CN106281636A - A kind of extraction camellia seed oil and method of tea saponin from tea-seed pancake - Google Patents

A kind of extraction camellia seed oil and method of tea saponin from tea-seed pancake Download PDF

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CN106281636A
CN106281636A CN201610640374.9A CN201610640374A CN106281636A CN 106281636 A CN106281636 A CN 106281636A CN 201610640374 A CN201610640374 A CN 201610640374A CN 106281636 A CN106281636 A CN 106281636A
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oil
tea
alcohol water
water liquid
seed
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周玥
周建平
郭华
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Hunan Agricultural University
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
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    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • C07H1/08Separation; Purification from natural products
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    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/24Condensed ring systems having three or more rings
    • C07H15/256Polyterpene radicals
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J63/00Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
    • C07J63/008Expansion of ring D by one atom, e.g. D homo steroids
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The present invention relates to a kind of method extracting camellia seed oil and oil tea saponin from tea-seed pancake.The method includes using reverse extracting mode to extract the oils and fats in tea-seed pancake and oil tea saponin with ethanol, then sub-cooled method is used, oil tea saponin is isolated from oil tea saponin liquid, and make extracting solution be regenerated, being used as to extract camellia seed oil and the extracting section liquid of oil tea saponin, the residue obtained can be used as fertilizer next time.The oil extracting rate of the inventive method can reach more than 90%, and gained oil tea saponin content reaches more than 62%.Ethanol used in the present invention is food stage, safety non-toxic, recyclable recycling, and the renewable recycling of extracting solution used.

Description

A kind of extraction camellia seed oil and method of tea saponin from tea-seed pancake
Technical field
The invention belongs to utilization of agricultural resources utilization technical field.Relate to a kind of extraction camellia seed oil and oil tea from tea-seed pancake The method of Saponin.
Background technology
Semen Camelliae (Oil-Camellia seed) is Chinese distinctive woody oleiferous plants.Whole nation oil-producing camellia oleosa seed 60~80 throughout the year Ten thousand tons.Semen Camelliae oil content is 18%~35%.Camellia seed oil mid-oleic is between 74%~85%, higher than olive oil, and contains Having the tea polyphenols and sasanguasaponin not having in olive oil, therefore camellia seed oil is a kind of high-grade edible that can match in excellence or beauty with olive oil Oil.Containing the protein of about 8% in Semen Camelliae, wherein essential amino acids content is enriched, can be as forage protein.In Semen Camelliae Possibly together with the oil tea saponin of about 12%.Oil tea saponin is a kind of natural nonionic surfactant, is soluble in hot water and second Alcohol, is widely used in the industries such as food, medicine, daily use chemicals, pesticide.Therefore, the Main Ingredients and Appearance of Semen Camelliae has been high exploitation value The natural resources of value.
At present, China from Semen Camelliae squeezing extract camellia seed oil method mainly have two kinds, one be use high temperature steam fry with High temperature squeezing combines and extracts camellia seed oil from Semen Camelliae, and the advantage of its maximum is that oil yield is high, but High Temperature High Pressure can cause In camellia seed oil, the loss of part nutrition, makes the quality of camellia seed oil reduce, and also can there is generation carcinogen 3-4 benzo The risk of pyrene;Another kind of method is that camellia seed oil is extracted in cold pressing, steams stir-fry process, no matter cold-press is from oil tea owing to eliminating high temperature The nutritive value of seed oil, or will be better than traditional high temperature steaming in the safety of product fries and high temperature milling process, but its shortcoming It is that the oils and fats remained in tea-seed pancake is higher.That is organic solvent solvent extraction method is used to extract cold pressed cake and heat respectively Squeezing cake, the leaching oil obtained in cold pressed cake is higher than the leaching oil obtained by hot moulding method.
China produces tea-seed pancake about 30 40 ten thousand tons per year at present, remains oils and fats logical with the extraction of oil tea saponin in tea-seed pancake It is often to use two kinds of techniques to complete.The former is that to use No. six organic solvent oil (light gasoline) to extract from squeezing (squeezing in advance) cake residual Stay oils and fats.No. six organic solvent oil contain the strong carcinogens such as 3-4 benzopyrene, add that No. six organic solvent oil are in leaching process Dissolved oil tea seed cake can affect some complicated compositions of camellia seed oil quality and safety, these compositions Zhongdao leaching hair In oil, the mass ratio causing oils and fats is poor, it is necessary to could eat through strict refine.Although Extractive crudeoil can after refine To improve the quality of oils and fats, but not only result in the loss of oil, the camellia seed oil resource that waste is valuable, also can remove major part molten Functional component in oil, greatly reduces nutritive value and the health care of camellia seed oil.And No. six organic solvent oil Inflammable and explosive, easily there is security incident in production process.It addition, No. six organic solvent oil can only extract camellia seed oil, and can not be straight Connect and extract the oil tea saponin of about 15% in tea-seed pancake, and the oil tea saponin contained in camellia seed meal can have a strong impact on animal Digestive function and palatability, therefore can not use directly as feedstuff, therefore causes the waste of a large amount of quality plant albumen.Due to oil Tea saponin has bactericidal action, can destroy soil microorganism environment, and make crop can not absorb nutrition and dead, therefore can not It is directly used as fertilizer.Only as the pool-cleaning agent raising prawn.Therefore, Semen Camelliae is processed with traditional organic solvent solvent extraction method Cake, can not obtain the camellia seed oil of high-quality, can not make full use of the high-quality resources such as the camellia oleosa seed albumen in cake and oil tea saponin. The latter is to utilize hot water or ethanol the dissolution characteristics of oil tea saponin to be extracted from camellia seed meal oil tea saponin, although technique is simple Single, but equipment investment is big, and energy consumption is high.Therefore, from making full use of resource, reduce production cost and set out, at present in the urgent need to one Both safety and environmental protection, can extract again the new technique of the camellia seed oil in tea-seed pancake and oil tea saponin simultaneously.
At present, it has been reported that have about extracting the research of oils and fats and oil tea saponin from tea-seed pancake:
Zhang Hailong is (extraction purification of tea saponin and qualification in cold pressing tea seed cake, in June, 2012, Wuhan University of Technology master learned Degree thesis whole-length) in using aquiferous ethanol as digestion agent, investigated the factors such as concentration of alcohol, temperature, solid-liquid ratio, time, pH value to oil The impact of tea saponin extraction yield.On the basis of single factor experiment, have selected L16(45) orthogonal table, to concentration of alcohol, temperature Degree, solid-liquid ratio, time, pH value carry out orthogonal experiment, obtain optimum condition and are: solid-liquid ratio (w/v) is 1:3, concentration of alcohol is 70%, temperature be 55 DEG C, time 3.0h, pH value be 8.5, tea saponin yield is 11.55% with this understanding.In the method by Higher in the determining alcohol used, it is unfavorable for diffusing out from grouts of oils and fats, therefore, the extraction of not mentioned camellia seed oil.
Liu Lingling, Li Qingsong, Zeng Liang, Shen Jiafu etc. (tea saponin Study on extraction in tea seed cake, food science and technology, Vol.17,2010, No.4) in describe the extraction process of tea saponin in tea seed cake, have studied temperature, time, ethanol dense The factors such as degree, liquid-solid ratio, on the impact of tea saponin extraction ratio in tea seed cake, determine tea saponin by orthogonal test and extract Good technique is: 95% ethanol solution, and liquid-solid ratio is 16 mL/g, and Extracting temperature is 80 DEG C, and extraction time is 3 h, this Under part, tea saponin yield is 19.82%.The extraction of camellia seed oil is not extracted the most yet.
Zhang Suyang, Cui Xiaoyan, Shao Jing, Han Yong equality is in (the extraction work of tea saponin in Optimized by Orthogonal Test teaseed cake dregs Skill.Southwest University for Nationalities journal natural science edition volume 35 the 5th phase 1028-1031) in, use orthogonal experiment method, from Extraction time, temperature, concentration of alcohol, 4 factors of liquid ratio are set out and are carried out the technique extracting tea saponin from teaseed cake dregs Research. with tea saponin yield and content as index, show that the optimum extraction condition of tea saponin is: extraction time is 5h, Extraction temperature is 70 DEG C, and concentration of alcohol is 80%, and solid-liquid ratio is 9:1.
Wang Ziming is in (leaching grease and Saponin, Food technology and economic 3rd phase in 1996,37-38 from tea cake) intermediary Continue with petroleum ether and alcohol be mixed into solvent single-steeping in rotocel extractor i.e. can get inferior tea oil and Saponin starch, shorten work Skill, omits the wet dregs of rice and repeats to steam baking, save energy consumption, change the traditional method of twice extraction.The method is extracted oil used Ether is inflammable and explosive, there is production safety problem, and inferior tea oil could must eat after refine.
Yan Jie, Wu Weiming etc. (from tea seed cake extract separate tea saponin, oil engineering technology) in test determine The optimum process condition extracted is: temperature 80 DEG C, volume fraction of ethanol 80%, solid-liquid ratio: 1:25 (g/ml), extracts 4h every time, carries Taking 3 times, the response rate of tea saponin is 95.3 %.On this basis, by the extracting solution that obtains through distillation and concentration, the body of concentrated solution is made Amass 10% for extracting liquid volume, then, the isolated and purified tea soap from concentrated solution by organic solvent precipitation method and column chromatography Element.
Yang Ruijin, Zhang Wenbin, Li Qiang, the camellia seed kernel and 3~6 that Hua Xiao, Zhao Wei et al. (CN102250681A) will pulverize Weight parts water and 0.4~0. weight portion alcoholic solution are mixed into the mixture of concentration expressed in percentage by volume 10%~25%, 40~70 DEG C with Extract 0.5~2h under conditions of pH7~pH10, be then centrifuged for isolated oil phase, aqueous phase and residue phase;Residue is mutually with 5~10 After weight parts water extracts 0.5~3h under conditions of temperature 40~70 DEG C, it is centrifugally separating to obtain aqueous phase and slag phase, according to said method weighs Extraction slag phase 2-4 time again.Then all aqueous phases are merged, then add flocculant KAl (SO4)2·12Η2O removing impurity by means of precipitation matter, then After being concentrated by aqueous phase, adding 3~5 volume ethanol solution and precipitate, the liquid phase of centrifugation gained, recovered ethanol is also dehydrated It is dried to obtain inferior tea Saponin.Although oil tea once can be extracted by the method with most of oil tea saponin, but with Semen Camelliae Core is raw material, and Saponin liquid complex disposal process, energy consumption is higher.
Summary of the invention
It is contemplated that overcome the deficiencies in the prior art, it is provided that a kind of extraction camellia seed oil and oil tea soap from tea-seed pancake The method of element.
In order to achieve the above object, the technical scheme that the present invention provides is:
From tea-seed pancake, extraction camellia seed oil comprises the steps: with the method for oil tea saponin
(1) adding alcohol water liquid after being pulverized by tea-seed pancake, the addition of alcohol water liquid is 28 times of tea-seed pancake grain weight amount, preferably It is 3 3.5 times, at 50 75 DEG C, under the conditions of preferably 65 70 DEG C, extracts 2 8h, preferably 3.5 5h, more preferably 3.5 4h, is centrifugally separating to obtain A alcohol water liquid, A liquid phase and A wet slag;Obtain thick Oleum Camelliae by after liquid phase standing separation, thick Oleum Camelliae is gone Obtaining camellia seed oil after miscellaneous dehydration, oil yield is more than 90%;
(2) A wet slag alcohol water liquid is extracted 2 6h under the conditions of 50 75 DEG C, be then centrifuged for isolated B alcohol water liquid and B is wet Slag;B alcohol water liquid is back to tea-seed pancake powder and is used as extract the alcohol water liquid of tea-seed pancake powder and repeat step (1);
(3) B wet slag alcohol water liquid being extracted under the conditions of 50 75 DEG C 1 3h, then filter pressing isolated C alcohol water liquid and C are wet Slag;C alcohol water liquid is back to A wet slag and is used as extract the alcohol water liquid of A wet slag and repeat step (2);
(4) it is 25% 80% by C wet slag addition concentration of volume percent, the ethanol of preferably 35% 40%, the addition of ethanol For 16 times of C wet slag volume, under the conditions of 50 75 DEG C, extracting 1 3h, filter pressing isolated D alcohol water liquid and D wet slag;D Alcohol water liquid is back to B wet slag and is used as extract the alcohol water liquid of B wet slag and repeat step (3);
(5) D wet slag is evaporated reclaiming under the conditions of temperature 60 90 DEG C, vacuum 0.07 0.099 MPa ethanol, dehydration Dried obtain oil tea saponin content less than 2%, protein containing being 8% 12%, the camellia seed meal of preferably 10%;
(6) by A alcohol water liquid in-15 0 DEG C, under the conditions of preferably-10 DEG C, cool down 2 36h, preferably 24h, use centrifugal and filter pressing Method isolate solid phase and B liquid phase, solid phase at 70 90 DEG C, preferably 80 DEG C, under the conditions of vacuum 0.07 0.099 MPa Decompression recycling ethanol dehydration obtain inferior tea Saponin;B liquid phase is back to tea-seed pancake powder and is used as to extract the alcohol water liquid of camellia seed oil And repeat step (1).It is achieved thereby that the recycling of extracting solution, non-wastewater discharge during Ti Quing.
Fineness after described tea-seed pancake is pulverized is less than 150 μm.
The present invention is described further below:
Raw material of the present invention is cold pressing or the tea-seed pancake using traditional method to obtain, and is crushed to granularity with cracker for medicine and is less than 150 μm, meticulous meeting causes disintegrating apparatus disposal ability to decline, and crosses and slightly can affect extraction effect.Described in step of the present invention (1) Extracting solution refer to the liquid that the alcoholic solution separated from step (2) and partial regeneration water are formed.The direct shadow of addition of water Ringing the extraction effect of oil, amount of water is very few, and extracting solution viscosity is big, poor fluidity, inferior separating effect, and oil yield is the lowest, oil tea soap Element extraction ratio is low;Add water excess and can reduce the treating capacity of equipment, increase energy consumption.The present invention is preferably added to carry according to oil content in cake Take ratio is tea-seed pancake weight 3.0 4.0 times of liquid.
During step (1) is extracted, the extraction effect of oils and fats and oil tea saponin is affected bigger by temperature.The too low meeting of temperature is made Becoming camellia seed oil yield low, the extraction ratio of oil tea saponin is low, but the too high meeting of temperature makes cost increase, the oxidation of oils and fats and crude oil Color and luster is deepened.The equipment used during the most described extraction is normally used in field institutes such as food, medicine, chemical industry With the various extraction pot of arrangements for speed regulation, use the rotary evaporator that Shanghai Yarong Biochemical Instrument Plant produces in the present invention.This When inventive method is centrifuged separating, the centrifuge that used is two-phase or three-phase sedimentation (screw unloading) formula centrifuge and dish Formula centrifuge, in the present invention, the rotating speed of described sedimentation centrifuge centrifugation is 1,000 4500 revs/min.Walk at this Suddenly the extraction equipment used is current normally used sealed type explosion-proof type extraction pot, to prevent ethanol from volatilizing, increases loss, Security incident is avoided to occur.The centrifugal separation equipment used in this step is to be led in food, pharmacy, chemical industry The hermetic type equipment often used.To prevent centrifuge volatilization of ethanol when high-speed cruising.Centrifuge used in the present invention The centrifuge produced such as Anting Scientific Instrument Factory, Shanghai, rotating speed 3000 revs/min.Described in step A) the hair oil handling side that obtains Method is, adds hot water stirs's washing, then stand or use disk centrifugal separator separation roguing, then vacuum dehydration in crude oil Obtain camellia seed oil finished product.
Step (2), from the wet slag of step (1) isolated, carries with the alcohol water liquid of resulting separation from step (3) Take.It is then centrifuged for isolated liquid phase and wet slag.The step for the extraction equipment that used be the most normally used being sealed Formula explosion-proof type extraction pot, to prevent ethanol from volatilizing, increases loss, it is to avoid security incident occurs.The separation equipment used be from Scheming or pressure filter.
The wet slag of step (2) the isolated alcohol water liquid of resulting separation from step (4) is carried by step (3) Take, then filter pressing or be centrifugally separating to obtain liquid phase and wet slag.The extraction equipment used in this step and step (2) phase With, it is normally used, at the sealed type explosion-proof type extraction pot sold in the market.The step for used centrifugal point From equipment be normally used hermetic type centrifuge on food, restriction, chemical industry, or closed type pressure filter.At this Filtering equipment used in invention is to stroll the laboratory room small-sized filter press that Science and Technology Ltd. sells in Shanghai.
Step (4), in the wet slag of step (3) isolated, adds ethanol solution and extracts, and then solid phase is isolated in filter pressing With liquid phase.Filter pressing separation method is identical with step (3), is sealed explosion-proof type pressure filter.Described from step (2) to step (4) use anti-phase to leach principle, not only save ethanol consumption, also make step (1) that the oil tea saponin liquid of higher amount can be obtained.
Step (6) is to be cooled down by the oil tea saponin liquid of step (5) isolated, and oil tea saponin is molten in cold alcohol-water solution Xie Du reduces, along with continuing of low temperature, oil tea saponin crystallization.Cooling material uses the centrifugal method with filter pressing to isolate solid phase With liquid phase.Inferior tea Saponin product is obtained, new needed for the preparation steps (4) of the ethanol of recovery after solid phase dealcoholysis dehydrate Fresh alcoholic solution.The liquid phase obtained can be used as step (1) and extracts the alcohol liquid of camellia seed oil.Can realize extracting following of process water Ring uses, non-wastewater discharge.
Compared with prior art, the invention have the benefit that
1, the inventive method utilizes alcohol-water solution to extract camellia seed oil and oil tea saponin from tea-seed pancake, with elder generation before simultaneously Leach with organic solvent and extract oils and fats, then from tea-seed pancake, extracts tea saponin with water or alcohol and compare, decrease abstraction process with The input of equipment, reduces production cost, meanwhile, improves nutritive value and the safety of proposed camellia seed oil.
2, in the inventive method, in step (2) to step (4) all employing ethanol solution as extracting solution, and use inverse From residue, oil tea saponin is extracted to extracting mode.Not only reduce the consumption of alcohol, and make step A can obtain the oil of high concentration Tea saponin liquid.
3, the inventive method in step (6) by the oil tea saponin liquid of step (1) institute isolated by be cooled to 0 DEG C with Under, make oil tea saponin because dissolubility declines Precipitation, and by filtering or centrifugal method isolated higher concentration Oil tea saponin slurry and alcohol water liquid, be both enriched oil tea saponin, again for obtaining the oil tea saponin of higher purity and further comprehensive utilization Condition is created with composition therein.The concentration of oil tea saponin is combined with the regeneration of alcoholic solution, with traditional method ratio Relatively, it is greatly saved processing cost.
4, in the inventive method, in step (6), the alcohol water liquid of isolated can be used as in lower whorl step (1) from Semen Camelliae Cake extracts the extracting solution of camellia seed oil and oil tea saponin, is truly realized the purpose of extraction process non-wastewater discharge.
In a word, the present invention uses reverse extracting mode to extract the oils and fats in tea-seed pancake and oil tea saponin with ethanol, so Rear employing sub-cooled method, isolates oil tea saponin from oil tea saponin liquid, and makes extracting solution be regenerated, and is used as to carry next time Taking the extracting section liquid of camellia seed oil and oil tea saponin, the residue obtained can be used as fertilizer.The oil extracting rate of the inventive method is permissible Reaching more than 90%, the oil tea saponin response rate reaches more than 90%.Ethanol used in the present invention is food stage, and safety non-toxic can Recycle and reuse, and extracting solution used is renewable follows.
Detailed description of the invention
Embodiment 1
From tea-seed pancake, extraction camellia seed oil comprises the steps: with the method for oil tea saponin
(1) adding alcohol water liquid after being pulverized by tea-seed pancake, the addition of alcohol water liquid is 28 times of tea-seed pancake grain weight amount, preferably It is 3 3.5 times, at 50 75 DEG C, under the conditions of preferably 65 70 DEG C, extracts 2 8h, preferably 3.5 5h, more preferably 3.5 4h, is centrifugally separating to obtain A alcohol water liquid, A liquid phase and A wet slag;Obtain thick Oleum Camelliae by after liquid phase standing separation, thick Oleum Camelliae is gone Obtaining camellia seed oil after miscellaneous dehydration, oil yield is more than 90%;
(2) A wet slag alcohol water liquid is extracted 2 6h under the conditions of 50 75 DEG C, be then centrifuged for isolated B alcohol water liquid and B is wet Slag;B alcohol water liquid is back to tea-seed pancake powder and is used as extract the alcohol water liquid of tea-seed pancake powder and repeat step (1);
(3) B wet slag alcohol water liquid being extracted under the conditions of 50 75 DEG C 1 3h, then filter pressing isolated C alcohol water liquid and C are wet Slag;C alcohol water liquid is back to A wet slag and is used as extract the alcohol water liquid of A wet slag and repeat step (2);
(4) it is 25% 80% by C wet slag addition concentration of volume percent, the ethanol of preferably 35% 40%, the addition of ethanol For 16 times of C wet slag volume, under the conditions of 50 75 DEG C, extracting 1 3h, filter pressing isolated D alcohol water liquid and D wet slag;D Alcohol water liquid is back to B wet slag and is used as extract the alcohol water liquid of B wet slag and repeat step (3);
(5) D wet slag is evaporated reclaiming under the conditions of temperature 60 90 DEG C, vacuum 0.07 0.099 MPa ethanol, dehydration Dried obtain oil tea saponin content less than 2%, protein containing being 8% 12%, the camellia seed meal of preferably 10%;
(6) by A alcohol water liquid in-15 0 DEG C, under the conditions of preferably-10 DEG C, cool down 2 36h, preferably 24h, use centrifugal and filter pressing Method isolate solid phase and B liquid phase, solid phase at 70 90 DEG C, preferably 80 DEG C, under the conditions of vacuum 0.07 0.099 MPa Decompression recycling ethanol dehydration obtain inferior tea Saponin;B liquid phase is back to tea-seed pancake powder and is used as to extract the alcohol water of tea-seed pancake powder Liquid also repeats step (1).It is achieved thereby that the recycling of extracting solution, non-wastewater discharge during Ti Quing.
Fineness after described tea-seed pancake is pulverized is less than 150 μm.
Implementation result: tea-seed pancake oil content 10.15%, after implementing said method, obtains camellia seed oil 9.19g/100g, oil Oleum Camelliae extraction ratio 90.54%, camellia seed meal feedstuff 59.5g/100g, wherein protein content 10.13%;Obtain inferior tea Saponin 25.63 g/100g, wherein oil tea saponin content 64.17%.

Claims (2)

1. the method extracting camellia seed oil and oil tea saponin from tea-seed pancake, it is characterised in that described method include as Lower step:
(1) adding alcohol water liquid after being pulverized by tea-seed pancake, the addition of alcohol water liquid is 28 times of tea-seed pancake grain weight amount, Extract 2 8h under the conditions of 50 75 DEG C, be centrifugally separating to obtain A liquid phase and A wet slag;Inferior tea seed is obtained after A liquid phase standing separation Oil, obtains camellia seed oil after thick Oleum Camelliae roguing being dehydrated, oil yield is more than 90%;
(2) A wet slag alcohol water liquid is extracted 2 6h under the conditions of 50 75 DEG C, be then centrifuged for isolated B alcohol water liquid and B is wet Slag;B alcohol water liquid is back to tea-seed pancake powder and is used as extract the alcohol water liquid of tea-seed pancake powder and repeat step (1);
(3) B wet slag alcohol water liquid being extracted under the conditions of 50 75 DEG C 1 3h, then filter pressing isolated C alcohol water liquid and C are wet Slag;C alcohol water liquid is back to A wet slag and is used as extract the alcohol water liquid of A wet slag and repeat step (2);
(4) by the ethanol that C wet slag addition concentration of volume percent is 25% 80%, the addition of ethanol is the 1 of C wet slag volume 6 times, under the conditions of 50 75 DEG C, extracting 1 3h, filter pressing isolated D alcohol water liquid and D wet slag;D alcohol water liquid is back to B wet slag It is used as extract the alcohol water liquid of B wet slag and repeat step (3);
(5) D wet slag is evaporated reclaiming under the conditions of temperature 60 90 DEG C, vacuum 0.07 0.099 MPa ethanol, dehydration Dried obtain oil tea saponin content less than 2%, protein is containing the camellia seed meal being 8% 12%;
(6) A alcohol water liquid is cooled down under the conditions of-15 0 DEG C 2 36h, use the centrifugal method with filter pressing to isolate solid phase and B Liquid phase, solid phase at 70 90 DEG C, preferably 80 DEG C, decompression recycling ethanol being dehydrated under the conditions of vacuum 0.07 0.099 MPa Obtain inferior tea Saponin;B liquid phase is back to tea-seed pancake powder and is used as extract the alcohol water liquid of camellia seed oil and repeat step (1).
2. the method for claim 1, it is characterised in that the fineness after described tea-seed pancake is pulverized is less than 150 μm.
CN201610640374.9A 2016-08-08 2016-08-08 A kind of extraction camellia seed oil and method of tea saponin from tea-seed pancake Pending CN106281636A (en)

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CN108329991A (en) * 2018-02-13 2018-07-27 江南大学 A kind of method of water-borne method extraction camellia seed oil
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