CN102002089B - Process for extracting tea saponin from tea seed cakes or meal - Google Patents
Process for extracting tea saponin from tea seed cakes or meal Download PDFInfo
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- CN102002089B CN102002089B CN201010541011A CN201010541011A CN102002089B CN 102002089 B CN102002089 B CN 102002089B CN 201010541011 A CN201010541011 A CN 201010541011A CN 201010541011 A CN201010541011 A CN 201010541011A CN 102002089 B CN102002089 B CN 102002089B
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- 241001122767 Theaceae Species 0.000 title claims abstract description 41
- 229930182490 saponin Natural products 0.000 title claims abstract description 35
- 150000007949 saponins Chemical class 0.000 title claims abstract description 35
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title abstract description 29
- 235000012054 meals Nutrition 0.000 title abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 30
- 238000000605 extraction Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000001704 evaporation Methods 0.000 claims abstract description 3
- 230000008020 evaporation Effects 0.000 claims abstract description 3
- 238000005516 engineering process Methods 0.000 claims description 28
- 239000002994 raw material Substances 0.000 claims description 19
- 239000002699 waste material Substances 0.000 claims description 14
- 239000012141 concentrate Substances 0.000 claims description 9
- 238000010298 pulverizing process Methods 0.000 claims description 9
- 238000010411 cooking Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 238000001035 drying Methods 0.000 abstract description 6
- 238000004134 energy conservation Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000003337 fertilizer Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 238000010025 steaming Methods 0.000 abstract 1
- 238000003860 storage Methods 0.000 abstract 1
- 235000017709 saponins Nutrition 0.000 description 29
- 238000002386 leaching Methods 0.000 description 7
- 239000002893 slag Substances 0.000 description 7
- 238000000638 solvent extraction Methods 0.000 description 5
- 239000007858 starting material Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 240000007594 Oryza sativa Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 241000526900 Camellia oleifera Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000010495 camellia oil Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HVCOBJNICQPDBP-UHFFFAOYSA-N 3-[3-[3,5-dihydroxy-6-methyl-4-(3,4,5-trihydroxy-6-methyloxan-2-yl)oxyoxan-2-yl]oxydecanoyloxy]decanoic acid;hydrate Chemical compound O.OC1C(OC(CC(=O)OC(CCCCCCC)CC(O)=O)CCCCCCC)OC(C)C(O)C1OC1C(O)C(O)C(O)C(C)O1 HVCOBJNICQPDBP-UHFFFAOYSA-N 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- 229930186217 Glycolipid Natural products 0.000 description 1
- BWPGKXYWPBQBPV-MWQJAWBESA-N Theasaponin Chemical compound O([C@H]1[C@H](O)[C@H](O[C@H]([C@@H]1O[C@H]1[C@@H]([C@@H](O)[C@@H](O)CO1)O[C@H]1[C@@H]([C@@H](O)[C@H](O)CO1)O)O[C@H]1CC[C@]2(C)[C@H]3CC=C4[C@@]([C@@]3(CC[C@H]2[C@@]1(CO)C)C)(C)C[C@@H](O)[C@@]1(CO)[C@@H](OC(C)=O)[C@@H](C(C[C@H]14)(C)C)OC(=O)C(\C)=C/C)C(O)=O)[C@@H]1O[C@H](CO)[C@H](O)[C@H](O)[C@H]1O BWPGKXYWPBQBPV-MWQJAWBESA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 cinestrip Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to a process for extracting tea saponin from tea seed cakes or meal after oil frying by applying an industrial production device. The process comprises the following steps: crushing the tea seed cakes or the meal (leading the particle size to be 1-3mm), then sending into a steaming and stir-frying cauldron, drying (preventing the water content from exceeding 7%), then leading the material to enter into a material storage cylinder, using a screw conveyor to send the material into a rotocel extractor, and adding a solvent for extraction; carrying out residue-liquid separation (the meal residue can be used as a feed or a fertilizer) after double extraction, leading extraction solution to enter into a long pipe evaporator, removing part of water by double evaporation, and recycling the solvent (which can be recycled); and concentrating the extraction solution via a vacuum concentration tank, then crystallizing and drying, and obtaining a fine saponin finished product for packaging and leaving a factory. A product produced by the process contains 81.5% of active matters, and the pH value is 5.9. Compared with other methods, the process has the advantages of high product purity, light color, high production rate (14%), energy conservation, low consumption, no pollution and environmental protection, and is easy for operation and the like.
Description
Technical field
The present invention relates to a kind of from from tea waste, extracting the technology of tea saponin.
Background technology
Tea saponin is a kind of nonionogenic tenside of excellent property; Emulsification, foaming, lubricated, surely there is good performance aspect such as bubble and decontamination, is widely used in material of construction, pesticide processing, aquaculture, food, light industry, medicine, wool spinning, industry such as knitting; Can be used for making various types of emulsifying agents, agricultural chemicals, rubber, extinguish material, cinestrip, Shampoo & Conditioner, foaming Steel Concrete, prawn culturing agent etc., can develop 180 surplus kind of series product, potentiality to be exploited is huge, market outlook are wide.About the extraction and the application of tea saponin, China has very years of researches and practice, and conclusion is got up, and 4 kinds of methods are arranged usually, and both water seaoning, absorption method, microwave/light wave dry method were extracted and the organic solvent extraction method.
Water seaoning is that tea-cake dregs is ground into meal, and 5 times hot water are added in the meal, under 30～35 ℃ of temperature, soaks 2h, and the lixiviate number of times is twice.Soak the back spinning, fertilizer is made in the residue oven dry.Merge vat liquor, add 2% flocculation agent, and leave standstill after being heated to certain temperature, separate and remove throw out, adopt the method for vacuum concentration that vat liquor is concentrated into 30 degree Beaume, get the liquid saponin.This production technique, equipment are simple, less investment, but yield rate is low, and the concentrate drying process consumes high, belongs to eliminating technology.
Absorption method adopts water or solvent lixiviate tea waste, with impurity such as the glycolipid in inorganics or the organic resin adsorbing and extracting liquid, juice, pigments, again through lixiviate, concentrate finished product.This method cost is high, yields poorly, and has pollution problem.Produce exhausted inorganics and organic resin difficult treatment in enormous quantities.
Organic solvent extraction method 1, solvent pairs substep extraction and separation process are removed grease remaining in the grouts with oil-dissolving solvent earlier, and the degreasing grouts are used 70%～95% organic solvent extraction saponin again, and the extracting solution process is filtered the back compression and concentrated, and gets thick saponin.2, single solvent extraction separating technology, this method obtains tea oil and two kinds of products of tea saponin simultaneously with a set of equipment, two kinds of solvents.Cake of camellia oleifera seeds is crushed to certain fineness, makes saponin dissolve leaching, again with stirring solvent mixing, extracting and separating, crude oil is isolated in clean then liquid layering, and remaining liquid gets thick saponin through concentrated, impurity elimination, reconcentration.Decolouring then, the dry finished product that gets.Its technology is loaded down with trivial details.Production process is used the very easily manufacturing environment pollution of multiple solvent.
The method of process for abstracting theasaponine by microwave/light wave dry, it is fluctuation, high frequency property, thermal property and a non-thermal property of utilizing little/light wave, and cake of camellia oleifera seeds is carried out dry process, lixiviate then, extraction, decolouring, drying are obtained the tea saponin finished product.Very convenient because of handling with microwave/light wave at a few hectogram raw materials of testing laboratory, tens tons in process of production, hundreds of ton have been handled just inconvenient with microwave/light wave, and consumes energy is huge.Moreover still want lixiviate, extraction, decolouring, drying after handling, its effect is not fairly obvious, has pollution problem simultaneously yet.
The present invention is in order to overcome the weak point that prior art exists, a kind of technology of from tea waste, extracting tea saponin to be provided, this technology have the product purity height, of light color, yield rate is high, energy-conservation, joint consumption, pollution-free, environmental protection, advantage such as easy to operate.
Summary of the invention
The present invention is in order to overcome the weak point that prior art exists, a kind of technology of from tea waste, extracting tea saponin to be provided, this technology have the product purity height, of light color, yield rate is high, energy-conservation, joint consumption, pollution-free, environmental protection, advantage such as easy to operate.
Technical solution problem of the present invention adopts following technical scheme:
From tea waste, extract the technology of tea saponin, comprise raw material pulverizing, oven dry, lixiviate, separation, concentrate, its process characteristic is:
Said raw material pulverizing is meant raw material pulverizing to granularity 1-3mm particulate state;
Said oven dry, be meant with the raw material after pulverizing deliver to automatic cooking pot dried through 10-30 minute to the raw material water cut less than 7%;
In the said lixiviate step, solvent is selected from the ethanolic soln that concentration is 75%-85%, and extraction time is 1-1.5 hour; Twice of lixiviate.
From tea waste, extract the technology of tea saponin, its process characteristic also is:
In the said lixiviate step, the temperature of extraction solvent is 40-50 ℃.
The weight ratio of said extraction solvent and tea waste is controlled at 3: 1-4: 1, promptly solvent be raw material 3-4 doubly.
In the said enrichment step, adopt the evaporation of secondary long tube, 50-80 ℃ of one-level temperature, 70-95 ℃ of secondary temperature; Automatically surplus temperature concentrates 2-4 hour naturally after importing vacuum concentration pot after 2-4 minute.
Compared with present technology, beneficial effect of the present invention is embodied in:
1, the present invention is crushed to the particulate state of 1-3mm with starting material leached tea oil slag or tea cake, and breaking in the past, people always think that starting material are thin more, the idea that saponin is leached more easily; Original technology is machined to 40 orders-120 order powdery with starting material, processes carefully to 300 orders, though the saponin dissolution rate after the pulverizing has been accelerated in addition even with it; But increased slag liquid separation difficulty degree; Simultaneously impurity such as a large amount of xylogen is present in the leach liquor, causes that saponin purity is low, color is dark, follow-uply also wants the removal of impurity, decolouring.The present invention has overcome former defective workmanship; Slag, liquid separate easily; Product purity is high, light; Reduced follow-up decolouring link, reduced tooling cost simultaneously, every day with tens of ton sometimes up to a hundred tons of tea cakes or the dregs of rice particulate state that is crushed to 1-3mm with former technology starting material are machined to 40 orders-120 order or 300 order powderies are compared the processing charges that will practice thrift thousands of units.
2, the present invention adopts stoving process, makes the starting material water content be no more than 7%, because of the excessive solvent of raw material moisture content is difficult for immersing, after oven dry, makes solvent be prone to immerse in the material, accelerates the saponin leaching velocity.
3, extraction solvent temperature of the present invention is 40-50 ℃, and the change of soaking temperature can have influence on the partition equilibrium of tea saponin at solid-liquid, because solvent extraction saponin and water specific rate are very fast, if improve solvent temperature, can quicken the dissolution rate of saponin.What have in the former technology does not heat, and the artificial leaching velocity that improves of great majority heats solvent temperature to more than 50 ℃.Do not heat or temperature to cross low leaching velocity slow, it is too high to heat, the saponin leaching velocity is accelerated, the pigment leaching velocity is accelerated simultaneously.And energy consumption is big, and the loss of solvent is also big.The present invention compares with former technology, and tea dregs of rice slag color is dark after separating, and also darker than the tea dregs of rice color of not extracting tea saponin, this explains that most of pigment remains in the slag.Energy-conservation, joint consumption that the present invention compares with former technology has increased one deck guarantee for reducing follow-up decolouring step simultaneously.
4, the production technique that the present invention's employing is flatted turn or pot group type combines.Leaching number of times is 2-3 time, and soak time 1-1.5h compares with former technology 2h-4h, improves work efficiency more than 1 times.
5, adopt the secondary long-tube evaportor in the enrichment step of the present invention; 50-80 ℃ of one-level temperature; Secondary 70-95 ℃, import vacuum concentration pot after 2-4 minute automatically and utilize surplus temperature to concentrate 2-4 hour naturally, adopt the ladder temperature to utilize temperature difference operation automatically from bottom to top; Improve the speed of concentrating, reduce solvent loss.Residual solvent all reclaims.Compare save energy and material consumption about 10% with former technology, and pollution-free.
6, the every equipment that contacts with saponin with solvent of production whole process of the present invention all adopts all steel manufacturing.And in whole sealing status, move.All round process only is suitable for a kind of solvent (ethanol), and recyclablely uses again.Deduct the decolouring link, overcome the environmental pollution that former technology uses multiple solvent, auxiliary agent to cause.The present invention is energy-conservation, joint consumes, environmental protection is fit to scale operation.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Below will combine embodiment that the present invention is further specified.
Embodiment:
Embodiment 1:
Take by weighing raw material 2000kg it be crushed to granularity 1-3mm particulate state, deliver to then cooking pot dried through 10-30 minute to the raw material water cut less than 7%; Using volumetric concentration then is that 75% ethanolic soln is as solvent; Solvent and tea waste carried out proportioning in 3: 1 by weight percentage; The entering digester of flatting turn is 40-50 ℃ of following lixiviate 1-1.5 hour in temperature, and twice back of lixiviate slag liquid separates automatically, and vat liquor gets into the secondary long-tube evaportor; 50-80 ℃ of one-level temperature, 70-95 ℃ of secondary temperature; Automatically surplus temperature concentrates 2-4 hour naturally after importing vacuum concentration pot after 2-4 minute, through dry light yellow powdery tea saponin 276kg, the yield rate 13.8% of getting.(product and feed ratio) exceeds 1.8% than former technology.Through chemical examination active matter content 81.5%; PH value 5.9.All meet or exceed former craft quality standard.
Embodiment 2
Take by weighing raw material 2000kg it be crushed to granularity 1-3mm particulate state, deliver to then cooking pot dried through 10-30 minute to the raw material water cut less than 7%; Use then volumetric concentration be 85% ethanolic soln as solvent, solvent and tea waste carried out proportioning in 4: 1 by weight percentage, getting into the digester of flatting turn is 40-50 ℃ of following lixiviate 1-1.5 hour in temperature; Twice back of lixiviate slag liquid separates automatically, and vat liquor gets into secondary long-tube evaportor, 50-80 ℃ of one-level temperature; 70-95 ℃ of secondary temperature; Automatically surplus temperature concentrates 2-4 hour naturally after importing vacuum concentration pot after 2-4 minute, through dry faint yellow powdery tea saponin 278.5kg, the yield rate 13.93% of getting.All reach and surpass former processing quality level through chemical examination.
Embodiment 3
Take by weighing 700 tons of raw materials, press embodiment 2 technological operations, move 17 days continuously (24 hours every days), obtain 98.5 tons of tea saponins at last.Yield rate 14.07%.Product sample presentation to Anhui Product Quality Supervision and Testing Institute checks, and tea saponin massfraction 64.30% exceeds 14% than former technology 50%; PH value 6.0 is than the high 0.1-0.3 of former technology; Active matter content 81.5% is than the high 5-15% of former technology; Color is light yellow and former resemble process.
Claims (3)
1. from tea waste, extract the technology of tea saponin, comprise raw material pulverizing, oven dry, lixiviate, separation, concentrate, it is characterized in that:
Said raw material pulverizing is meant raw material pulverizing to granularity 1-3mm particulate state;
Said oven dry, be meant with the raw material after pulverizing deliver to automatic cooking pot dried through 10-30 minute to the raw material water cut less than 7%;
In the said lixiviate step, solvent is selected from the ethanolic soln that concentration is 75%-85%, and extraction time is 1-1.5 hour; Twice of lixiviate;
In the said enrichment step, adopt the evaporation of secondary long tube, 50-80 ℃ of one-level temperature, 70-95 ℃ of secondary temperature; Automatically surplus temperature concentrates 2-4 hour naturally after importing vacuum concentration pot after 2-4 minute.
2. the technology of from tea waste, extracting tea saponin according to claim 1, it is characterized in that: in the said lixiviate step, the temperature of extraction solvent is 40-50 ℃.
3. the technology of from tea waste, extracting tea saponin according to claim 1, it is characterized in that: in the said lixiviate step, the weight ratio of extraction solvent and tea waste is controlled at 3: 1-4: 1, promptly solvent is 3-4 a times of raw material.
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| CN201010541011A CN102002089B (en) | 2010-11-12 | 2010-11-12 | Process for extracting tea saponin from tea seed cakes or meal |
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Families Citing this family (9)
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| CN102229637B (en) * | 2011-04-18 | 2016-05-11 | 浙江久晟油茶科技股份有限公司 | A kind of technique of extracting Tea Saponin employing membrane separation concentration |
| CN102250681B (en) * | 2011-06-20 | 2012-10-31 | 江南大学 | Method for extracting camellia oil and tea saporin from tea seeds |
| CN105238551B (en) * | 2015-10-09 | 2018-12-21 | 福建天斯顿生物科技有限公司 | A kind of supercritical CO2The method of abstraction purification camellia seed oil |
| CN105461780B (en) * | 2015-12-09 | 2018-03-16 | 中国林业科学研究院亚热带林业研究所 | A kind of inexpensive Tea Saponin high-efficiency and continuous extraction process |
| CN106565812B (en) * | 2016-09-26 | 2018-12-07 | 中国林业科学研究院亚热带林业研究所 | A kind of continuous Extraction solvent high efficiente callback technique of Tea Saponin |
| CN109456384A (en) * | 2018-09-25 | 2019-03-12 | 江西久晟油茶发展有限公司 | A kind of Tea Saponin negative pressure continuously leaches method for concentration |
| CN109628209A (en) * | 2019-01-07 | 2019-04-16 | 蒋文昌 | A kind of tea seed essence production technology |
| CN111187333A (en) * | 2019-04-11 | 2020-05-22 | 杭州千岛湖天鑫有限公司 | Method for extracting tea saponin applied to cosmetics |
| CN114231349A (en) * | 2021-12-20 | 2022-03-25 | 查雨欣 | Processing system of strong aromatic tea oil |
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| CN101423544A (en) * | 2008-12-04 | 2009-05-06 | 上海大学 | Method for extracting residual oil and tea saponin from tea seed cake after oil extraction |
| CN101695336A (en) * | 2009-10-28 | 2010-04-21 | 胡国田 | Application and preparation method of tea seed episperm bioactive extracts |
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| 叶雪良.茶皂素的开发与利用.《化工生产与技术》.2002, * |
| 叶雪良.茶皂素的开发与利用.《化工生产与技术》.2002,第9卷(第2期),第6-8页. * |
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Denomination of invention: Process for extracting tea saponin from tea seed cakes or meal Effective date of registration: 20190104 Granted publication date: 20120905 Pledgee: Lu'an rural commercial bank Limited by Share Ltd Pledgor: Anhui Yingshanhong Biological Technology Co., Ltd. Registration number: 2018340000804 |
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Date of cancellation: 20200313 Granted publication date: 20120905 Pledgee: Lu'an rural commercial bank Limited by Share Ltd Pledgor: ANHUI YINGSHANHONG BIOLOG TECHNOLOGY Co.,Ltd. Registration number: 2018340000804 |