CN1824748A - Method of producing low alcohol or alcohol less raw juice formentation alcoholic beverage using osmotic gasification-rectification coupling method - Google Patents
Method of producing low alcohol or alcohol less raw juice formentation alcoholic beverage using osmotic gasification-rectification coupling method Download PDFInfo
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- Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to a method for producing low-alcohol or alcohol-free raw juice fermented alcoholic beverage by utilizing pervaporation-rectification coupling process. Said method is characterized by including the following steps: (1), utilizing pervaporation membrane component to make dealcoholization separation of raw liquor; (2), utilizing rectification tower to make fine separation of raw liquor; and (3), adding distilled water and making final modification so as to obtain low-alcohol or alcohol-free raw juice fermented alcoholic beverage with good flavour and taste.
Description
Technical field
The present invention relates to the production method of low alcohol or non-alcohol beverage from raw juice fermented wine, specifically, be that a kind of infiltration vaporization membrane module and multi-stage condensing-many side lines extraction rectifying tower (hereinafter to be referred as PV-MCMSD) coupling technique efficiently and directionally of utilizing removes ethanol in the beverage from raw juice fermented wine and other objectionable impurities, carry out the purpose that has of each fragrant substance in the former wine simultaneously and separate and reorganization, to produce low alcohol or not have the method for the novel alcohol product of alcohol.
Background technology
(1) origin of not having alcohol and hanging down alcohol beverage from raw juice fermented wine
Beverage from raw juice fermented wine mainly comprises beer, fruit wine (grape wine, hard cider, Hawthorn Fruit Wine, plum wine, Yangtao wine and other fruit juice fermentation brewing wine etc.) and yellow rice wine, occupies very large portion in whole beverage market.Ethanol content is between 3～5% (w/w) in the beer of common former wheat juice fermentative production, ethanol content is at 9～10% (w/w) or 11～12% (v/v) in the grape wine of former Sucus Vitis viniferae fermentative production, and glutinous rice adds in the yellow rice wine of distiller's yeast fermentative production ethanol content then between 15～25% (w/w).In recent years, along with the raising of people's living standard and the enhancing of health perception, and the constraint of some job specification, nothing alcohol and low pure alcohol beverage more and more are welcomed by the general public and like.This class beverage is owing to reduced the content of alcohol, reduced the harm of alcohol to human body, kept simultaneously its original color and luster and local flavor to a great extent, and contain the human body various amino acids necessary, polyphenolic substance and trace element, low in calories, aid digestion, reduce fatty deposits in the blood vessel, the demand that meets the green health propensity to consume is particularly suitable for all kinds of crowds' such as Ms, old man, children, driver, disease patient and fashion youth needs.Under above background, especially American-European in the world western developed countries, good nothing alcohol reaches the market outlook of low pure alcohol beverage, actively develops and produce the product of this respect, has obtained gratifying achievement.
(2) definition of alcohol-free or low alcohol alcoholic beverage
Present domestic relevant department and brewage worker, can be summarized as follows the basic definition that does not have alcohol and low alcohol: alcohol-free beer is that the alcohol volume fraction is at a kind of beer drink below 0.5%.Its starting material are identical with common traditional beer, and base style approaches common traditional beer, but are a kind of novel beers with certain characteristic.Low alcohol beer is that the alcohol volume fraction is 0.5%～2.5% novel beer.Its used starting material is identical with ordinary beer, and style approaches ordinary beer, and some product has certain characteristic.
Played clearly definition in the enforcement " Chinese grape wine technical specifications " on January 1st, 2003: low-alcohol wine is meant employing fresh grape or Sucus Vitis viniferae through all or part of fermentation, through the alcoholic drink that special warfare processes, and contained wine degree 1%-7% (v/v); Alcohol-Free wine is meant and adopts fresh grape or Sucus Vitis viniferae through all or part of fermentation that through the alcoholic drink that the special warfare dealcoholysis processes, contained wine degree is no more than 1% (v/v).
As for the definition of alcohol-free or low alcohol yellow rice wine, country does not still have special industry standard regulation at present.We think, ethanol content is lower than 10% yellow rice wine can think low-alcohol yellow rice wine, and the yellow rice wine that is lower than 1% ethanol content can think not have alcohol yellow rice wine.
(3) present nothing alcohol reaches the production technology of hanging down alcohol beverage from raw juice fermented wine
At present, produce the method for not having alcohol or low pure alcohol drink in the world and mainly contain two classes.One class is to reduce the ethanol content that generates in the system wine fermentation process with the method for restricted fermentation, and another kind of is to make after the alcoholic beverage dealcoholization again.Last class methods mainly comprise single-minded yeast fermentation, change Mashing process and change zymotechnique etc., its need not be extra facility investment, but complex technical process, and when restriction ethanol generates, also limit the generation of other flavour substancess in the wine to a great extent, caused the decline of wine quality.Since the eighties, emerged in an endless stream, replaced preceding class technology substantially about the research of class methods afterwards.This class research method mainly comprises unit operations such as distillation, extraction, membrane sepn, overcritical, freezing and crystallizing.Wherein the infiltration evaporation method is a kind of new membrane separation method that is used to prepare low alcohol at present both at home and abroad or does not have pure fermented drink.It is under the promotion of component steam pressure difference in liquid mixture, utilizes the dissolving of component by film to separate with different realization of rate of diffusion.The typical feature of this method is the restriction that sepn process is not subjected to the component vapor-liquid equilibrium, by selecting suitable mould material and film-forming method for use, might make the bigger film of separation factor.In addition, the infiltration evaporation process can be operated at normal temperatures and pressures, and this has just been avoided in the processes such as distillation because of the improper influence to the wine quality of heating operation.And do not need in the process to introduce other chemical reagent, avoided the pollution of product, simultaneously if adopt preferential saturating pure hydrophobic membrane, then can avoid processes such as reverse osmosis, dialysis to form variation because of the wine liquid that changes water greatly and cause.Therefore the infiltration evaporation process is used for alcoholic beverage dealcoholysis field huge advantage and potentiality.Escudier[is referring to Escudier J.L., Le Bouar M., Applicationand evaluation of pervaporation for the production of low alcohol wines, Proceedings of thethird International Conference on Pervaporation Processes in the Chemical Industry.Englewood, NJ, Bakish Materials Corp., 1988,387-397] and Kimmerle[referring to Kimmerle K., Gudernatsch W., Pilot dealcoholization of beer by pervaporation, Proceedings of the fifthInternational Conference on Pervaporation Processes in the Chemical Industry.Englewood, NJ, Bakish Materials Corp., 1991,291-307] early start the infiltration evaporation legal system be equipped with the research of alcohol-free or low alcohol alcoholic beverage; Lee etc. [referring to: Lee, Eric K., Kalyani, Vinay J., Matson, Stephen L., Process oftreating alcoholic beverages by vapor-arbitrated pervaporation, US Patent 5013447,1991] once adopted crosslinked polyureas composite membrane that grape wine is carried out the infiltration evaporation dealcoholysis in 1991; Brueschke etc. [referring to: Brueschke, Hartmut E.A., Schneider, Walter H., Tusel, Guenter F., Process for the reductionof the alcohol content of alcoholic beverages, US Patent 5385647,1995] in PDMS composite membrane dealcoholysis from beer and grape wine that nineteen ninety-five uses PDMS, the modification PDMS of heat cross-linking respectively and dosed the silicon zeolite, all obtained dealcoholysis wine product.
Aromatoising substance in the former wine is the volatile organic matter of some lower concentrations (ppm level), comprises alcohols, aldehydes, and the ester class, lactone, carboxylic-acid, hydro carbons, phenol, ethers and terpenes, the atmospheric boiling point scope is at 40～200 ℃.According to boiling spread, these aromatoising substances can be divided into four classes: (1) boiling point is lower than ethanol class fragrant substance, mainly comprises methyl alcohol, ethyl acetate, acetaldehyde etc., (2) ethanol; (3) boiling point is higher than ethanol class fragrant substance, is mainly potato spirit, i.e. n-propyl alcohol, primary isoamyl alcohol, butanols, isopropylcarbinol etc.; (4) the highest fragrant substance of boiling point is mainly acetic acid, ethyl lactate, hexanol, octanol etc.A certain amount of natural aromatic material can be followed ethanol-with deviating from the dealcoholysis process of former wine, thereby causes the flavor loss of product wine, if heat treated is improper, easily causes producing thermally denature simultaneously.Special needs to be pointed out is some aromatised fraction such as methyl alcohol in the former wine, the fusel wet goods is the harmful substances that mainly contains in the former wine, drinks the people is seriously poisoned after excessive.Meta-bolites-the formaldehyde of methyl alcohol and the toxicity of formic acid are bigger.Too high potato spirit can make neural system hyperemia, and the people is had a headache, and its toxicity increases with molecular weight and aggravates, and the fusel wet goods is out of proportion in former wine in addition, then can cause strange taste such as the hardship of product wine, puckery, sour, suffering.It all is simply the main fragrant substance composition in the former wine (being mainly beer and grape wine etc.) to be reclaimed that forefathers are equipped with in the document of dealcoholysis wine product and the patent report about single infiltration evaporation legal system, if and cause in the existing former wine fragrant substance component ratio undesirable because of fermentation stage, and according to the variation needs of market taste demand fragrant substance is formed and to be made corresponding adjustment, existing document and patent all do not provide effective solution.Escudier for example, Kimmerle, Lee and Bmeschke etc. only adopt simple multistage partial condenser that the gaseous mixture that film sees through side is carried out the segmentation condensation, can not reach the effect of fine separation water, ethanol and each fragrant substance like this, thereby can not obtain the high purity ethanol product on the one hand, can not form fragrant substance in the product wine on the other hand and make optimization.Therefore this patent adopt special P V-MCMSD coupling technique to separate gentle, directed, subtly and the former wine of recombinating in all kinds of natural aromatic materials, thereby both can fully guarantee the mouthfeel of product, the maintenance of local flavor, can adjust effectively the not good enough former wine of quality again, more can be optimized and innovate new variety wine according to market demand.
Three, technology contents
The present invention is that core constitutes a coupling process with infiltration vaporization membrane module and multi-stage condensing-many side lines extraction rectifying tower, be used for ethanol and other objectionable impurities that efficiently and directionally removes beverage from raw juice fermented wine such as beer, fruit wine (grape wine, hard cider, Hawthorn Fruit Wine, plum wine, Yangtao wine and other fruit juice fermentation brewing wine) and yellow rice wine etc., carry out the purpose that has of each fragrant substance simultaneously and separate and reorganization, to make low alcohol or not have pure novel alcohol product.
Technical scheme of the present invention is as follows:
The method of low alcohol of a kind of osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, it is made up of the following step basically:
(1) former wine at first carries out preliminary dealcoholysis separation through infiltration vaporization membrane module, and per-meate side obtains the gaseous mixture of each fragrant substance in water, ethanol and the former wine, enters rectifier bottoms, holds back side and then obtains the dealcoholysis feed liquid;
(2) gaseous mixture with per-meate side gained in the step (1) enters rectifier bottoms, carry out rectifying, rectifying tower is taked rectification under vacuum, cat head multi-stage condensing and many side lines of body of the tower extraction mode, the fragrant substance of different boiling scope in fine separation and the former wine of reorganization, the rectifying tower top is provided with multistage partial condenser, partial condensation liquid passes back into behind the tower with rising gaseous mixture from the infiltration vaporization membrane module per-meate side and crosses, and carries out the mass-and heat-transfer effect, finishes the fine separation process.Overhead fraction is that boiling point is lower than the alcoholic acid fragrant substance, by control tower directed such fragrant substance of extraction of mode of level partial condenser temperature and control reflux ratio at most, and has purpose to remove methyl alcohol; Tower middle part side line extraction high purity ethanol product; But tower bottom side line extraction boiling point is higher than alcoholic acid fragrant substance (potato spirit), and debris then is the highest fragrant substance composition of boiling point at the bottom of the tower.
(3) with the dealcoholysis feed liquid that side obtains of holding back of infiltration vaporization membrane module, fragrant substance mixed at the bottom of the rectifying tower cat head was removed the fragrant substance of methyl alcohol and rectifying Tata, and appropriate supplement adding distil water and carry out the later stage and modify, the low alcohol or the non-alcohol beverage from raw juice fermented wine of can be maintained original local flavor and mouthfeel.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, the film that uses in the described infiltration vaporization membrane module is a kind of multilayer complex films, it is made of two-layer different mould material at least, top layer is the preferential saturating organism mould material of dense non-porous, plays the effect of isolating active layer; Have one deck porous supporting layer below the active coating at least, make composite membrane have favorable mechanical and physicals.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, the preferential saturating organism mould material of the top layer dense non-porous of described multilayer complex films is a silicon rubber, polyvinylidene difluoride (PVDF), polypropylene, poly-trimethyl silicane propine, poly-trimethylammonium alkyl ethene, polyhutadiene, tetrafluoroethylene, nylon, polycarbonate, ethylene-propylene-diene terpolymers; styrene-butadiene rubber(SBR); paracril, polyphenyl imidazolone, poly-two phenoxyphosphazenes; polyphenylene ether-polyamide segmented copolymer or polyethylene etc. and their derivative are good with silicon rubber and derivative thereof.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, described silicon rubber and derivative thereof are meant with the polysiloxane to be the polymer based material, as dimethyl siloxane, ethylene methacrylic radical siloxane, methyl phenyl vinyl siloxanes and methyl trifluoro propyl silicon etc.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, multilayer complex films in the described infiltration vaporization membrane module, its supporting layer is the polymer materials of one or more parent's alcohol, the selectively removing that helps alcohols in the wine, its average pore diameter is preferably between 0.1～1 μ m between 0.01～10 μ m.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, described preferential saturating organic active coating thickness is preferably between 1～10 μ m between 0.1～50 μ m; Supporting layer thickness is preferably between 100～500 μ m between 50～1000 μ m.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, the multilayer complex films that uses in the described infiltration vaporization membrane module can be flat, tubular type, rolling, tubular fibre formula and other pattern, with flat be good.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, the infiltration vaporization membrane module that uses in the described infiltration vaporization membrane module can be plate and frame, tubular fibre formula, spirally wound or other pattern, is good with plate and frame.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, described infiltration evaporation dealcoholysis process can be a batch cycle dealcoholysis process, the dealcoholysis that circulates in the loop that the composite membrane assembly by encloses container, pump, interchanger and a composite membrane assembly or a plurality of parallel connections constitutes of original juice fermentation wine drops to below the target value up to alcohol concn.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, described infiltration evaporation dealcoholysis process can be a continuous dealcoholysis process, original juice fermentation wine in the encloses container is through pump, interchanger, enter a composite membrane assembly or a plurality of placed in-line composite membrane assembly carries out dealcoholysis, the disposable alcohol concn that makes drops to below the target value.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, the feed temperature of said step (1) infiltration evaporation dealcoholysis process is at 10～50 ℃, at 30 ℃ is good, and seeing through wall pressure is 700Pa～7100Pa, is good at 1200Pa.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, described rectifying tower are that theoretical tray is the above rectifying tower of 40 blocks of column plates, and the cat head working pressure is good at 600Pa～7000Pa at 1100Pa.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, described cat head adopts multistage partial condenser to carry out condensation, and condensing temperature is between-30～20 ℃.
The method of low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, according to dealcoholysis wine taste needs, rectifying tower bottom side line extraction part boiling point is higher than alcoholic acid fragrant substance (potato spirit) can account for 0～100% of potato spirit content in the former wine.
Among the present invention, the atmospheric boiling point scope of the fragrant substance composition that the boiling point of the tower bottom extraction of described rectifying tower is the highest is at 120～200 ℃.
Among the present invention, described process can be carried out the finished product of beverage from raw juice fermented wine, also can carry out (as when the fermentation) in certain intermediate stage of the brewing process of wine.
Method production unit of the present invention is simple, the rate of recovery that the atmospheric boiling point of the cat head extraction of rectifying tower is lower than the alcoholic acid fragrant substance reaches as high as 95%, and the highest 80% of the former wine methanol content that accounts for of the methyl alcohol of removing, the ethanol mass content of the tower middle part side line extraction alcohol product of rectifying tower is between 60%～95%.In addition, the operating parameters by regulating infiltration vaporization membrane module and cat head multi-stage condensing actuator temperature and each line produced quantity of rectifying tower are adjustablely allotted differently flavoured new wine product.
Low alcohol that method of the present invention is produced or the ethanol mass content of not having a novel alcohol product of alcohol can be lower than the ethanol content of former wine as required arbitrarily, minimumly reach 0.5%.
Four, description of drawings
Fig. 1 is the batch production process synoptic diagram of low alcohol of osmotic gasification-rectification coupled method of the present invention production or non-alcohol beverage from raw juice fermented wine method, and wherein: 1 is former wine hold-up vessel; 2 is pump; 3 is interchanger; 4,5 and 6 is infiltration vaporization membrane module; 7 is rectifying tower; 8 is the one-level partial condenser; 9 is storage tank; 10 is the secondary partial condenser; 11 is three grades of partial condensers; 12 is complete condenser; 13,14,15 and 16 is pump; 17 is the methyl alcohol storage tank; 18 is the alcohol storage tank; 19 is the potato spirit storage tank; 20 for hanging down alcohol or not having pure product wine storage tank.
Fig. 2 is the continous way production process synoptic diagram of low alcohol of osmotic gasification-rectification coupled method of the present invention manufacturing or non-alcohol beverage from raw juice fermented wine method, and wherein: 1 is former wine hold-up vessel; 2 is pump; 3 is interchanger; 4,5 and 6 is infiltration vaporization membrane module; 7 is rectifying tower; 8 is the one-level partial condenser; 9 is storage tank; 10 is the secondary partial condenser; 11 is three grades of partial condensers; 12 is complete condenser; 13,14,15 and 16 is pump; 17 is the methyl alcohol storage tank; 18 is the alcohol storage tank; 19 is the potato spirit storage tank; 20 for hanging down alcohol or not having pure product wine storage tank.
Five, embodiment
Embodiment 1. adopts infiltration vaporization membrane module and multi-stage condensing-many side lines extraction rectifying tower coupling technique continuous production alcohol-Free wine.Adopt the plate and frame infiltration vaporization membrane module in the present embodiment, wherein use the flat composite membrane of homemade silicon rubber, active coating is a polydimethylsiloxane, thickness is 8 μ m, (new Asia, Shanghai purifies device factory to porous support layer, the cellulose acetate microfiltration membrane) average pore diameter is at 0.45 μ m, and thickness is 100 μ m.Polydimethylsiloxane film liquid (Shanghai synthetic resin plant, the tetraethoxy of adding 2% and 1% dibutyl tin dilaurate in the n-heptane solution of dimethyl siloxane 5%, stirring) blade coating is on supporting layer, treating that solvent evaporates is intact promptly gets composite silicone rubber membrane, and its effective film area is 10m altogether
2The SINOPAK-500 wire packing that uses Jiangsu Hua Jita already to produce in the rectifying tower, diameter is 200mm, the rectifying tower number of theoretical plate is 40.Press the flow process of Fig. 2, get dry red winew with the inlet amount of 100Kg/h from container 1 and (open abundant extra dry red wine, Yantai Zhang Yu company, former wine alcohol concn is about 15.77% (w/w)) be heated to 30 ℃ and enter the plural serial stage infiltration vaporization membrane module, it is 1200Pa that film sees through the side working pressure.Water, ethanol and fragrant substance gaseous mixture that film sees through side are about 20Kg/h, enter rectifying tower 7; Film is held back the dealcoholysis feed liquid of side extraction 80Kg/h, delivers into low alcohol or does not have pure product wine storage tank 20.The rectifying tower top working pressure is 1100Pa, and cat head one-level partial condenser 8 temperature are about 15 ℃, and secondary partial condenser 10 temperature are about 8 ℃, and three grades of partial condenser 11 temperature are about-20 ℃.The about 0.07Kg/h of aromatic liquid thing under three grades of partial condenser 11 condensations enters low alcohol or does not have pure product wine storage tank 20; Steam under three grades of condensers 11 are uncooled enters complete condenser 12 (temperature is about-30 ℃), and under complete condenser 12 condensations is methyl alcohol, is stored in methyl alcohol enrichment storage tank 17 after the condensation, and flow is about 0.03Kg/h.Rectifying Tata middle part (approximately from last several 20 blocks of column plates) obtains industrial spirit, delivers into industrial spirit storage tank 18 through pump 14, and flow is about 14Kg/h, and ethanol content is 90～95%.Rectifying Tata bottom (approximately from last several 30 blocks of column plates) obtains the potato spirit component, delivers into potato spirit storage tank 19 through pump 15, and flow is about 4.4Kg/h.The rectifying tower tower bottom obtains the highest fragrant substance component of boiling point, delivers into low alcohol or does not have pure product wine storage tank 20 through pump 16, and flow is about 4.4Kg/h.Low alcohol or do not have product wine in the pure product wine storage tank 20 held back side by infiltrating and vaporizing membrane three grades of partial condenser 11 condensations of dealcoholysis feed liquid, rectifying tower cat head down fragrant substance and the rectifying Tata at the bottom of fragrant substance mix, and add an amount of distilled water and carry out the later stage modification.Low alcohol or alcohol-Free wine appearance color and former wine are identical, and the mouthfeel of trial test is almost completely identical with former wine.The composition analysis of product wine shows that ethanol content is 0.5%, and methanol content declines to a great extent, and only is 50% of former wine, and potato spirit content is suitably downward modulation as required, and other fragrant substance component contents are no change almost.
The wall pressure that sees through of embodiment 2. infiltration evaporation dealcoholysis processes is 700Pa, and the cat head working pressure of rectifying tower is at 600Pa, and cat head one-level partial condenser 8 temperature are about 5 ℃, and secondary partial condenser 10 temperature are about-4 ℃, and three grades of partial condenser 11 temperature are about-30 ℃.The effective film area of composite silicone rubber membrane is 8m
2All the other experiment conditions are identical with embodiment 1.Result and embodiment 1 basically identical.
The wall pressure that sees through of embodiment 3. infiltration evaporation dealcoholysis processes is 7100Pa, and the cat head working pressure of rectifying tower is at 7000Pa, and cat head one-level partial condenser 8 temperature are about 20 ℃, and secondary partial condenser 10 temperature are about 10 ℃, and three grades of partial condenser 11 temperature are about-10 ℃.The effective film area of composite silicone rubber membrane is 20m
2All the other experiment conditions are identical with embodiment 1.Result and embodiment 1 basically identical.
Embodiment 4. uses the flat composite membrane of homemade polydimethylsiloxane, active coating is a polydimethylsiloxane, and thickness is 0.1 μ m, and (new Asia, Shanghai purifies device factory to porous support layer, the cellulose acetate microfiltration membrane) average pore diameter is at 0.01 μ m, and thickness is 50 μ m.Polydimethylsiloxane film liquid (Shanghai synthetic resin plant, the tetraethoxy of adding 2% and 1% dibutyl tin dilaurate in the n-heptane solution of dimethyl siloxane 5%, stirring) blade coating is on supporting layer, treating that solvent evaporates is intact promptly gets composite silicone rubber membrane, and its effective film area is 4m altogether
2All the other experiment conditions are identical with embodiment 1.Result and embodiment 1 basically identical.
Embodiment 9. adopts tubular fibre formula infiltration vaporization membrane module, wherein use homemade silicon rubber tubular fibre formula composite membrane (the polydimethylsiloxane film hydraulic pressure of preparation among the embodiment 1 to be gone into 0.45 micron the micropore ps hollow fiber uf membrane inner chamber that German GKSS company produces, with high pure nitrogen its inside is purged half an hour again, leave standstill in the air and can get), active coating polydimethylsiloxane thickness is 0.1 μ m, and its effective film area is 4m altogether
2。All the other experiment conditions are identical with embodiment 1.The result is consistent with embodiment 1.
The feed temperature of embodiment 10. infiltration evaporation dealcoholysis processes is at 10 ℃.The effective film area of composite silicone rubber membrane is 16m
2All the other experiment conditions are identical with embodiment 1.Result and embodiment 1 basically identical.
The feed temperature of embodiment 11. infiltration evaporation dealcoholysis processes is at 50 ℃.The effective film area of composite silicone rubber membrane is 8.5m
2All the other experiment conditions are identical with embodiment 1.Result and embodiment 1 basically identical.
The gaseous mixture quality of water, ethanol and fragrant substance is 36Kg, enter rectifying tower 7, the rectifying tower top working pressure is 1100Pa, and cat head one-level partial condenser 8 temperature are about 14-18 ℃, secondary partial condenser 10 temperature are about 6-10 ℃, and three grades of partial condenser 11 temperature are about-25--15 ℃.The about 0.1Kg of aromatic liquid thing under three grades of partial condenser 11 condensations enters low alcohol or does not have pure product wine storage tank 20; Steam under three grades of condensers 11 are uncooled enters complete condenser 12, and the temperature of complete condenser 12 is about-30 ℃, and under the condensation is methyl alcohol, is stored in methyl alcohol storage tank 17 after the condensation, and quality is 0.06Kg.Rectifying Tata middle part (approximately from last several 20 blocks of column plates) obtains industrial spirit, delivers into industrial spirit storage tank 18 through pump 14, and quality is 25.2Kg, and ethanol content is 90～95%.Rectifying Tata bottom (approximately from last several 30 blocks of column plates) obtains the potato spirit component, delivers into potato spirit storage tank 19 through pump 15, and quality is 7.82Kg.The rectifying tower tower bottom obtains the highest fragrant substance component of boiling point, delivers into low alcohol or does not have pure product wine storage tank 20 through pump 16, and quality is 2.82Kg.Low alcohol or do not have product wine in the pure product wine storage tank 20 held back side by infiltrating and vaporizing membrane three grades of partial condenser 11 condensations of dealcoholysis feed liquid, rectifying tower cat head down fragrant substance and the rectifying Tata at the bottom of fragrant substance mix, and add an amount of distilled water and carry out the later stage modification.Low alcohol or do not have the alcohol yellow rice wine appearance color and former wine is identical, the mouthfeel of trial test is almost completely identical with former wine.The composition analysis of product wine shows that ethanol content is 10%, and methanol content declines to a great extent, and only is 60% of former wine, and potato spirit content is suitably downward modulation as required, and other fragrant substance component contents are no change almost.
Claims (10)
1. the method for low alcohol of osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine is characterized in that it is made up of the following step basically:
(1) former wine at first passes through infiltration vaporization membrane module (4,5 and 6) and carries out preliminary dealcoholysis and separate, and per-meate side obtains the gaseous mixture of each fragrant substance in water, ethanol and the former wine, enters rectifying tower (7) bottom, holds back side and then obtains the dealcoholysis feed liquid;
(2) gaseous mixture with per-meate side gained in the step (1) enters rectifying tower (7) bottom, carry out rectifying, rectifying tower is taked rectification under vacuum, many side lines of cat head multi-stage condensing-body of the tower extraction mode, the fragrant substance of different boiling scope in fine separation and the former wine of reorganization, the rectifying tower top is provided with multistage partial condenser (8,10 and 11), partial condensation liquid passes back into behind the tower with rising gaseous mixture from the infiltration vaporization membrane module per-meate side and crosses, and carries out the mass-and heat-transfer effect, finishes the fine separation process.Overhead fraction is that boiling point is lower than the alcoholic acid fragrant substance, by control tower directed such fragrant substance of extraction of mode of level partial condenser temperature and control reflux ratio at most, and has purpose to remove methyl alcohol; Tower middle part side line extraction high purity ethanol product; But tower bottom side line extraction boiling point is higher than the alcoholic acid fragrant substance, and debris then is the highest fragrant substance composition of boiling point at the bottom of the tower;
(3) with the dealcoholysis feed liquid that side obtains of holding back of infiltration vaporization membrane module, fragrant substance mixed at the bottom of the rectifying tower cat head was removed the fragrant substance of methyl alcohol and rectifying Tata, and appropriate supplement adding distil water and carry out the later stage and modify, the low alcohol or the non-alcohol beverage from raw juice fermented wine of can be maintained original local flavor and mouthfeel.
2. the method for low alcohol of osmotic gasification-rectification coupled method according to claim 1 production or non-alcohol beverage from raw juice fermented wine, it is characterized in that: the film that uses in the described infiltration vaporization membrane module is a kind of multilayer complex films, it is made of two-layer different mould material at least, top layer is the preferential saturating organism mould material of dense non-porous, play the effect of isolating active layer, have one deck porous supporting layer below the active coating at least, make composite membrane have favorable mechanical and physicals.
3. the method for low alcohol of osmotic gasification-rectification coupled method according to claim 2 production or non-alcohol beverage from raw juice fermented wine, it is characterized in that: the preferential saturating organism mould material of the top layer dense non-porous of described multilayer complex films is a silicon rubber, polyvinylidene difluoride (PVDF), polypropylene, poly-trimethyl silicane propine, poly-trimethylammonium alkyl ethene, polyhutadiene, tetrafluoroethylene, nylon, polycarbonate, ethylene-propylene-diene terpolymers, styrene-butadiene rubber(SBR), paracril, the polyphenyl imidazolone, poly-two phenoxyphosphazenes, polyphenylene ether-polyamide segmented copolymer or polyethylene etc. and their derivative, its supporting layer are the polymer materialss of one or more parent's alcohol, the selectively removing that helps alcohols in the wine, its average pore diameter is between 0.01～10 μ m.
4. the method for low alcohol of osmotic gasification-rectification coupled method according to claim 2 production or non-alcohol beverage from raw juice fermented wine is characterized in that: the preferential saturating organism mould material of the top layer dense non-porous of described multilayer complex films is silicon rubber and derivative thereof.
5. the method for low alcohol of osmotic gasification-rectification coupled method according to claim 2 production or non-alcohol beverage from raw juice fermented wine is characterized in that: described preferential saturating organic active coating thickness is between 0.1～50 μ m; Supporting layer thickness is between 50～1000 μ m.
According to claim 1 the method for the low alcohol of above-mentioned osmotic gasification-rectification coupled method production or non-alcohol beverage from raw juice fermented wine, it is characterized in that: described infiltration evaporation dealcoholysis process can be a batch cycle dealcoholysis process, the dealcoholysis that circulates in the loop that the composite membrane assembly by encloses container, pump, interchanger and a composite membrane assembly or a plurality of parallel connections constitutes of original juice fermentation wine drops to below the target value up to alcohol concn.
7. the method for low alcohol of osmotic gasification-rectification coupled method according to claim 1 production or non-alcohol beverage from raw juice fermented wine, it is characterized in that: described infiltration evaporation dealcoholysis process can be a continuous dealcoholysis process, original juice fermentation wine in the encloses container is through pump, interchanger, enter a composite membrane assembly or a plurality of placed in-line composite membrane assembly carries out dealcoholysis, the disposable alcohol concn that makes drops to below the target value.
8. the method for low alcohol of osmotic gasification-rectification coupled method according to claim 1 production or non-alcohol beverage from raw juice fermented wine, it is characterized in that: the feed temperature of described step (1) infiltration evaporation dealcoholysis process is at 10～50 ℃, and seeing through wall pressure is 700Pa～7100Pa.
9. the method for low alcohol of osmotic gasification-rectification coupled method according to claim 1 production or non-alcohol beverage from raw juice fermented wine, it is characterized in that: described rectifying tower is that theoretical tray is the above rectifying tower of 40 blocks of column plates, and the cat head working pressure is 600Pa～7000Pa.
10. the method for low alcohol of osmotic gasification-rectification coupled method according to claim 1 production or non-alcohol beverage from raw juice fermented wine, it is characterized in that: described cat head adopts multistage partial condenser to carry out condensation, and condensing temperature is between-30～20 ℃.
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| CNA200510022687XA CN1824748A (en) | 2005-12-28 | 2005-12-28 | Method of producing low alcohol or alcohol less raw juice formentation alcoholic beverage using osmotic gasification-rectification coupling method |
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| CNA200510022687XA CN1824748A (en) | 2005-12-28 | 2005-12-28 | Method of producing low alcohol or alcohol less raw juice formentation alcoholic beverage using osmotic gasification-rectification coupling method |
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