CN101457190B - Method for preparing spirit flavoring wine or spirit flavour liquid mainly with fragrance - Google Patents

Method for preparing spirit flavoring wine or spirit flavour liquid mainly with fragrance Download PDF

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Publication number
CN101457190B
CN101457190B CN2008101481060A CN200810148106A CN101457190B CN 101457190 B CN101457190 B CN 101457190B CN 2008101481060 A CN2008101481060 A CN 2008101481060A CN 200810148106 A CN200810148106 A CN 200810148106A CN 101457190 B CN101457190 B CN 101457190B
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liquid
spirit
liquor
composite bacteria
wine
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CN101457190A (en
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黄建林
李平
汪淑容
季良威
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Sichuan Yinfan Biotechnology Co Ltd
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Sichuan Yinfan Biotechnology Co Ltd
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Abstract

The invention discloses a method for preparing a spirit flavoring spirit or a spirit flavoring liquor mainly aroma through liquid state fermentation and biological esterificaiton by using wastes produced from solid fermentation spirit production as culture mediums of composite bacteria. The composite bacteria comprise clostridium butyricum with a bacteria number of SICC1. 91, clostridium koseri with a bacteria number of SICC1. 13 and clostridium barati with a bacteria number of SICC1. 2; the composite bacteria fermentation mediums comprise yellow water, tail water, lees solution and pot-bottom water with a weight ratio of 7-8: 0. 5-1: 0. 5-1: 0. 5-1. Sodium acetate 1. 5and dibasic potassium phosphate 0. 04are added in the mixture solution, and ammonium bicarbonate is added to adjust pH value to 6. 5-7. 0, 95 degree ethanol 2 0s added after sterilization, then the mixture solution is sterilized at temperature 105 DEG C for 20min. The invention solves the pollution problem of the wastes to the water environment from the solid spirit production process. The added spirit body is more coordinate, which prevents the defect that the addition of monomer product easily generates float fragrant flavor. The spirit has strong nature feeling, and the recovered bacterial sludge and other residual nutritive matters can be recycled in the fermentation process and avoid secondary environment pollution.

Description

With perfume (or spice) is master's the liquor seasoning wine or the preparation method of liquor seasoning liquid
Technical field
The present invention relates to a kind of liquor seasoning wine of edible distillate spirit or preparation method of sauce of being used for; Particularly; The present invention relates to a kind of employing biotechnology, utilize the waste of liquor-making by solid fermentation to be raw material, is master's the liquor seasoning wine or the method for sauce with perfume (or spice) through the liquid state fermentation preparation.
Background technology
The production history in existing hundreds of years of China white wine, but most what still follow so far is ancient and traditional production process, different fully with the mode of production of liquors such as external whisky, brandy, gin, vodka.
At present the production status of commodity liquor mainly comprises following several kinds: one, through heads removal, pluck the wine that the wine tail steams, generally at 50 °~70 °, tentatively be combined to form fragrance former wine in a basic balance, storing through half a year or 1 year promptly becomes base liquor.Foreshot, the wine tail won when two, a part is steamed wine, long time stored through more than 2 years can be used as foreshot, wine tail flavouring wine; Another part is then taked more special manufacture craft, and batching is different, and many wheels are continuous poor, and the pit entry fermentation time is long, and the wine that steams can be obtained self flavouring wine fragrant or the flavor characteristics that have of many complicacies such as wine, old cellar for storing things perfume, old flavor through long time stored.Three, in base liquor, add the finished wine that a certain amount of various flavouring wine just form various styles, various tastes.This process is to taste personnel and carry out by blending, commenting basically, is referred to as to collude wine (i.e. combination), again through the storage of half a year to one year, lets perfume (or spice) and the flavor of wine reach a kind of state of relative equilibrium, can dispatch from the factory.For the wine of various different wine precision, before colluding accent, form through adding slurry (or adding water) degree of falling as 25 °~62 °.
According to statistics, China white wine has had the very huge consumer group in recent years, and nearly 6,000,000 tons/year in the occupancy volume in market, solid state fermentation liquor wherein, the solid-liquid fermentation combines wine can reach 60%, nearly 3,600,000 tons.Though this type liquor the yield of liquor is high, flavour ingredient obviously lacks, and need add flavouring wine, monomer perfume remedies, and can't satisfy the demand of " organic, green, All Pure Nature food " that the human consumer thirsts for day by day.
We know: on the one hand; Solid state fermentation liquor can produce a large amount of wastes of polluted water environment in process of production; Promptly lose poor liquid, bottom pot water, yellow water and tail water (being called for short " four water "); Wherein, the composition in the yellow water has: total acid 0.538~0.65%, starch 2.5~2.7%, total ester 0.16~0.24%, reducing sugar 2.62~2.92%, ethanol 3.8~4%, total nitrogen 0.3~0.43% (wherein amino nitrogen accounts for 30%); Composition in the poor liquid has: starch 5.5~5.9%, crude protein 5.1~6.2%, total acid: count 2.02~3%, count 0.16~0.19% with acetate with lactic acid, total reducing sugar 0.03~0.06%; Composition in the bottom pot water has: acetate is about 0.128%, acetaldehyde 0.016%, ETHYLE ACETATE 0.027%, propionic acid 0.031%, NSC 8882 0.08%, ethyl lactate 0.076%; Composition in the tail water has: 6~8% ethanol, 0.3% organic acid, 0.256% ester, aldehyde, alcohols, 0.0012% amino acid and little peptide.Economize greatly as domestic wine brewing in Sichuan Province, and former wine output has accounted for more than 67%, in recent years of national ultimate production; Except that the large-scale liquor-making enterprise of minority to waste " four water " partially disposed; As: adopt and lose the poor white carbon black of producing, evaporation waste water reuse, the good anaerobism technology of holding concurrently biochemical treatment; Or utilize and to lose poor and poor liquid and produce the DDGS high protein feed, but this method is because technology is high with power consumption, and the feed palatability is poor, and prospect for sales is bad, and liquor enterprise also abandons basically; The enterprise that also has " four water " anaerobic biologicals such as utilizing yellow water to produce biogas, but a large amount of medium-sized and small enterprises do not add processing and directly discharging basically.
Following table is the test result of Qionglai City Environmental Protection Agency to contamination index:
CoDcr BoD 5 SS NH 3-N
Yellow water 2.17×10 5 15000 1800 40
Lose poor liquid 5.65×10 5 20000 24000 40
Residual water 4.74×10 5 20000 25000 40
Tail water 4.06×10 3 1500 800 40
On the other hand, because liquor is mainly by the second alcohol and water that accounts for 98% or more, and the flavor and fragrance substance of less than 2% forms, thereby the purpose of brewed spirit is promptly produced alcohol and is ester that perfume (or spice) is flavor, aldehyde, ketone, acid, alcohol etc.According to a large amount of documents and actual test; The utilization ratio of starch is merely about 60% in the solid state fermentation, and the extraction yield of flavour ingredient is merely 40%, the beneficiating ingredient that can be utilized basically all at the above-mentioned yellow water that abandons, lose in poor liquid, residual water, the tail water; In total acid; Acetic acid, butyric acid, caproic acid, lactic acid are the staples that is flavor in the liquor, and vinyl acetic monomer, ethyl n-butyrate, ethyl lactate, NSC 8882 etc. are the main aroma-producing substances of liquor in total ester.Yellow water also contains the multiple genus bacillus of raising and train for a long time about 10 9Individual/100mL, be the probiotics that produces caproic acid and NSC 8882.Starch in the yellow water, reducing sugar can further be converted into ethanol under zymin and zymic effect.The water except that about 90%, about 10% composition is the beneficiating ingredient in the liquor, if be not used, 4.8 ten thousand tons/year the resource of will having an appointment every year is wasted.
Summary of the invention
The object of the present invention is to provide the substratum of a kind of waste that produces in producing with liquor by solid fermentation as composite bacteria, is the main liquor seasoning wine or the method for liquor seasoning liquid with perfume (or spice) through liquid state fermentation and biological esterification preparation.
For realizing the foregoing invention purpose, the concrete technical scheme that the present invention adopts is following:
With perfume (or spice) is master's the liquor seasoning wine or the preparation method of liquor seasoning liquid, it is characterized in that process step is following:
A, preparation fermention medium
By weight; With the yellow water that produces in the liquor by solid fermentation production, lose poor liquid, tail water and bottom pot water by 7~8: 0.5~1: 0.5~1: 0.5~1 mix after; In mixed solution, add sodium acetate 1.5%, potassium hydrogenphosphate 0.04% again; Transfer pH to 6.5~7.0 with the carbon ammonium, in 105 ℃ of sterilizations 20 minutes, 95 ° of ethanol that add 2% (V/V) at last promptly got.
Carbon in the said fermention medium, nitrogen ratio are 1: 1.2~1.9.
B, access composite bacteria carry out liquid state fermentation
In the fermention medium that steps A makes, insert 20% composite bacteria liquid by volume, be under 6.5~7.0 the anaerobically fermenting condition, to cultivate 7~13d and get fermented liquid at 34~37 ℃, pH.
The self-produced air pressure of said yeast phase indirect fermentation jar remains on 0.25~0.30Mpa.
Said composite bacteria comprises the clostridium butylicum that bacterium numbering is SICC1.91, Ke Shi clostridium and the bacterium numbering that bacterium numbering is SICC1.13 is the Acetobacter pasteurianus of SICC1.2.
More than three kinds of bacterial classifications all available from Sichuan Province Research for Industrial Microbial Germ preservation administrative center, its bacterium numbering is recorded in respectively on P63, P72 and the P73 of the bacterial classification DB of being issued by Sichuan Province Microbial resources platform DSMZ.
The substratum of said three kinds of bacterial classifications and composite bacteria is:
1, slant strains substratum: sodium acetate 0.5%, potassium hydrogenphosphate 0.04%, sal epsom 0.02, ammonium sulfate 0.05%, yeast extract paste 0.5%, lime carbonate 1%, agar 2%;
2, seed culture medium: sodium acetate 0.5%, potassium hydrogenphosphate 0.04%, sal epsom 0.02%, ammonium sulfate 0.05%, yeast extract paste 0.5%, 1%, 105 ℃ of sterilization of lime carbonate add 95 ° of ethanol of 2% (V/V) after 20 minutes;
3, composite bacteria fermention medium: yellow water: tail water: poor liquid: residual water=7~8: 0.5~1: 0.5~1: 0.5~1 (W/W); Sodium acetate 1.5%, potassium hydrogenphosphate 0.04%, carbon ammonium transfer pH to 6.5~7.0, sterilization back to add 95 ° of ethanol of 2% (V/V); Sterilization: 105 ℃; 20 minutes, wherein carbon, nitrogen ratio were 1: 1.2~1.9.
The compound method of said composite bacteria liquid is:
I, the inoculum size of pressing Acetobacter pasteurianus Fourth Ring, Ke Shi clostridium three rings, clostridium butylicum one ring insert said seed culture medium, behind 35~37 ℃ of cultivation 7d, the bacterium colony that forms are transferred in the slant strains substratum again, and 4 ℃ of preservations are subsequent use in refrigerator.
II, get composite bacteria and carry out two~three grades of seeds by the seed culture based formulas (10L~100L) is enlarged culturing step by step, and every grade all promptly gets three grades of composite bacteria liquid in 35~37 ℃ after cultivating 7d.
Obtaining through refining of C, fermented liquid
After the fermentation ends, fermented liquid is through solid-liquid separation (bacterium mud reclaims with recycle), and centrifugate is transferred pH3.5~4.0 with food grade sulfuric acid; Reheat to 80 ℃ makes the free protein sex change, adds the base liquor of 72 ° of 20% (V/V) subsequently, makes the rapid sedimentation of impurity; Open air compressor machine ventilation deodorizing simultaneously; Treat that stink eliminates again and remove impurity with filtering centrifuge, gained centrifugate concentrates through economic benefits and social benefits vacuum distilling, becomes three sections liquid fractionations through the rectifying tower fractionation is refining again: alcohol section, water section, heat up in a steamer back segment; 72 ° of base liquors that in water section liquid fractionation, add compound bio zymin and 20% then; Put under 34 ℃ of temperature and intermittently stir; Promptly whenever stirred 10 minutes with 120r.p.m at a distance from 2 hours, behind esterification 4~7d, it is main liquor seasoning wine or sauce that esterifying liquid promptly obtains with perfume (or spice) after distillation again.
Said compound bio zymin is made up of Daqu, red colouring agent for food, also used as a Chinese medicine and SHENGXIANG yeast, and its add-on is respectively Daqu 20%, red colouring agent for food, also used as a Chinese medicine 10%, SHENGXIANG yeast 1% by W/V.
The solid-liquid separation of said fermented liquid adopts tripod pendulum type batch centrifugal, and continuously feeding is centrifugal under the condition of 1450r.p.m.
Compared with prior art, beneficial effect of the present invention shows:
1, the invention solves the pollution problem of the waste that produced in the solid spirit production process, make resource circulation utilization simultaneously, for enterprise has created certain economic benefits to water surrounding.
2, product of the present invention has played effective supplementary function to the deficiency of complex ester in the aroma daqu liquor; Wine body after the interpolation is coordinated more, and strong sense strengthens, and is biological products because of product of the present invention simultaneously; Thereby avoided adding the shortcoming that monomer product is prone to produce floating fragrance, it is strong that the wine body is felt naturally.
3, bacterial content is more in the liquid state fermentation liquid of the present invention; And go back remnants starch, sugar, protein and ammonium are arranged; These available resources are separated through solid, liquid, can the bacterium mud that reclaim and other remaining nutritive substance recycle during the fermentation be avoided causing secondary environmental pollution.
4, product of the present invention is main liquor seasoning wine or sauce toxicological harmless effect with perfume (or spice); In whole process of production; Adopt microbial fermentation engineering and biological enzyme technology; Do not add any chemical catalyst, used former, auxiliary material is biological level, food grade products, and " safety, green, environmental protection " meets the FAR standard.
5, production technique of the present invention " energy-saving and emission-reduction, consumption reduction synergy ", and make by-product resource.
Embodiment
The preparation of embodiment one fermention medium
By weight; With the yellow water that produces in the liquor by solid fermentation production, lose poor liquid, tail water and bottom pot water by 7: 1: 1: 1 mix after; In mixed solution, add sodium acetate 1.5%, potassium hydrogenphosphate 0.04% again; Transfer pH to 6.5~7.0 with the carbon ammonium, in 105 ℃ of sterilizations 20 minutes, 95 ° of ethanol that add 2% (V/V) at last promptly got.
Carbon in the said fermention medium, nitrogen ratio are 1: 1.2~1.9.
The liquid state fermentation of embodiment two composite bacterias
In fermention medium, insert 20% composite bacteria liquid by volume, be under 6.5~7.0 the anaerobically fermenting condition, to cultivate 7~13d and get fermented liquid at 34~37 ℃, pH.
The self-produced air pressure of said yeast phase indirect fermentation jar remains on 0.25~0.30Mpa.
Said composite bacteria comprises the clostridium butylicum that bacterium numbering is SICC1.91, Ke Shi clostridium and the bacterium numbering that bacterium numbering is SICC1.13 is the Acetobacter pasteurianus of SICC1.2.
The substratum of said three kinds of bacterial classifications and composite bacteria is:
1, slant strains substratum: sodium acetate 0.5%, potassium hydrogenphosphate 0.04%, sal epsom 0.02, ammonium sulfate 0.05%, yeast extract paste 0.5%, lime carbonate 1%, agar 2%;
2, seed culture medium: sodium acetate 0.5%, potassium hydrogenphosphate 0.04%, sal epsom 0.02%, ammonium sulfate 0.05%, yeast extract paste 0.5%, 1%, 105 ℃ of sterilization of lime carbonate add 95 ° of ethanol of 2% (V/V) after 20 minutes;
3, composite bacteria fermention medium: yellow water: tail water: poor liquid: residual water=7: 1: 1: 1 (W/W); Sodium acetate 1.5%, potassium hydrogenphosphate 0.04%, carbon ammonium transfer pH to 6.5~7.0, sterilization back to add 95 ° of ethanol of 2% (V/V); Sterilization: 105 ℃; 20 minutes, wherein carbon, nitrogen ratio were 1: 1.2~1.9.
The compound method of said composite bacteria liquid is:
1, press the inoculum size of Acetobacter pasteurianus Fourth Ring, Ke Shi clostridium three rings, clostridium butylicum one ring, insert said seed culture medium, behind 35~37 ℃ of cultivation 7d, the bacterium colony that forms is transferred in the slant strains substratum again, 4 ℃ of preservations are subsequent use in refrigerator.
2, getting composite bacteria carries out two~three grades of seeds by the seed culture based formulas (10L~100L) is enlarged culturing step by step, and every grade all promptly gets three grades of composite bacteria liquid in 35~37 ℃ after cultivating 7d.
Obtaining through refining of embodiment three fermented liquids
After the fermentation ends, fermented liquid is placed tripod pendulum type batch centrifugal, and continuously feeding is centrifugal under the condition of 1450r.p.m; Bacterium mud reclaims with recycle, and centrifugate is with food grade sulfuric acid accent pH3.5~4.0, and reheat to 80 ℃ makes the free protein sex change; 72 ° of base liquors that add 20% (V/V) subsequently; Make the rapid sedimentation of impurity, open air compressor machine ventilation deodorizing simultaneously, treat that stink eliminates to remove impurity again with filtering centrifuge; Gained centrifugate concentrates through economic benefits and social benefits vacuum distilling, becomes three sections liquid fractionations through the rectifying tower fractionation is refining again: alcohol section, water section, heat up in a steamer back segment; 72 ° of base liquors that in water section liquid fractionation, add Daqu 20%, red colouring agent for food, also used as a Chinese medicine 10%, SHENGXIANG yeast 1% and 20% then; Put under 34 ℃ of temperature and intermittently stir; Promptly whenever stirred 10 minutes with 120r.p.m at a distance from 2 hours; Behind the esterification 7d, it is main liquor seasoning wine or liquor seasoning liquid that esterifying liquid promptly obtains with perfume (or spice) after distillation again.
Through detecting, of the present invention is that the correlation technique index of main liquor seasoning wine or sauce is following with perfume (or spice):
Test item Unit Detection method Detected result
NSC 8882 g/L Gas chromatography determination 10.66
Total acid g/L Neutralization titration is measured 21.17
The wine degree %vol Vinometor is measured 62

Claims (6)

1. one kind is master's the liquor seasoning wine or the preparation method of liquor seasoning liquid with perfume (or spice), it is characterized in that process step is following:
A, preparation fermention medium
By weight; With the yellow water that produces in the liquor by solid fermentation production, lose poor liquid, tail water and bottom pot water and mix by 7~8:0.5~1:0.5~1:0.5~1 after; In mixed solution, add sodium acetate 1.5%, potassium hydrogenphosphate 0.04% again; Transfer pH to 6.5 ~ 7.0 with the carbon ammonium,, add 95 ° of ethanol of 2% at last and promptly get in 105 ℃ of sterilizations 20 minutes;
B, access composite bacteria carry out liquid state fermentation
In the fermention medium that steps A makes, insert 20% composite bacteria liquid by volume, be under 6.5 ~ 7.0 the anaerobically fermenting condition, to cultivate 7 ~ 13d and get fermented liquid at 34 ~ 37 ℃, pH;
Said composite bacteria comprises the clostridium butylicum that bacterium numbering is SICC1.91, Ke Shi clostridium and the bacterium numbering that bacterium numbering is SICC1.13 is the Acetobacter pasteurianus of SICC1.2;
The compound method of said composite bacteria liquid is:
Ι, the inoculum size of pressing Acetobacter pasteurianus Fourth Ring, Ke Shi clostridium three rings, clostridium butylicum one ring insert said seed culture medium, behind 35 ~ 37 ℃ of cultivation 7d, the bacterium colony that forms are transferred in the slant strains substratum again, and 4 ℃ of preservations are subsequent use in refrigerator;
II, get composite bacteria and carry out two~three grades of seeds enlarged culturing step by step by the seed culture based formulas, every grade all promptly gets three grades of composite bacteria liquid in 35 ~ 37 ℃ after cultivating 7d;
Obtaining through refining of C, fermented liquid
After the fermentation ends, fermented liquid is through solid-liquid separation, and centrifugate is transferred pH3.5~4.0 with food grade sulfuric acid; Reheat to 80 ℃ makes the free protein sex change, adds 72 ° of base liquors of 20% subsequently, in the settled while of impurity; Open air compressor machine ventilation deodorizing, treat that stink eliminates to remove impurity again with filtering centrifuge, gained centrifugate through economic benefits and social benefits vacuum distilling concentrate and the rectifying tower fractionation refining; 72 ° of base liquors that in water section liquid fractionation, add compound bio zymin and 20% then; Put under 34 ℃ of temperature and whenever stirred 10 minutes with 120r.p.m at a distance from 2 hours, behind esterification 4 ~ 7d, it is main liquor seasoning wine or sauce that esterifying liquid promptly obtains with perfume (or spice) after distillation again;
Said compound bio zymin is made up of Daqu, red colouring agent for food, also used as a Chinese medicine and SHENGXIANG yeast, and its add-on is respectively Daqu 20%, red colouring agent for food, also used as a Chinese medicine 10%, SHENGXIANG yeast 1% by W/V.
2. as claimed in claim 1 is master's the liquor seasoning wine or the preparation method of liquor seasoning liquid with perfume (or spice), it is characterized in that: the carbon in the said fermention medium of steps A, nitrogen are than being 1:1.2~1.9.
3. as claimed in claim 1 is master's the liquor seasoning wine or the preparation method of liquor seasoning liquid with perfume (or spice), and it is characterized in that: the self-produced air pressure of fermentor tank remains on 0.25~0.30Mpa during the said liquid state fermentation of step B.
4. as claimed in claim 1 is master's the liquor seasoning wine or the preparation method of liquor seasoning liquid with perfume (or spice), and it is characterized in that: the slant strains substratum of the composite bacteria of the said Acetobacter pasteurianus of step B, Ke Shi clostridium, clostridium butylicum and these three kinds of bacterial classifications is: sodium acetate 0.5%, potassium hydrogenphosphate 0.04%, sal epsom 0.02%, ammonium sulfate 0.05%, yeast extract paste 0.5%, lime carbonate 1%, agar 2%.
5. as claimed in claim 1 is master's the liquor seasoning wine or the preparation method of liquor seasoning liquid with perfume (or spice); It is characterized in that: the seed culture medium of the composite bacteria of the said Acetobacter pasteurianus of step B, Ke Shi clostridium, clostridium butylicum and these three kinds of bacterial classifications is: sodium acetate 0.5%, potassium hydrogenphosphate 0.04%, sal epsom 0.02%, ammonium sulfate 0.05%, yeast extract paste 0.5%, 1%, 105 ℃ of sterilization of lime carbonate add 95 ° of ethanol of 2% after 20 minutes.
6. as claimed in claim 1 is master's the liquor seasoning wine or the preparation method of liquor seasoning liquid with perfume (or spice), it is characterized in that: the solid-liquid separation of the said fermented liquid of step C adopts tripod pendulum type batch centrifugal, and continuously feeding is centrifugal under the condition of 1450r.p.m.
CN2008101481060A 2008-12-30 2008-12-30 Method for preparing spirit flavoring wine or spirit flavour liquid mainly with fragrance Expired - Fee Related CN101457190B (en)

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