CN103070364A - Liquid and powder persimmon tannin and separation and extraction process thereof - Google Patents

Liquid and powder persimmon tannin and separation and extraction process thereof Download PDF

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CN103070364A
CN103070364A CN2013100603470A CN201310060347A CN103070364A CN 103070364 A CN103070364 A CN 103070364A CN 2013100603470 A CN2013100603470 A CN 2013100603470A CN 201310060347 A CN201310060347 A CN 201310060347A CN 103070364 A CN103070364 A CN 103070364A
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persimmon
tannin
juice
fermentation
alcohol
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敖常伟
辛国贤
凌敏
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Heibei Agricultural University
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Heibei Agricultural University
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Abstract

The invention relates to liquid or powder persimmon tannin from green persimmon and a corresponding extraction and separation process technology thereof. A liquid persimmon tannin is obtained by selecting persimmon raw materials, juicing, fermenting, removing alcohol, ageing, removing impurities and the like, or persimmon tannin powder is obtained by drying and crushing, and the tannin content in the product is 2-99%. The invention overcomes the defects of the prior persimmon tannin product and process, respectively processes according to the characteristics of different components in the persimmon, and provides a series of effective separation and purification extraction processes for persimmon tannin, which adopt yeast fermentation to convert sugar in persimmon juice into alcohol, evaporate and separate the alcohol in vacuum, promote the polymerization of the persimmon tannin into high molecules by aging, filter and remove micromolecular peculiar smell substances such as acetic acid and the like. The production process of the persimmon fruit powder does not add any chemical reagent, the final product is a pure natural persimmon fruit component, and the persimmon fruit powder can be used as a clarifying agent of beer and wine, an additive of cosmetics, an additive of various deodorizers, a sewage treatment agent, an adsorbent of precious metals and the like, and has wide market prospect.

Description

A kind of liquid state and pulvis persimmon tannin and separation-extraction technology thereof
Technical field
The present invention relates to a kind of liquid state or pulvis persimmon tannin and corresponding extraction and separation process technology thereof that derives from blue or green persimmon.
Background technology
Approximately 2,560,000 tons of the annual persimmon total outputs in the whole world, wherein the output of China has 1,830,000 tons (FAO, 2005).Because the not anti-storage characteristic of persimmon is very short during eating raw, and other deep processed product kind of persimmon is limited, be processed into the lower dried persimmon of added value such as part, persimmon wine, beverage etc., a large amount of persimmons are wasted.China is the original producton location of persimmon, and a plurality of different cultivars are arranged, and most of kinds all contain more tannin, feels obvious astringent taste when causing immature persimmon entrance.Persimmon is the highest a kind of fruit of tannin content, and tannin content is up to more than 2% of persimmon fresh weight.Persimmon has the shedding phase twice before ripe in addition, and the shedding amount is very large, accounts for 20% of persimmon result quantities.Because it is high to fall the Chinese olive tannin content, distinguishes the flavor of very puckery inedibility.But can be used as the raw material that extracts tannin.Tannin has the activity with protein, polysaccharide, alkaloid, a lot of metal ions and the reaction of low molecular volatile substances, also have anti-oxidant, remove free radical and the function such as antibiotic.Its application prospect and wide scope.The tannin of present different plant origins extracts and is applied as aspects such as deodorant, cosmetic additive agents at drinks processing, sewage disposal, precious metal, in the past few years, the applicant has carried out fruitful research to the characteristic of persimmon tannin with extracting to separate.Persimmon tannin belongs to typical polyphenol compound, the outer research of Present Domestic finds that the polyphenol compound in the general plant mainly is present in the plant with free state or in conjunction with the attitude mode, tannin in the persimmon is no exception, in the different maturity periods of persimmon, persimmon tannin also have free state and in conjunction with two kinds of forms of attitude.Free state persimmon tannin molecular weight, solvable at solution such as water, easily combine with protein, can make our tongue feel obvious astringent taste, the free state tannin also has certain antibiotic and sterilizing ability.In the immature persimmons such as blue or green persimmon mainly take the free state tannin as main.The existence of the free state tannin in the blue or green persimmon is a kind of self-protection mechanism of persimmon, can prevent that insect and disease are to the infringement of persimmon.In conjunction with the attitude tannin general with the persimmon cell membrane on cellulose, hemicellulose, lignin and pectin etc. combine, perhaps self-polymerization forms high polymer, water insoluble solution and other solvents, our tongue can not be felt its existence.In the persimmon of ripe later stage of persimmon and deliquescing slaking mainly take in conjunction with the attitude tannin as main.The free state tannin content can adopt several phenols content assaying methods commonly used directly to measure, and could measure after becoming the free state tannin and measure to be hydrolyzed to it in conjunction with the attitude tannin content.Domestic persimmon tannin extraction process mainly is to adopt the variable concentrations organic solvent of adjusting the pH value to extract.The employings such as Gu Haifeng contain the absolute methanol of 1%HCL as the tannin in the extractant extraction persimmon; The scholar who also has adopts acetone as the extraction solvent of tannin in the Pericarpium Kaki.These procedures are loaded down with trivial details, and add the pollution that a large amount of chemical reagent cause tannin, and be not suitable for large batch of production, common organic solvents can only will extract than the small-molecular weight tannin in the persimmon in addition, the tannin of a large amount of higher degrees of polymerization (such as molecular weight greater than more than 1000) almost can not dissolve in organic solvent, thereby can not be extracted.Cause a large amount of wastes of raw material.Adopt blue or green persimmon or acerbity-removing persimmon through freeze drying in the invention disclosed such as CN101328194A and the CN1759697 patent, ultramicro grinding obtains the ultra micro persimmon powder or through enzymolysis, filters, and makes persimmon powder after the freeze drying.In this class persimmon powder product otherwise tannin content is lower, otherwise the recovery rate of tannin is low, perhaps complex process, thus need the participation etc. of multiple biological enzyme formulation to increase production cost, be difficult for industrialization promotion and application.The present invention processes respectively according to the characteristic of the different component in the persimmon, has proposed a kind of comparatively easy persimmon tannin extraction process, has effectively overcome the weak point of above-mentioned technique.
Summary of the invention
The technical problem to be solved in the present invention is: determine the suitable persimmon Chinese olive collecting period, adopt rational production technology to separate other non-tannis composition of removing in the persimmon, obtain liquid state or the pressed powder All Pure Nature persimmon tannin product of different extent of polymerizations.
Constituted mode of the present invention is: by the persimmon raw material is selected, squeezed the juice, the processes such as fermentation, dealcoholization, ageing, impurity elimination obtain a kind of liquid persimmon tannin or again drying, the persimmon tannin pulvis that obtains after pulverizing, tannin content is between 2-99% in this product.
The technical solution adopted in the present invention is: take the main puckery persimmon kind of China such as Mopan Persimmon, OX-heart persimmon and lotus flower persimmon etc. as extracting the raw material of tannin.In the persimmon growth course, measure tannin content in the blue or green persimmon, pluck in the time of near free state tannin content in the persimmon reaches the peak; The material such as insoluble crude fibres such as the persimmon of plucking really cleaned, went the base of a fruit, fragmentation, squeezes the juice, filtration etc. separates persimmon pericarp, slag is obtained persimmon juice.Owing to except tannin, also having the main soluble component such as sugar, acid and pectin in this juice, be alcohol by adopting fermentation mode with the thorough decomposition and inversion of carbohydrate, yeast is killed in the complete rear heating of fermenting, remove the coarse granules such as yeast by suitable aperture filter-cloth filtering, adopt the cryogenic vacuum separated to obtain alcohol.Juice behind the dealcoholization is processed by the ageing of certain hour, tannin in the juice progressively polymerization polymeric form that forms HMW freezes the shape body, thereby adopts and filter and clean the liquid persimmon tannin that some smell components that produce in the little molecule acids composition of getting rid of solubility and fermentation, the traditional aging process obtain frees from extraneous odour freezing shape body polymer.Perhaps the tanning matter with liquid state carries out processed by spray-drying, low-temperature vacuum drying or freeze drying, and finally obtains solid tannin powder.Adopt conventional tannin assay method, the tannin content scope is between 2-99% in this liquid state or the pressed powder attitude product.
Specific implementation process of the present invention is as follows:
1, raw material tannin analysis and gathering: ripe previous month of persimmon, tannin content in measuring persimmon in 3 to 5 days is prepared fruit picking and is collected raw material when tannin content approaches or arrives 2%.Can adopt Forint phenol method to measure tannin content in the persimmon, be the best time of picking of persimmon thereby determine to contain in the persimmon growth course free state tannin the abundantest period;
2, persimmon juice preparation: the Chinese olive raw material of results needs in the processing of squeezing the juice as early as possible in 2 to 3 days.Persimmon adopts stainless steel knife to dig out top base of fruit part after cleaning, and broken rear employing screw juicer squeezes out the juice in the raw material, and juice can carry out filtering and impurity removing through 60 order filter clothes again to be processed;
3, fermentation desugar: persimmon juice can be decomposed into alcohol with sugar by spontaneous fermentation or artificial fermentation's mode and reach the desugar processing.Adopt under the spontaneous fermentation mode, persimmon juice is directly deposited in the inherent room temperature bottom fermentation of generic container without high-temperature process, adopts saccharometer to measure soluble solid content in the juice, can stop fermentation when soluble solid content is lower than 2%.General fermentation time is about 7 to 10 days.Adopt under artificial fermentation's mode, need the juice heating of filtering is cooled to room temperature after the sterilization more than 60 ℃, juice inoculation saccharomycete (comprising the saccharomycete of commercially available various active dry yeast or separation cultivation etc.) is in 30 ℃ of left and right sides temperature bottom fermentations until soluble solid content stops fermentation after being lower than below 2%.Killed yeast in 5 minutes and remove yeast and partial suspended thing etc. by 80-100 order filter-cloth filtering through nature or the complete 60 ℃ of heating of persimmon juice of artificial fermentation;
4, zymotic fluid alcohol separates: the compositions such as alcohol that fermentation generates in the juice separate recovered alcohol in the Vacuum Concentration mode being lower than under 50 ℃ of temperature; The alcohol residue amount is lower than 0.5% in the zymotic fluid after the evaporation;
5, ageing: the persimmon juice sealing lucifuge that removes alcohol is stored in the dark environment 6-24 month, and the mutual polymerization of persimmon tannin forms macromolecule and fetters the part hydrone and forms and freezes the shape body;
6, filtering and removing peculiar smell: the shape body that freezes that forms after adopting 100-200 order filter cloth that ageing is finished filters, and clean with clear water, making high molecular persimmon tannin is that the main shape thing that freezes is retained in the filter cloth, and hazel semisolid or liquid persimmon tannin are finally obtained in the separated removals of composition such as little molecule solubility acids;
7, drying: the persimmon tannin of liquid towards can directly adopt the modes such as spray-drying, low-temperature vacuum drying and freeze drying and pulverizing to obtain solid tannin powder.
The raw materials used Chinese olive before the persimmon prematurity of the present invention is as main, because of the region of China persimmon cultivation wider, there is larger difference the suitable collecting period according to the region difference, begin all can pluck to the late September in the north from the July in zone, south, can judge by measuring the bear fruit content of later stage free state tannin of persimmon, as adopt Forint phenol method to measure, general tannin content all can be plucked when 1.5-2% is above, too early or spend evening and pluck and tannin can not effectively be extracted and cause wastage of material.The fruit that can not become the commodity fruit for the shedding of fruit thinning phase, malformed fruit, fruitlet etc. also can use, can be relatively on the low side for the tannin recovery rate in this class fruit.Process of producing product of the present invention does not add any chemical reagent, persimmon composition for pure natural, can be used as beer, fining agent vinous, the additive of cosmetics, various deodorants additive, sewage-treating agent, precious metal adsorbent etc., market prospects are wide.
The specific embodiment:
Embodiment 1: produce blue or green persimmon as raw material production solid, powdery persimmon tannin take the Hebei Wild jujube in Taihang Mountain Area:
(1) about September 20, gathered the persimmon Chinese olive, in fruit washing machine, rinse well with running water and drain away the water, excise base of fruit with stainless steel knife, be cut into small pieces and drop into squeezing collection juice in the spiral juice extractor, remaining pomace squeezes after adding a small amount of water mixing again, merges the juice of twice squeezing;
(2) the persimmon juice behind 60 order filter-cloth filterings places 60 ℃ of heating of jacketed pan sterilization in 10 minutes, then pour cool to room temperature in the fermentation tank into, adding 0.05% grape wine by the weighing scale of persimmon juice ferments with active dry yeast, fermented about 5 days and measure the zymotic fluid soluble solid content, heating zymotic fluid to 60 ℃ when content is lower than 2%, be incubated 5 minutes and stop fermentation, and adopt while hot 80 order filter cloth centrifugal filtrations to remove the insoluble matters such as yeast;
(3) filtrate imports in the vacuum concentration pot and is being lower than appropriateness evaporation and collection alcohol under 50 ℃ of temperature, and the alcohol of evaporation and steam vapour amount are about 10% of original volume;
(4) separate juice behind the alcohol and placed in the food grade plastic bucket ageing of sealing lucifuge 8 months, that treats that persimmon tannin fully forms high molecular polymer freezes the shape body;
(5) filter and clean to remove solubility acids and little molecule smell component with 150 order filter clothes to freezing the shape body;
(6) the persimmon tannin solution after cleaning spreads disc thickness 3cm ,-40 ℃ freezing 10 hours, under 65Pa vacuum, 40 ℃ of dryings 25 hours.Then unload dish, beat powder, be packaged to be the powdery persimmon tannin.
Embodiment 2: the cull fruit that falls take the Hebei Wild jujube in Taihang Mountain Area persimmon fruit thinning phase is produced liquid persimmon tannin as raw material:
(1) collects scattered persimmon cull fruit of mid or late August, clean, go the base of a fruit, obtain juice after squeezing the juice;
(2) juice places and adopts the spontaneous fermentation mode to ferment about 10 days in the fermentation tank, measure the soluble solid content of zymotic fluid, 60 ℃ of zymotic fluids of heating when content is lower than 2% be incubateds 5 minutes and stop fermenting, and use while hot the insoluble matter such as 80 order filter cloth centrifugal filtration separated yeast;
(3) filtrate imports in the vacuum concentration pot and is being lower than appropriateness evaporation and collection alcohol under 50 ℃ of temperature, and the alcohol of evaporation and steam vapour amount are about 10% of original volume;
(4) separate juice behind the alcohol and placed in the food grade plastic bucket ageing of sealing lucifuge 8 months, that treats that persimmon tannin fully forms high molecular polymer freezes the shape body;
(5) filter and clean to remove solubility acids and little molecule smell component with 150 order filter clothes to freezing the shape body.Quantitatively bottling or pack, are incubated sterilization in 5 minutes and obtain liquid persimmon tannin by 60 ℃.

Claims (7)

1. a liquid state or solid powder attitude persimmon tannin product, it is characterized in that: by the persimmon raw material is selected, squeezed the juice, the processes such as fermentation, dealcoholization, ageing, impurity elimination obtain a kind of liquid persimmon tannin or again drying, the persimmon tannin pulvis that obtains after pulverizing, tannin content is between 2-99% in this product.
2. at persimmon tannin according to claim 1, its production technology is characterised in that: take the main puckery persimmon kind of China such as Mopan Persimmon, etc. as extracting the raw material of tannin; Select to pluck when the free state tannin reaches the peak in the fruit; The material such as insoluble crude fibres such as the persimmon of plucking really cleaned, went the base of a fruit, fragmentation, squeezes the juice, filtration etc. separates persimmon pericarp, slag is obtained persimmon juice; Owing to except tannin, also having the main soluble component such as sugar, acid and pectin in this juice, be alcohol by adopting the saccharomycetes to make fermentation mode with the thorough decomposition and inversion of carbohydrate content, yeast is killed in the complete rear heating of fermenting, remove the coarse granules such as yeast by suitable aperture filter-cloth filtering, adopt the cryogenic vacuum separated to obtain alcohol; Juice behind the dealcoholization is processed by the ageing of certain hour, tannin in the juice progressively polymerization polymeric form that forms HMW freezes the shape body, thereby adopts and filter and clean the liquid persimmon tannin that some smell components that produce in the little molecule acids composition of getting rid of solubility and fermentation, the traditional aging process obtain frees from extraneous odour freezing shape body polymer; Perhaps the tanning matter with liquid state obtains solid tannin powder by spray-drying, low-temperature vacuum drying and freeze drying etc. and after pulverizing.
3. persimmon according to claim 2 is really plucked requirement, it is characterized in that: ripe previous month of persimmon, and tannin content in persimmon of 3 to 5 days mensuration, the preparation fruit picking is collected and is processed raw material when tannin content approaches or arrives 2%.
4. fermentation process technique according to claim 2 is characterized in that: squeezing gained persimmon juice can be decomposed into alcohol with sugar by spontaneous fermentation or artificial fermentation's mode and reach desugar and process; Adopt under the spontaneous fermentation mode, persimmon juice is directly deposited in the inherent room temperature bottom fermentation of generic container without high-temperature process, adopts saccharometer to measure soluble solid content in the juice, can stop fermentation when soluble solid content is lower than 2%; General fermentation time is about 7 to 10 days; Adopt under artificial fermentation's mode, need be cooled to room temperature after the sterilization more than 50-60 ℃ to the juice heating of filtering, juice inoculation saccharomycete (comprising the saccharomycete of commercially available various active dry yeast or separation cultivation etc.) ferments in 20-35 ℃ of temperature range until soluble solid content stops fermenting after being lower than below 2%; Killed yeast in 5 minutes and remove yeast and partial suspended thing etc. by 80-100 order filter-cloth filtering through nature or the complete 60 ℃ of heating of persimmon juice of artificial fermentation.
5. zymotic fluid alcohol separating technology according to claim 2, it is characterized in that: the compositions such as alcohol that generated by sugar fermentation in the persimmon juice separate and recovered alcohol in the Vacuum Concentration mode in vacuum concentration pot or other vacuum evaporator being lower than under 50 ℃ of temperature, make that alcoholic strength is lower than 0.5% in the final zymotic fluid.
6. zymotic fluid ageing according to claim 2 and impurity removal process is characterized in that: the persimmon juice sealing lucifuge that removes alcohol is stored in the dark environment 6-24 month, and the mutual polymerization of persimmon tannin forms macromolecule and fetters the part hydrone and forms and freezes the shape body; The shape body that freezes that forms after adopting 100-200 order filter cloth that ageing is finished filters, and clean with clear water, making high molecular persimmon tannin is that the main shape thing that freezes is retained in the filter cloth, and free from extraneous odour, hazel semisolid or liquid persimmon tannin are finally obtained in the separated removals of composition such as little molecule solubility acids.
7. drying process according to claim 2 is characterized in that: the persimmon tannin of liquid towards can directly adopt spray-drying or the modes such as low-temperature vacuum drying or freeze drying to carry out that drying and dehydrating is processed and the final solid tannin powder that obtains.
CN2013100603470A 2013-02-27 2013-02-27 Liquid and powder persimmon tannin and separation and extraction process thereof Pending CN103070364A (en)

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CN103525610A (en) * 2013-10-31 2014-01-22 赫忠友 Red grape spirit production technology
CN104013557A (en) * 2014-06-24 2014-09-03 刘小峰 Application of persimmon extract freeze-dried powder as deodorant functional material
CN104664377A (en) * 2015-02-07 2015-06-03 陕西学前师范学院 Preparation method for health care sugar-free natural product powder
CN105581217A (en) * 2015-12-14 2016-05-18 山东省果树研究所 Method for removing arsenic in apple juice
CN106008616A (en) * 2016-07-05 2016-10-12 深圳市美漾无华生物科技有限公司 Method for extracting persimmon tannin from persimmons
CN106380495A (en) * 2016-08-15 2017-02-08 中国农业科学院农产品加工研究所 Method for continuous extraction of tannin and pectin from persimmon peel
CN107779371A (en) * 2017-11-09 2018-03-09 江南大学 Specificity removes the method for dimerization alpha amylase inhibitor and class avenin in yellow rice wine
CN109568993A (en) * 2018-11-05 2019-04-05 广州柿宝生物科技有限公司 Dehydration and drying process of persimmon tannin concentrated solution
CN110314652A (en) * 2018-03-29 2019-10-11 河北农业大学 Method for adsorbing and recovering precious metal gold by using persimmon residues
CN110509384A (en) * 2018-05-21 2019-11-29 河北农业大学 Green persimmon extraction product for controlling formaldehyde release
CN112972742A (en) * 2021-02-23 2021-06-18 浙江思享家环保科技有限公司 Environment-friendly plant composite extract for removing formaldehyde, decomposing peculiar smell and sterilizing and preparation thereof
CN115300236A (en) * 2022-07-05 2022-11-08 深圳全棉时代科技有限公司 Odor-eliminating and odor-inhibiting adult absorbent product and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN103525610B (en) * 2013-10-31 2015-03-25 赫忠友 Red grape spirit production technology
CN103525610A (en) * 2013-10-31 2014-01-22 赫忠友 Red grape spirit production technology
CN104013557A (en) * 2014-06-24 2014-09-03 刘小峰 Application of persimmon extract freeze-dried powder as deodorant functional material
CN104664377A (en) * 2015-02-07 2015-06-03 陕西学前师范学院 Preparation method for health care sugar-free natural product powder
CN105581217A (en) * 2015-12-14 2016-05-18 山东省果树研究所 Method for removing arsenic in apple juice
CN105581217B (en) * 2015-12-14 2018-02-13 山东省果树研究所 A kind of method of arsenic in removal cider
CN106008616A (en) * 2016-07-05 2016-10-12 深圳市美漾无华生物科技有限公司 Method for extracting persimmon tannin from persimmons
CN106008616B (en) * 2016-07-05 2018-08-07 深圳市美漾无华生物科技有限公司 A method of extracting persimmon tannin from persimmon
CN106380495B (en) * 2016-08-15 2019-05-21 中国农业科学院农产品加工研究所 The method of tannin and pectin is continuously extracted from Pericarpium Kaki
CN106380495A (en) * 2016-08-15 2017-02-08 中国农业科学院农产品加工研究所 Method for continuous extraction of tannin and pectin from persimmon peel
CN107779371A (en) * 2017-11-09 2018-03-09 江南大学 Specificity removes the method for dimerization alpha amylase inhibitor and class avenin in yellow rice wine
CN110314652A (en) * 2018-03-29 2019-10-11 河北农业大学 Method for adsorbing and recovering precious metal gold by using persimmon residues
CN110509384A (en) * 2018-05-21 2019-11-29 河北农业大学 Green persimmon extraction product for controlling formaldehyde release
CN110509384B (en) * 2018-05-21 2022-03-22 河北农业大学 Green persimmon extraction product for controlling formaldehyde release
CN109568993A (en) * 2018-11-05 2019-04-05 广州柿宝生物科技有限公司 Dehydration and drying process of persimmon tannin concentrated solution
CN112972742A (en) * 2021-02-23 2021-06-18 浙江思享家环保科技有限公司 Environment-friendly plant composite extract for removing formaldehyde, decomposing peculiar smell and sterilizing and preparation thereof
CN115300236A (en) * 2022-07-05 2022-11-08 深圳全棉时代科技有限公司 Odor-eliminating and odor-inhibiting adult absorbent product and preparation method thereof

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Application publication date: 20130501