opening (2), described body of the tower section is coated with recirculated water chuck (12), the section of leaving standstill under described (8) top is provided with lower charging opening (3), the bottom is provided with lower discharge port (5), on the section of leaving standstill and under be equipped with glass spring in the section of leaving standstill, motor is provided with rotating shaft (10), described rotating shaft by on the section of leaving standstill be through to the body of the tower section, the rotating shaft in the body of the tower section is provided with rotating disk (11); Charging opening links to each other with the first storage tank on the extraction tower, extraction tower top discharge mouth links to each other with the second storage tank, charging opening links to each other with the second storage tank under the extraction tower, the extraction tower lower discharge port links to each other with charging opening on the stripping column, charging opening links to each other with the 3rd storage tank under the stripping column, the stripping column lower discharge port links to each other with the 4th storage tank, and stripping column top discharge mouth links to each other with the 5th storage tank, it is characterized in that comprising the steps:
A. tealeaves is removed impurity, the water-alcohol mixture that with volume ratio is 5: 1～3: 1 obtains the tea-polyphenol vat liquor at 60～90 ℃ of lower lixiviate 0.5～1.5h, and then the alcohol that rotary evaporation is removed in the vat liquor obtains the tea-polyphenol concentrated solution, and with pH damping fluid dilution concentrated solution between 1～6, obtain concentration between 8～15g/L, the pH tea-polyphenol stoste between 1～6;
B. take tea-polyphenol stoste as raw material, take propyl carbinol, vanay, ethyl acetate, butylacetate or primary isoamyl alcohol as extraction agent, 2: 1 by volume～1: 2 with stoste and extraction agent respectively adverse current pump in the extraction tower, what relative density was little is entered by column bottoms pump, what relative density was large is pumped into by cat head, and two-phase liquid is fully contact under the rotation of rotating disk, finishes extraction process, last heavy phase leaves standstill at the bottom of tower, gently leaves standstill at cat head;
C. take the damping fluid of pH as 4～12 as strippant, 2: 1 by volume～1: 2 with extraction phase and strippant respectively adverse current pump in the stripping column, what relative density was little among both is entered by column bottoms pump, what relative density was large is pumped into by cat head, two-phase liquid is fully contact under dial rotation, finishes the back extraction process, and last heavy phase leaves standstill at the bottom of tower, gently leave standstill at cat head, whole process extraction phase is continuous extraction and the operation 0.5～5h that strips in two rotating disc contactors;
D. after stripping column separated, stripping obtained the tea-polyphenol sterling after vacuum-drying;
E. separate the anti-extracting phase that obtains, can be as the extraction agent recycle behind washing or rotary evaporation.
2. the method for utilizing the rotating disc contactor countercurrent extraction device to prepare tea-polyphenol according to claim 1 is characterized in that: the described starting material that are used for cooking vat liquor are tealeaves, and the pH of tea-polyphenol stoste is between 2～5, and the pH of strippant is between 4～11.
3. the method for utilizing the rotating disc contactor countercurrent extraction device to prepare tea-polyphenol according to claim 1, it is characterized in that: extraction process turntable rotating speed is 50～350r/min, the body of the tower temperature is controlled at 5～50 ℃.
4. the method for utilizing the rotating disc contactor countercurrent extraction device to prepare tea-polyphenol according to claim 1, it is characterized in that: back extraction process turntable rotating speed is 50～350r/min, and the body of the tower temperature is controlled at 20～90 ℃.
5. the method for utilizing the rotating disc contactor countercurrent extraction device to prepare tea-polyphenol according to claim 1, it is characterized in that: the damping fluid among the described step a is: Repone K-hydrochloride buffer pH 1-2 or Sodium phosphate dibasic-citrate buffer solution pH 2-7.
6. the method for utilizing the rotating disc contactor countercurrent extraction device to prepare tea-polyphenol according to claim 1, it is characterized in that: the described rotating disk center of circle is provided with shaft hole, and average mark is furnished with one group of diameter less than the through hole of shaft hole around the shaft hole.
7. the method for utilizing the rotating disc contactor countercurrent extraction device to prepare tea-polyphenol according to claim 1, it is characterized in that: the damping fluid among the described step c is Sodium phosphate dibasic-citrate buffer solution pH 4-7, Tris-hydrochloride buffer pH 8-9 or sodium bicarbonate-sodium hydrate buffer solution pH 10-11.
8. the method for utilizing the rotating disc contactor countercurrent extraction device to prepare tea-polyphenol according to claim 1 is characterized in that: extraction phase continuous extraction and the operation 0.5～5h that strips in two towers among the described step c.
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| CN112210398A (en) * | 2020-10-23 | 2021-01-12 | 泉州市欧美润滑油制品有限公司 | Production line and production process of high-quality lubricating oil |
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