CN1054788A - Process for extracting grease and tea saponin by one-step leaching of cake dregs - Google Patents
Process for extracting grease and tea saponin by one-step leaching of cake dregs Download PDFInfo
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- CN1054788A CN1054788A CN90101339A CN90101339A CN1054788A CN 1054788 A CN1054788 A CN 1054788A CN 90101339 A CN90101339 A CN 90101339A CN 90101339 A CN90101339 A CN 90101339A CN 1054788 A CN1054788 A CN 1054788A
- Authority
- CN
- China
- Prior art keywords
- leaching
- tea
- tea saponin
- lower alcohol
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 238000002386 leaching Methods 0.000 title claims abstract description 46
- 150000007949 saponins Chemical class 0.000 title claims abstract description 39
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 38
- 229930182490 saponin Natural products 0.000 title claims abstract description 38
- 241001122767 Theaceae Species 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000004519 grease Substances 0.000 title claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000003921 oil Substances 0.000 claims abstract description 12
- 239000010495 camellia oil Substances 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000001556 precipitation Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000012141 concentrate Substances 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003672 processing method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000002411 adverse Effects 0.000 claims 1
- 239000002699 waste material Substances 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 10
- 238000004064 recycling Methods 0.000 abstract description 2
- 235000012054 meals Nutrition 0.000 abstract 2
- 238000011084 recovery Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 240000007594 Oryza sativa Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 229960004756 ethanol Drugs 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- -1 glycoside compounds Chemical class 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000526900 Camellia oleifera Species 0.000 description 1
- 235000009024 Ceanothus sanguineus Nutrition 0.000 description 1
- 240000003553 Leptospermum scoparium Species 0.000 description 1
- 235000015459 Lycium barbarum Nutrition 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000012993 chemical processing Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000013316 zoning Methods 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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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- Fats And Perfumes (AREA)
Abstract
The invention relates to a process method for extracting grease and tea saponin from oil tea or tea seed cake.
The present invention provides a method for extracting oil and tea saponin from cake by one-step extraction by using single aqueous lower alcohol as solvent and adopting gradient leaching method. The method has the advantages of simple process, low equipment investment, high and stable extraction efficiency, and convenient recovery and recycling of the leaching solvent. The method can obtain three products of tea oil, tea saponin and detoxified residual meal, so that the cake meal can be comprehensively utilized.
Description
The invention belongs to oil plant byproduct grouts chemical processing technology.
Grouts are meant the seed of plant of theaceae oil tea or tea tree, resulting byproduct after oil is carried in the machine press for extracting juice.
Fresh grouts contain Residual oil 5～7%, glycoside compounds such as tea saponin 10～16%, and materials such as protein, starch and Mierocrystalline cellulose.Tea saponin is a kind of good natural nonionogenic tenside.Grouts do not have bitter taste after carrying most tea saponin, can be processed into feed, make it obtain comprehensive utilization.
Japanese Patent 173963(clear and 19 years) and russian patent 957910(1982) all adopt two-step approach, promptly use grease in a kind of organic solvent extraction grouts, use another kind of solvent extraction tea saponin again.Domestic prior art is all continued to use two-step process.Its shortcoming is to have used two kinds of solvents, build two cover extraction elements, so facility investment is big, and long and cost height of production cycle causes many producers only to build up the extract oil device and grouts can not be made full use of.
Domestic patent 86106634 proposes the single stage method extraction process, promptly adopts the mixed solvent leaching grouts of acetone and lower alcohol, extracts tea oil and tea saponin simultaneously.Owing to the difference of mixed solvent each component boiling point, when the heating leaching, easily produce fractionation, make leaching can internal solvent composition heterogeneity and influence extraction efficiency, also give solvent recuperation simultaneously and recycle and bring certain degree of difficulty.
The objective of the invention is to overcome above-mentioned shortcoming, use a kind of single organic solvent, adopt the gradient leaching method, grease and tea saponin all extract simultaneously in a step leaches grouts.Present method technology is simple, and facility investment is few, and extraction efficiency is high and stable, because of extracting solvent is single organic solvent, reclaims and recycles easily, and the solvent price is low, is beneficial to reduce cost.
Master operation principle of the present invention is:
Grease and tea saponin are that two class polarity differ bigger compound.Grease is at anhydrous lower alcohol (ethanol or Virahol, down together) certain solubleness is arranged, solubleness is all very little in moisture lower alcohol, and tea saponin is just opposite with grease, therefore, be difficult to make grease and tea saponin that the solubleness that meets processing requirement is all arranged with a kind of alcohol solution of concentration separately.This technology is used the lower alcohol aqueous solution of different concns, and grouts are carried out repeatedly the gradient leaching, reaches the purpose that grease in the grouts and tea saponin are all extracted.Extracting solution is through concentrating, and the lower alcohol evaporation is reclaimed, and the concentration of alcohol is very low in the concentrated solution, and grease is insoluble and layering is separated out, and very easily separates with tea saponin.
This processing method master operation is: single organic solvent gradient leaching-concentrate and divide oil-tea saponin purifying.
Accompanying drawing is this process method flow chart.
Grouts (1) are put into leaching can group (2) through the fragmentation oven dry, carry out the gradient leaching with a kind of lower alcohol aqueous solution (3), and lower alcohol can be ethanol or Virahol, and its concentration is 65～100%(V/V%, down together).The solvent strength gradient can adopt second order gradient (65～95%, 95～100%) or three ladder degree (65～85%, 85～95%, 95～100%).Otherwise gradient leaching order can be high earlier afterwards low or.In order to improve leaching efficiency, group jar (2) connects into the counter-current extraction mode.65～75 ℃ of leaching temperatures, single jar of 3～6 hours total time of leaching, the total consumption of solvent is 2～3 times (W/W) of raw material.The leaching residual dregs of rice in back (4) get the residual dregs of rice of finished product (6) through precipitation (5).Extracting solution (7) enters the enrichment process distillation and concentrates, and concentration ratio is 1/6～1/10.Recovered solvent (3) recycles.Concentrated solution is cooled to normal temperature and leaves standstill more than 8 hours, thick tea saponin slurries of primary products (12) and (9) layering of thick oil and separated.Thick oil (9) is 75～95% solvents (3) normal temperature washing (10) three times with concentration, gets product tea oil (11), and washings (3) returns leaching can (2) and makes extracting solvent.Above-mentioned operation can independently be implemented till (12).In order to obtain the refined theasapogenin product, slurry (12) is sent into deposition and purification jar (13), under stirring at normal temperature, add the precipitation agent (14) of 2～3 times of slurry weight, make the tea saponin precipitation.Precipitation agent can be acetone or ether or both mixtures.Leave standstill and solid-liquid separation, precipitation is washed once with small amount of precipitate agent (14), and drying is pulverized the back and is highly industry tea saponin powder (15).Mother liquor (16) is put into distillation tower (17) distillation and is reclaimed precipitation agent (14), recycles, and obtains the residual slurry of byproduct still (18).
A group jar number in the above-mentioned technology, the concentration gradient exponent number of solvent, single jar of leaching number of times can be according to the height that in producing grease and tea saponin extraction efficiency is required, and composite factors such as total consumption of solvent and cost are determined.
In order further to illustrate the characteristics of three master operations of this technology, a kind of with this processing method promptly is raw material with the cake of camellia oleifera seeds, and industrial alcohol is a solvent, adopts the leaching of three jars of group second order gradients to be described as follows for example:
1. gradient is leached operation
Leaching can group (2) leaching (adopting the leaching of second order gradient) is put in the broken oven dry of fresh feed (1).Add dehydrated alcohol (〉=99%) or water in the industrial alcohol and be made into the extracting solvent of two kinds of different concns: A(96.4～97.4%) and C(89～91%).C behind the first A of leaching order.Jar group (2) is made up of five jars, wherein has three jars to leach at the same time, and two jars of head and the tail are prepared jar and precipitation discharge tank for charging.The counter-current extraction jar group that connects into five jars leaching operation that circulates.
This example leaching operation main technologic parameters is:
Raw material granularity:＜4mm
Raw material water ratio:＜3%
Every jar of raw material loading amount: 1.2Kg
Extracting solvent: aqueous ethanolic solution, second order gradient
A＝96.4～97.4%，C＝89～91%
The total consumption of solvent: solvent: raw material=2: 1(W/W)
Single jar of leaching number of times: 6 times
Leaching temperature: 65～75 ℃
Leaching time: average single jar of single 1 hour
Single jar of total leaching time 6 hours
2. concentrate and divide oily operation
The extracting solution (A, C leaching liquid can merge) that comes from the leaching operation distills concentrated, reclaims＞95% and＜95% ethanol respectively in order to recycling.1/6～1/7 postcooling that is concentrated to extracting solution is to room temperature, and leaves standstill more than 8 hours.Thick grease separates with saponin slurry AUTOMATIC ZONING.Thick oil obtains faint yellow limpid tea oil for 3 times with fresh C solvent wash.Washings returns the leaching operation and makes extracting solvent.The saponin slurry can directly be sold or be dried to thick saponin powder-product or change purification procedures over to as primary products.
3. purification procedures
Last operation saponin slurry slowly adds the precipitation agent acetone of 3 times of slurry weight under the stirring at normal temperature situation, saponin is precipitated.Separate mother liquor, precipitation is washed an after drying with small amount of acetone and is pulverized, and gets the refined theasapogenin powder.Mother liquor is after acetone is reclaimed in distillation, and the residual slurry of its still is one of byproduct, can make common emulsifying agent and use.
This case process effect and quality product:
Extraction efficiency: grease＞95%, tea saponin＞85%
The residual dregs of rice (6): yield 65～70%
Fat content≤0.3%, total saponin content≤2%
Tea oil (11): yield: 〉=4.0%
Quality: light yellow transparent liquid
Thick tea saponin slurry (12): reddish-brown thick liquid, total saponin content
40～50%
Highly industry tea saponin (15): yield: 12～16%, faint yellow or sundown powder, total saponin content 〉=90%
The residual slurry of still (18): dark red brown viscous liquid
Claims (7)
1, through step leaching, from oil tea or tea waste, extract the processing method of grease and tea saponin, its craft technical feature is to make solvent with a kind of single moisture lower alcohol, adopts the gradient leaching method, a step is extracted grease and the tea saponin in the grouts.Master operation is: the gradient leaching, and----concentrate and divide oil----tea saponin purifying, wherein preceding two operations can independently be implemented.
2, by the described method of claim 1, it is characterized in that can be ethanol or Virahol as the moisture lower alcohol that extracting solvent is used, its concentration is 65～100%(V/V%, down together).
3, by the described method of claim 1, it is characterized in that taking grouts being done repeatedly the gradient leaching with the different concns lower alcohol, (concentration is 65～85% for available second order gradient (concentration is 65～95% and 95～100%) or three ladder degree, 85～95%, 95～100%), the leaching order can be earlier with the leaching of high density lower alcohol, the back lower alcohol of low concentration, otherwise or the total solvent ratio is: solvent/grouts=2～3/1(W/W).
4, by claim 1 and 3 described methods, it is characterized in that adopting adverse current jar group circulation leaching device.65～75 ℃ of leaching temperatures, single jar of single leaching time 0.5～1 hour, single jar of total leaching time 3～6 hours.Group jar number, leaching time and single jar of leaching number of times can be determined according to production requirement.
5, by the described method of claim 1, it concentrates the technical characterictic that divides oily operation is each gradient leaching liquid to be merged distillation concentrate, and concentration ratio is 1/6～1/10.Primary products tea saponin slurry separates with the grease standing demix.Grease gets tea oil three times with lower alcohol (concentration 75～95%) washing.The lower alcohol of distillation and washing usefulness returns leaching technology and recycles.
6, by the described method of claim 1, the feature of tea saponin purification procedures is to add 2～3 times of precipitation agents of its weight under the normal temperature to make tea saponin precipitation and purifying in slurry, and precipitation agent can be acetone or ether or both mixtures.
7,, it is characterized in that preceding two procedures (gradient leaching-concentrate and divide oil) can independently implement by the described method of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90101339A CN1038427C (en) | 1990-03-09 | 1990-03-09 | Method for extracting grease and tea saponin by one-step leaching cake meal |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90101339A CN1038427C (en) | 1990-03-09 | 1990-03-09 | Method for extracting grease and tea saponin by one-step leaching cake meal |
| CN 91102493 CN1054608A (en) | 1991-04-23 | 1991-04-23 | Improve the coal tar processing technology of naphthalene concentration degree |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1054788A true CN1054788A (en) | 1991-09-25 |
| CN1038427C CN1038427C (en) | 1998-05-20 |
Family
ID=25742624
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN90101339A Expired - Fee Related CN1038427C (en) | 1990-03-09 | 1990-03-09 | Method for extracting grease and tea saponin by one-step leaching cake meal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1038427C (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997029630A1 (en) * | 1996-02-14 | 1997-08-21 | Zhejiang Agricultural University | A method of preventing animals from diseases and improving immune function of animals |
| CN1042538C (en) * | 1995-10-25 | 1999-03-17 | 西南石油学院 | Method for extracting refined theasapogenin |
| CN1314703C (en) * | 2005-04-29 | 2007-05-09 | 北京林业大学 | Technique for preparing saponin of gleditschia horrida and application |
| CN100355872C (en) * | 2006-03-27 | 2007-12-19 | 郴州邦尔泰苏仙油脂有限公司 | Physical low-temperature cold-squeezing process for tea-seed oil |
| CN101974062A (en) * | 2010-10-30 | 2011-02-16 | 衢州刘家香食品有限公司 | Method for extracting tea saponin from tea seed meal |
| CN102161689A (en) * | 2011-03-14 | 2011-08-24 | 湖南文理学院 | Method for extracting tea saponin from oil-tea-cake |
| CN101550377B (en) * | 2009-05-25 | 2011-10-05 | 侯梦斌 | Preparation method of simultaneously extracting tea-seed oil and tea saponin from the kernel |
| 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 |
-
1990
- 1990-03-09 CN CN90101339A patent/CN1038427C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042538C (en) * | 1995-10-25 | 1999-03-17 | 西南石油学院 | Method for extracting refined theasapogenin |
| WO1997029630A1 (en) * | 1996-02-14 | 1997-08-21 | Zhejiang Agricultural University | A method of preventing animals from diseases and improving immune function of animals |
| US6007822A (en) * | 1996-02-14 | 1999-12-28 | Zhejian Agricultural University | Animal feed compositions and uses of triterpenoid saponin obtained from Camellia L. plants |
| CN1314703C (en) * | 2005-04-29 | 2007-05-09 | 北京林业大学 | Technique for preparing saponin of gleditschia horrida and application |
| CN100355872C (en) * | 2006-03-27 | 2007-12-19 | 郴州邦尔泰苏仙油脂有限公司 | Physical low-temperature cold-squeezing process for tea-seed oil |
| CN101550377B (en) * | 2009-05-25 | 2011-10-05 | 侯梦斌 | Preparation method of simultaneously extracting tea-seed oil and tea saponin from the kernel |
| CN101974062A (en) * | 2010-10-30 | 2011-02-16 | 衢州刘家香食品有限公司 | Method for extracting tea saponin from tea seed meal |
| CN101974062B (en) * | 2010-10-30 | 2012-10-03 | 衢州刘家香食品有限公司 | Method for extracting tea saponin from tea seed meal |
| CN102161689A (en) * | 2011-03-14 | 2011-08-24 | 湖南文理学院 | Method for extracting tea saponin from oil-tea-cake |
| CN102161689B (en) * | 2011-03-14 | 2013-02-27 | 湖南文理学院 | Method for extracting tea saponin from oil-tea-cake |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1038427C (en) | 1998-05-20 |
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