CN1068360A - From oil tea (tea-seed) grouts, extract the technology of tea oil and saponin - Google Patents
From oil tea (tea-seed) grouts, extract the technology of tea oil and saponin Download PDFInfo
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- CN1068360A CN1068360A CN91106741A CN91106741A CN1068360A CN 1068360 A CN1068360 A CN 1068360A CN 91106741 A CN91106741 A CN 91106741A CN 91106741 A CN91106741 A CN 91106741A CN 1068360 A CN1068360 A CN 1068360A
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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Abstract
The technology of extracting tea oil and saponin from oil tea (tea-seed) grouts belongs to the method for extracting saponin from vegetable material.The present invention is with 1-15% single alcohol kind solvent and water extraction, raw material and solvent extract simultaneously in the side-filtering type whizzer after with 1: 1.5-2.5 mixed and separate, in the three-phase helical-conveyer centrifugal, isolate tea oil, saponin and residue then, concentrating under reduced pressure again, decolouring, deodorization, clean liquid drying.Extract saponin with processing method of the present invention, extraction yield is 9.5-14.5% of a raw material, and the content of thick saponin is 70-80%.This technology is the plant factor height not only, and solvent consumption is little, and extraction time shortens work efficiency raising, especially the extraction yield height of saponin, extensive, the serialization production of suitable factory.
Description
The technology of extracting tea oil and saponin from oil tea (tea-seed) grouts belongs to the method for extracting saponin from vegetable material.
The technology of extracting tea oil and saponin both at home and abroad from oil tea (tea-seed) grouts generally adopts multi-solvent substep extraction and separation process, as Japanese Patent 173963(clear and 19 years) saponin that extracts in the tea waste is to use methanol extraction below 0 ℃, use the ether sedimentation saponin again, the product purity height, but operational requirement strictness, solvent consumption is big, and extraction yield is 7.7% of a raw material; Russian patent 957910(1982) tea oil of Ti Chuing and saponin extracting method are to extract tea oil earlier with ethylene dichloride under 60-70 ℃ of temperature condition, after getting tea saponin with the methyl alcohol or the quintessence of drinking again, use acetone precipitation again, though product purity height, product yield also can reach the 14-16% of raw material, but still be multistep solvent method, and consume three kinds of solvents, acetone is also incomplete to the precipitation of saponin, so the production cost height, and using has certain difficulty.Domestic have part factory to take to extract tea oil with the 6# solvent oil earlier, and with methyl alcohol or extraction using alcohol saponin, extraction yield is the 8-10% of raw material to its residual dregs of rice again, but need the molten equipment of two covers, thereby increase investment and production cost; Some factory adopts the hot water extraction saponin, though technology is simple, does not consume organic solvent, and quality product is low, and rough saponin content only is 30-40%, just reach 60-70% after making with extra care, and extraction yield only is the 7-8% of raw material.CN86106634.A adopts mixed solvent one step from grouts to extract tea oil and saponin technology, though reduced desolventizing equipment, but need leave standstill more than 8 hours during extraction, treat that tea oil is separated after the layering voluntarily, separate out saponin in the concentrated solution with acetone again, therefore prolonged the production cycle, or solved with increasing the oily tower of jumbo branch, facility investment still fails to reduce.
The present invention is intended to same set of equipment, a kind of solvent, realizes that separating and extracting carries out synchronously, and the extraction yield height, and extraction time is short, solves the problem that remains in the current prior art.
The technical scheme that realizes task of the present invention is: with single alcohol kind solvent and the water extracting and separating of 1-15%, raw material and solvent are with 1: the amount 1.5-2.5(weight ratio) extracts and separation circuit in the side-filtering type whizzer simultaneously in the mixed back of abundant stirring, the vat liquor that takes off slag after separating separates tea oil, saponin and residue in the three-phase helical-conveyer centrifugal, the centrifugate that contains saponin behind the multiple-effect evaporator concentrating under reduced pressure again through centrifugal impurity elimination drying, the extraction yield of saponin is the 9.5-14.5% of raw material, and the content of thick saponin is 70-80%.Concentration is that the single alcohol kind solvent of 1-15% can be methyl alcohol, ethanol, Virahol, propyl carbinol or primary isoamyl alcohol, and the extracting and separating operation of carrying out synchronously in the side-filtering type whizzer should extract 2-3 time repeatedly, and each time is 10-30 minute.
Be described in further detail the present invention below in conjunction with accompanying drawing.
Figure one tea oil and saponin extraction process schema
1, tea cake pulverizing 10, decoloration and deodorization
2, stir mixed 11, clean liquid
3, solvent or water 12, liquid tea saponin finished product
4, extracting and separating 13, drying
5, liquid, liquid, separate 14 admittedly, tea saponin dry powder
6, second and third not good liquor basin 15, column chromatography
7, the residual dregs of rice reclaim solvent 16, tea cake residue
8, evaporation precipitation 17, crude oil are made with extra care
9, multiple-effect concentrate 18, the edible camellia oil finished product
Oil tea (tealeaves seed) grouts are crushed to more than 40 mesh sieves, any extract and separate in the organic solvents such as methyl alcohol, ethanol, isopropyl alcohol, n-butanol or isoamyl alcohol of employing 1-15%, when extract and separate for the second time or for the third time, can adopt water, raw material and solvent are 1 by weight: after the amount of 1.5-2.5 fully stirs and mixes, in the side-filtering type centrifuge, under 55-70 ℃ temperature conditions, adverse current, stirring, Centrifugical extraction saponin, tea oil, tannin, caffeine, aliphatic acid and other lipides obtain the residual dregs of rice of tea cake simultaneously. With rare alcohols solvent extraction, both made solvent dissolving Tea Saponin and miscible tea oil, the polarity of adjustable water again makes that Tea Saponin is easier to be dissolved in the water, utilize simultaneously the characteristics of butanols, the different solubility of isoamyl alcohol solvent in the hot water or cold water, when heating was extracted, organic solvent overflowed from water, thereby Tea Saponin and tea oil are dissolved out from the tea cake, when temperature reduces, solvent is dissolved in the water again, thereby has reduced the volatilization of solvent, has reduced the loss of solvent.
The present invention has selected the side-filtering type centrifuge to realize that extraction is with centrifugal, carry out synchronously, namely extract and take off liquid and finish simultaneously, particle d＜the 0.01mm that separates, taking off liquid measure is 10T/h, each Centrifugical extraction time is 10-30 minute, adopt repeatedly 2-3 centrifugal way of extraction, namely add for the first time organic solvent extract centrifugal after, to being present in that residue in the centrifuge is proceeded for the second time again even Centrifugical extraction for the third time, available organic solvent extraction is centrifugal for the second time, for the third time available water extraction is centrifugal, and the 2nd, the time of the 3rd extraction rotary process is about 5-10 minute, extracts centrifugal total time＜30 minute for three times, so with short production cycle, recovery rate can reach the 9.5-14.5% of raw material.
The technological parameter that extracts Tea Saponin and tea oil is as follows:
More than grouts grinding particle size 40 mesh sieves
Solvent 1-15% methyl alcohol, ethanol, Virahol, propyl carbinol or primary isoamyl alcohol
Grouts and weight of solvent are than 1: 1.5-2.5
The extracting mode adverse current stirs, Centrifugical extraction carries out synchronously
Extraction time 10-30 minute
PH 5.5-6.8 or 4-5
Auxiliary agent 0-5%NaCl
Temperature 55-70 ℃
Pressure 0-3kg/cm
2
The residual dregs of rice contain saponin＜0.5%
Residual dregs of rice oil-containing＜0.3%
Vat liquor after taking off liquid is by the three-phase helical-conveyer centrifugal, realize liquid-liquid-solid automatic separation, isolate tea oil, solvent and residue, fractional dose is 10T/h, isolated tea saponin centrifugate is through the triple-effect evaporator concentrating under reduced pressure, and tail gas enters the immersion type condenser and reclaims rare solvent.Crude extractive behind concentrating under reduced pressure, the decoloration and deodorization is dissolved in the 60-80 ℃ of hot water, through washing cool off again centrifugal after the clean liquid that obtains of the removal of impurity obtain rough saponin through the vacuum concentration drying, content＞70%.The process for purification of rough saponin can add 5%NaCl earlier by behind the alumina column before the vacuum concentration drying, regulates PH4-5, carries out liquid-liquid extraction with butanols, and extraction liquid obtains the refining saponin of content＞85% through the reduced vacuum concentrate drying.Isolated rough tea oil is produced high-quality tea oil and recovery part organic solvent through high temperature (130-150 ℃) vacuum (640-660mmHg) evaporation precipitation.The residual dregs of rice of gained tea cake added 60-80 ℃ of hot water by 1: 1.5, centrifugal washing 5-10 minute, reclaimed remaining tea saponin in the organic solvent that adsorbs in the residual dregs of rice and the residual dregs of rice.
Example one: take by weighing and contain fat tea-cake dregs 1000kg, put into jar, the weight ratio 1: 2 of pressing raw material and solvent adds 8% propyl carbinol and 92% water, in the lixiviate jar of overcoat steam insulation, under 60 ℃ of temperature condition, fully stir and be blended into pasty state and do not have cluster of grains, send into automatic side-filtering type centrifuge again, extract synchronously and centrifugation, for the first time extracted centrifugation time about 15 minutes, tea cake residue in whizzer is re-extract 2 times again, still use for the second time 8% butanols, the extraction time is 8 minutes, water for the third time, and the extraction time is 5 minutes, the extraction liquid that merges three times is through liquid-liquid-solid three-phase centrifugation, saponin liquid decolours after sending into the triple-effect evaporator concentrating under reduced pressure again, deodorization, quiet liquid removal of impurities, drying obtains rough tea saponin pulvis 179.72kg, and product yield is 17.97%, thick saponin purity is 76.23%, the tea saponin extraction yield is 13.7% of a raw material, produces tea oil 35kg only, and it is 3.5% that raw material is put forward the tea oil rate.
In actual production process, go mouldy for preventing grouts, utilize this complete equipment to extract tea oil earlier in grouts purchase back, and then water produce saponin, can improve the quality of products like this, again the abundant potentiality of excavating equipment.
Example two
Take by weighing tea-cake dregs 1000kg after the degreasing, put into blend tank, add 60 ℃ of hot water at 1: 2.5 by solid-to-liquid ratio (weight), stirring is blended into sends into extracting and separating in the automatic side-filtering type centrifuge after pasty state does not have cluster of grains, vat liquor is sent into subsequent processing and is concentrated, tea cake residue adds water and continues for the second time extracting and separating for the third time in whizzer, the intact residue of extracting and separating is discharged outside the machine automatically, parting liquid concentrates the rear decoloring deodorization through triple-effect evaporator, then enter the quiet liquid removal of impurities of triphase horizontal helical-conveyer centrifugal, carry out drying again.Get rough tea saponin pulvis 126.43kg.Tea saponin purity is 79.81%, and the raw material extraction yield is 10.09%, and thick saponin productive rate is 12.64%.
Adopt tea oil of the present invention and saponin extraction process, a kind of solvent of a set of equipment can be realized the extraction of tea oil and saponin, plant factor height not only, solvent consumption is few, and extraction time shortens, work efficiency improves, and especially the extraction yield of saponin improves, and is suitable for therefore that factory is extensive, serialization production.
Claims (3)
1, a kind of technology of from oil tea (tea-seed) grouts, extracting tea oil and saponin, water or organic solvent extraction separate, the invention is characterized in single alcoholic solvent and water extracting and separating with 1-15%, is 1 with raw material and solvent with weight ratio: after the amount of 1.5-2.5 fully stirs and mixes, in the side-filtering type whizzer, extract simultaneously and separation circuit, after separating, take off the leaching liquid of slag and in the three-phase helical-conveyer centrifugal, isolate tea oil, saponin and residue, the centrifugate that contains saponin behind the multiple-effect evaporator concentrating under reduced pressure again through centrifugal impurity elimination, dry, the extraction yield of saponin is the 9.5-14.5% of raw material, and the content of thick saponin is 70-80%.
2, by the described technology of extracting tea oil and saponin from oil tea (tea-seed) grouts of claim 1, the single alcoholic solvent that it is characterized in that 1-15% can be methyl alcohol, ethanol, Virahol, propyl carbinol or primary isoamyl alcohol.
3, by the described technology of extracting tea oil and saponin from oil tea (tea-seed) grouts of claim 1, it is characterized in that the extraction and the separation circuit that carry out synchronously in the side-filtering type whizzer should extract 2-3 time repeatedly, each time is 10-30 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN91106741A CN1034346C (en) | 1991-07-03 | 1991-07-03 | Process of abstracting tea oil and saponin from tea-oil seed (and tea seed) dregs |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN91106741A CN1034346C (en) | 1991-07-03 | 1991-07-03 | Process of abstracting tea oil and saponin from tea-oil seed (and tea seed) dregs |
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| CN1068360A true CN1068360A (en) | 1993-01-27 |
| CN1034346C CN1034346C (en) | 1997-03-26 |
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| CN91106741A Expired - Fee Related CN1034346C (en) | 1991-07-03 | 1991-07-03 | Process of abstracting tea oil and saponin from tea-oil seed (and tea seed) dregs |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996005278A1 (en) * | 1994-08-16 | 1996-02-22 | Dr. Frische Gmbh | Process for extracting native products which are not water-soluble from native substance mixtures by means of centrifugal force |
| WO1996031579A1 (en) * | 1995-04-04 | 1996-10-10 | Trenntec Trenntechnik Gmbh | Process for extracting oils or fats from oleaginous natural substances and use thereof |
| CN1061352C (en) * | 1997-01-24 | 2001-01-31 | 中国科学院化学研究所 | Extraction method of oil-tea camellia seed saponin |
| WO2002061023A1 (en) * | 2000-12-21 | 2002-08-08 | Huang Bao-Sheng | The method for purifying tea seed oil |
| CN101775334A (en) * | 2010-03-01 | 2010-07-14 | 郑小非 | Method for extracting tea seed oil by using water |
| CN101906350A (en) * | 2010-08-25 | 2010-12-08 | 国家粮食局科学研究院 | Method for extracting grease from oil-tea camellia seed kernel and recovering saponin and saccharide active substances |
| CN102061217A (en) * | 2011-01-05 | 2011-05-18 | 华侨大学 | Method for extracting tea seed oil by using enzymatic hydrolysis method |
| CN102061219A (en) * | 2011-01-05 | 2011-05-18 | 华侨大学 | Method for extracting tea seed oil |
| CN102488095A (en) * | 2011-12-23 | 2012-06-13 | 南京正宽医药科技有限公司 | Green feedstuff additive containing camellia seed triterpenoid saponin |
| CN102586026A (en) * | 2012-02-26 | 2012-07-18 | 湖南大三湘油茶科技有限公司 | Recovery treatment method of oil-tea camellia seed oil decoloration waste |
| CN102839046A (en) * | 2012-08-28 | 2012-12-26 | 湖南省林业科学院 | Process for synchronously extracting grease and products with high added values through grinding and n-butyl alcohol |
| CN103060084A (en) * | 2013-01-27 | 2013-04-24 | 管天球 | Method for leaching and processing residual oil of tea cakes |
| CN107653055A (en) * | 2017-09-29 | 2018-02-02 | 浙江工业大学 | A kind of method of ultrasonic wave added extracting tea seed oil by using enzymatic hydrolysis |
| CN108948124A (en) * | 2018-08-01 | 2018-12-07 | 永兴县悠香山茶油有限公司 | A kind of preparation method of Tea Saponin |
| CN109705974A (en) * | 2019-02-25 | 2019-05-03 | 湖南粮食集团有限责任公司 | A kind of method of the synchronous extraction tea oil and saponin of wet grinding original position microemulsified |
-
1991
- 1991-07-03 CN CN91106741A patent/CN1034346C/en not_active Expired - Fee Related
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996005278A1 (en) * | 1994-08-16 | 1996-02-22 | Dr. Frische Gmbh | Process for extracting native products which are not water-soluble from native substance mixtures by means of centrifugal force |
| US5928696A (en) * | 1994-08-16 | 1999-07-27 | Dr. Frische Gmbh | Process for extracting native products which are not water-soluble from native substance mixtures by centrifugal force |
| WO1996031579A1 (en) * | 1995-04-04 | 1996-10-10 | Trenntec Trenntechnik Gmbh | Process for extracting oils or fats from oleaginous natural substances and use thereof |
| CN1061352C (en) * | 1997-01-24 | 2001-01-31 | 中国科学院化学研究所 | Extraction method of oil-tea camellia seed saponin |
| WO2002061023A1 (en) * | 2000-12-21 | 2002-08-08 | Huang Bao-Sheng | The method for purifying tea seed oil |
| CN101775334A (en) * | 2010-03-01 | 2010-07-14 | 郑小非 | Method for extracting tea seed oil by using water |
| CN101906350A (en) * | 2010-08-25 | 2010-12-08 | 国家粮食局科学研究院 | Method for extracting grease from oil-tea camellia seed kernel and recovering saponin and saccharide active substances |
| CN102061219A (en) * | 2011-01-05 | 2011-05-18 | 华侨大学 | Method for extracting tea seed oil |
| CN102061217A (en) * | 2011-01-05 | 2011-05-18 | 华侨大学 | Method for extracting tea seed oil by using enzymatic hydrolysis method |
| CN102061217B (en) * | 2011-01-05 | 2013-08-14 | 华侨大学 | Method for extracting tea seed oil by using enzymatic hydrolysis method |
| CN102488095A (en) * | 2011-12-23 | 2012-06-13 | 南京正宽医药科技有限公司 | Green feedstuff additive containing camellia seed triterpenoid saponin |
| CN102488095B (en) * | 2011-12-23 | 2013-02-27 | 重庆优宝生物技术有限公司 | Green feedstuff additive containing camellia seed triterpenoid saponin |
| CN102586026A (en) * | 2012-02-26 | 2012-07-18 | 湖南大三湘油茶科技有限公司 | Recovery treatment method of oil-tea camellia seed oil decoloration waste |
| CN102839046A (en) * | 2012-08-28 | 2012-12-26 | 湖南省林业科学院 | Process for synchronously extracting grease and products with high added values through grinding and n-butyl alcohol |
| CN103060084A (en) * | 2013-01-27 | 2013-04-24 | 管天球 | Method for leaching and processing residual oil of tea cakes |
| CN107653055A (en) * | 2017-09-29 | 2018-02-02 | 浙江工业大学 | A kind of method of ultrasonic wave added extracting tea seed oil by using enzymatic hydrolysis |
| CN108948124A (en) * | 2018-08-01 | 2018-12-07 | 永兴县悠香山茶油有限公司 | A kind of preparation method of Tea Saponin |
| CN109705974A (en) * | 2019-02-25 | 2019-05-03 | 湖南粮食集团有限责任公司 | A kind of method of the synchronous extraction tea oil and saponin of wet grinding original position microemulsified |
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| Publication number | Publication date |
|---|---|
| CN1034346C (en) | 1997-03-26 |
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