CN102051309B - Multi-strain compound fermentation type jujube wine and brewing method thereof - Google Patents

Multi-strain compound fermentation type jujube wine and brewing method thereof Download PDF

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CN102051309B
CN102051309B CN 201010502867 CN201010502867A CN102051309B CN 102051309 B CN102051309 B CN 102051309B CN 201010502867 CN201010502867 CN 201010502867 CN 201010502867 A CN201010502867 A CN 201010502867A CN 102051309 B CN102051309 B CN 102051309B
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jujube
jujube juice
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red date
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CN102051309A (en
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马强
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Shanxi Yuebulin Venture Investment Co Ltd
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Abstract

The invention discloses multi-strain compound fermentation type jujube wine and a brewing method thereof. The jujube wine obtained by carrying out compound fermentation on candida, hansenula polymorpha, pichia pastoris, kloeckera and saccharomyces cerevisiae is obviously superior to jujube wine prepared by fermenting single saccharomyces cerevisiae in flavor and taste. In the invention, non-saccharomyces generate aromatic matters, i.e. higher alcohol, lower fatty acids, esters, and the like, and special flavor components so that the jujube wine is obviously improved in flavor characteristics and has smoother taste and stronger flavor, thereby overcoming the defects of single saccharomyces fermentation and generating positive effects on the total flavor of the jujube wine; and in addition, the jujube wine has the advantages of full wine body, rose color, clarification, brightness, mellow and smooth taste and pure and elegant jujube aroma and bouquet.

Description

A kind of many strain compound fermentation type jujube wines and brewing method thereof
Technical field
The present invention relates to a kind of many strain compound fermentation type jujube wines and brewing method thereof, belong to brewing technical field.
Background technology
Red date is one of distinctive fruit of China, in northern China very large cultivated area is arranged, and the red date fruit has the effect of " tonify Qi of the kidney, grow taste, protect liver and gall, moisten cardiopulmonary ", has good medicine and health care to be worth.In recent years, China's jujube tree production development is rapid, and output increases substantially, in the production in the urgent need to seeking the approach of deep processing.At present, China's jujube converted products mainly contains candied date, jujube tea, nourishing Chinese date crystalline substance etc.Red date wine production mainly is liquor, and is also few to the research of fermented type jujube wine.Fermented jujube wine is to carry out saccharomycetes to make fermentation take red date as raw material, take full advantage of a kind of low-alcoholic beverage of the sugar generation alcohol in the red date, not only kept the nutritive substance that enriches in the red date, also contain the synthetic benefit materials of many microbial metabolisms, have unique local flavor and nutritive value, very favourable to HUMAN HEALTH, have good development prospect.But the red date wine that ferments does not at present also have suitable yeast, yeast saccharomyces cerevisiae behind many employing wine yeasts or the purifying carries out the fermentation of single yeast, these yeast mainly are for the seed selection of grape wine brew institute, good effect might not be arranged in the production of jujube wine, though therefore jujube wine nutritive value height but mouthfeel is not good, local flavor is too flat.So, in order to optimize the production technique of jujube wine, improve the quality of jujube wine, the jujube brewer yeast be selected to the subject matter that jujube wine already faces.
Summary of the invention
The object of the invention provides a kind of many strain compound fermentation type jujube wines and brewing method thereof, overcomes single yeast-leavened deficiency, mainly solves the problem that the red date wine mouthfeel is not good, local flavor is too flat.This technique has solved the problems referred to above.
The present invention uses Saccharomyces Cerevisiae in S accharomyces cerevisiae, candiyeast Candida sp., spore debaryomyces hansenii Hanseniaspora sp., pichia spp Pichia sp. and Ke Leke yeast Kloeckera sp. five primary yeast complex ferments.
Specifically, the present invention includes following steps:
(1) select materials, wash select complete, without the red date of canker insect pest, rinse well with water purification;
(2) the red date steam treatment 10~30min after steam treatment is cleaned;
(3) protect the water that red date that look, hot dipping steam treatment cross adds 4~8 times, then add parts by weight and be the composite phosphate of 0.05%~0.10% citric acid and 0.05%~0.15% as colour protecting agent, process 90~150min for 60~80 ℃; Described composite phosphate is sodium hexametaphosphate: the mixture of sodium polyphosphate=1: 1~1: 1.5;
The red date of (4) making beating, the above-mentioned processing of filtration is pulled an oar, and screenings separates, and removes jujube nuclear, then filters to get jujube juice a and jujube slag b;
(5) add respectively citric acid among enzymolysis jujube juice a and the jujube slag b, regulate pH to 3~4, the control temperature is at 40~60 ℃, then adds parts by weight among the jujube juice a and be 0.02%~0.10% polygalacturonase and 0.02%~0.08% α-amylase, enzymolysis 15~35min filters to get jujube juice c; Add 0.05%~0.10% cellulase and 0.01%~0.06% hemicellulase among the jujube slag b, under strength of current 0.6A/25w~1.5A/275w, carry out ultrasonic enzymolysis processing 20~40min with the probe type ultrasonic extraction apparatus, then filter to get jujube juice d, jujube juice c and jujube juice d are mixed;
(6) be filled with the SO of 90~140mg/L in the above-mentioned mixing jujube of the sterilization juice 2, stir, 100 ℃ are carried out germicidal treatment 15~30min;
(7) inoculation, fermentation will be cooled to 20 ℃~30 ℃ mixing jujube juice and squeeze into fermentor tank, access respectively 5 good primary yeasts of activation in the fermentor tank: candiyeast, spore debaryomyces hansenii, pichia spp, Ke Leke yeast and yeast saccharomyces cerevisiae, stir, inoculum size is controlled at respectively 1%~10%, adopt temperature controlled fermentation, leavening temperature is controlled at 20~25 ℃, and fermentation time is 10~20d;
(8) after the ageing fermentation former wine packed into and be placed with in the container of oak chip, former wine is carried out supersound process, ultrasonic frequency is 20~30kHz, and power is 40~60W, and the time is 5~15min;
(9) red date wine that must clarify is at last filtered the wine liquid after the ageing in clarification by diatomite filter.
Single fermentation by saccharomyces cerevisiae and composite yeast of the present invention fermentation, the quality of wine compares:
Figure BSA00000297729700021
The jujube wine that uses as can be seen from the above table jujube wine taste mouthfeel that composite yeast fermentation obtains to make significantly better than single fermentation by saccharomyces cerevisiae.The mensuration alcoholic strength is 10~12%v/v.
Used yeast of the present invention: Saccharomyces Cerevisiae in S accharomyces cerevisiae, candiyeast Candida sp., spore debaryomyces hansenii Hanseniaspora sp., pichia spp Pichia sp. and Ke Leke yeast Kloeckera sp. can select commercially available finished product or be used through after the enlarged culturing by test tube strains.
Described enlarged culturing method is as follows:
Malt extract medium, substratum consists of: 5~12 ° of Be ' worts, solid medium contains 1.5~2.0% agar, and culture temperature is 25~30 ℃, the pH nature.
Cultivate flow process: bacterial classification → slant tube → liquid tube → triangular flask cultivation → Ka Shi tank.
Concrete propagation method is: at aseptic condition bacterial classification is accessed fresh slant tube and activate, so that yeast is in vigorous animation, in 25~30 ℃ of heat insulating culture 3 days, treat to grow on the inclined-plane white lawn, namely cultivate ripe.From slant tube picking one ring yeast thalline, the liquid tube of 10ml wort is equipped with in access, after shaking up, puts 25~30 ℃ of heat insulating culture 24 hours with inoculating needle, treats liquid level a large amount of CO of emerging 2, the access triangular flask is cultivated.Enter afterwards the fastening tank cultivation and make distiller's yeast.Ka Shi tank substratum can use the distiller's yeast converted mash, so that yeast adapts to large productive culture condition gradually.The converted mash that the Ka Shi tank is used is for subsequent use after the sterilization separately, if the factory hygiene management condition is better, and also can not sterilization.
The invention has the beneficial effects as follows: adopt yeast saccharomyces cerevisiae and Non-Saccharomyces candiyeast, spore debaryomyces hansenii, pichia spp and Ke Leke yeast complex ferment in the jujube wine fermentation, these Non-Saccharomyces produce aromatoising substance and the special flavor compound such as some higher alcoholss, lower fatty acid and ester class in fermentation, the flavor characteristic of wine is obviously improved, jujube wine mouthfeel is more lubricated, more enriching is pure for local flavor, overcome single yeast-leavened deficiency, the overall local flavor of jujube wine has been produced active influence.Gained jujube wine wine body is plentiful, is rose, clarifies glossyly, and mouthfeel is mellow lubricated, has pure quiet and tastefully laid out red date fruital and aroma.
Embodiment
The present invention is further described for following examples:
Embodiment 1
(1) select materials, wash select complete, without the red date of canker insect pest, rinse well with water purification;
(2) the red date steam treatment 10min after steam treatment is cleaned;
(3) protect the water that red date that look, hot dipping steam treatment cross adds 8 times, then add parts by weight and be the composite phosphate of 0.05% citric acid and 0.15% as colour protecting agent, process 90min for 80 ℃; Described composite phosphate is sodium hexametaphosphate: the mixture of sodium polyphosphate=1: 1;
The red date of (4) making beating, the above-mentioned processing of filtration is pulled an oar, and screenings separates, and removes jujube nuclear, then filters to get jujube juice a and jujube slag b;
(5) add respectively citric acid among enzymolysis jujube juice a and the jujube slag b, regulate pH to 3, the control temperature is at 40 ℃, then adds parts by weight among the jujube juice a and be 0.10% polygalacturonase and 0.02% α-amylase, and enzymolysis 35min filters to get jujube juice c; The cellulase of adding 0.05% and 0.06% hemicellulase carry out ultrasonic enzymolysis processing 20min with the probe type ultrasonic extraction apparatus among the jujube slag b under strength of current 1.5A/275w, then filter to get jujube juice d, and jujube juice c and jujube juice d are mixed;
(6) be filled with the SO of 90mg/L in the above-mentioned mixing jujube of the sterilization juice 2, stir, 100 ℃ are carried out germicidal treatment 30min;
(7) inoculation, fermentation will be cooled to 20 ℃ of mixing jujube juice and squeeze into fermentor tank, access respectively 5 good primary yeasts of activation in the fermentor tank: candiyeast, spore debaryomyces hansenii, pichia spp, Ke Leke yeast and yeast saccharomyces cerevisiae, stir, inoculum size is controlled at respectively 1%, adopt temperature controlled fermentation, leavening temperature is controlled at 20 ℃, and fermentation time is 20d;
(8) after the ageing fermentation former wine packed into and be placed with in the container of oak chip, former wine is carried out supersound process, ultrasonic frequency is 20kHz, and power is 60W, and the time is 5min;
(9) red date wine that must clarify is at last filtered the wine liquid after the ageing in clarification by diatomite filter.The mensuration alcoholic strength is 10%v/v.
Single fermentation by saccharomyces cerevisiae and composite yeast fermentation, the quality of wine compares:
Embodiment 2
(1) select materials, wash select complete, without the red date of canker insect pest, rinse well with water purification;
(2) the red date steam treatment 30min after steam treatment is cleaned;
(3) protect the water that red date that look, hot dipping steam treatment cross adds 4 times, then add parts by weight and be the composite phosphate of 0.10% citric acid and 0.05% as colour protecting agent, process 150min for 60 ℃; Described composite phosphate is sodium hexametaphosphate: the mixture of sodium polyphosphate=1: 1.5;
The red date of (4) making beating, the above-mentioned processing of filtration is pulled an oar, and screenings separates, and removes jujube nuclear, then filters to get jujube juice a and jujube slag b;
(5) add respectively citric acid among enzymolysis jujube juice a and the jujube slag b, regulate pH to 4, the control temperature is at 60 ℃, then adds parts by weight among the jujube juice a and be 0.02% polygalacturonase and 0.08% α-amylase, and enzymolysis 15min filters to get jujube juice c; The cellulase of adding 0.10% and 0.06% hemicellulase carry out ultrasonic enzymolysis processing 40min with the probe type ultrasonic extraction apparatus among the jujube slag b under strength of current 0.6A/25w, then filter to get jujube juice d, and jujube juice c and jujube juice d are mixed;
(6) be filled with the SO of 140mg/L in the above-mentioned mixing jujube of the sterilization juice 2, stir, 100 ℃ are carried out germicidal treatment 15min;
(7) inoculation, fermentation will be cooled to 30 ℃ of mixing jujube juice and squeeze into fermentor tank, access respectively 5 good primary yeasts of activation in the fermentor tank: candiyeast, spore debaryomyces hansenii, pichia spp, Ke Leke yeast and yeast saccharomyces cerevisiae, stir, inoculum size is controlled at respectively 10%, adopt temperature controlled fermentation, leavening temperature is controlled at 25 ℃, and fermentation time is 10d;
(8) after the ageing fermentation former wine packed into and be placed with in the container of oak chip, former wine is carried out supersound process, ultrasonic frequency is 30kHz, and power is 40W, and the time is 5min;
(9) red date wine that must clarify is at last filtered the wine liquid after the ageing in clarification by diatomite filter.The mensuration alcoholic strength is 12%v/v.
Single fermentation by saccharomyces cerevisiae and composite yeast fermentation, the quality of wine compares:
Figure BSA00000297729700051
Embodiment 3
(1) select materials, wash select complete, without the red date of canker insect pest, rinse well with water purification;
(2) the red date steam treatment 20min after steam treatment is cleaned;
(3) protect the water that red date that look, hot dipping steam treatment cross adds 6 times, then add parts by weight and be the composite phosphate of 0.08% citric acid and 0.10% as colour protecting agent, process 120min for 75 ℃; Described composite phosphate is sodium hexametaphosphate: the mixture of sodium polyphosphate=1: 1.2;
The red date of (4) making beating, the above-mentioned processing of filtration is pulled an oar, and screenings separates, and removes jujube nuclear, then filters to get jujube juice a and jujube slag b;
(5) add respectively citric acid among enzymolysis jujube juice a and the jujube slag b, regulate pH to 3.5, the control temperature is at 50 ℃, then adds parts by weight among the jujube juice a and be 0.06% polygalacturonase and 0.05 α-amylase, and enzymolysis 25min filters to get jujube juice c; The cellulase of adding 0.07% and 0.03% hemicellulase carry out ultrasonic enzymolysis processing 30min with the probe type ultrasonic extraction apparatus among the jujube slag b under strength of current 0.9A/75w, then filter to get jujube juice d, and jujube juice c and jujube juice d are mixed;
(6) be filled with the SO of 110mg/L in the above-mentioned mixing jujube of the sterilization juice 2, stir, 100 ℃ are carried out germicidal treatment 20min;
(7) inoculation, fermentation will be cooled to 25 ℃ of mixing jujube juice and squeeze into fermentor tank, access respectively 5 good primary yeasts of activation in the fermentor tank: candiyeast, spore debaryomyces hansenii, pichia spp, Ke Leke yeast and yeast saccharomyces cerevisiae, stir, inoculum size is controlled at respectively 3%, adopt temperature controlled fermentation, leavening temperature is controlled at 22 ℃, and fermentation time is 15d;
(8) after the ageing fermentation former wine packed into and be placed with in the container of oak chip, former wine is carried out supersound process, ultrasonic frequency is 25kHz, and power is 50W, and the time is 10min;
(9) red date wine that must clarify is at last filtered the wine liquid after the ageing in clarification by diatomite filter.The mensuration alcoholic strength is 11%v/v.
Single fermentation by saccharomyces cerevisiae and composite yeast fermentation, the quality of wine compares:
Figure BSA00000297729700061

Claims (5)

1. strain compound fermentation type jujube wine brewing method more than a kind, it is characterized in that, use Saccharomyces Cerevisiae in S accharomyces cerevisiae, candiyeast Candida sp., spore debaryomyces hansenii Hanseniaspora sp., pichia spp Pichia sp. and Ke Leke yeast Kloeckera sp. complex ferment, may further comprise the steps:
(1) select materials, wash: select complete, without the red date of canker insect pest, rinse well with water purification;
(2) steam treatment: the steam treatment 10~30min of the red date after cleaning;
(3) protect look, hot dipping: red date that steam treatment is crossed adds 4~8 times water, then adds parts by weight and be the composite phosphate of 0.05%~0.10% citric acid and 0.05%~0.15% as colour protecting agent, processes 90~150min for 60~80 ℃; Described composite phosphate is sodium hexametaphosphate: the mixture of sodium polyphosphate=1: 1~1: 1.5;
(4) making beating, filtration: the red date of above-mentioned processing is pulled an oar, and screenings separates, and removes jujube nuclear, then filters to get jujube juice a and jujube slag b;
(5) enzymolysis: add respectively citric acid among jujube juice a and the jujube slag b, regulate pH to 3~4, the control temperature is at 40~60 ℃, then adds parts by weight among the jujube juice a and be 0.02%~0.10% polygalacturonase and 0.02%~0.08% α-amylase, enzymolysis 15~35min filters to get jujube juice c; Add 0.05%~0.10% cellulase and 0.01%~0.06% hemicellulase among the jujube slag b, under strength of current 0.6A/25w~1.5A/275w, carry out ultrasonic enzymolysis processing 20~40min with the probe type ultrasonic extraction apparatus, then filter to get jujube juice d, jujube juice c and jujube juice d are mixed;
(6) sterilization: the SO that is filled with 90~140mg/L in the above-mentioned mixing jujube juice 2, stir, 100 ℃ are carried out germicidal treatment 15~30min;
(7) inoculation, fermentation: will be cooled to 20 ℃~30 ℃ mixing jujube juice and squeeze into fermentor tank, access respectively 5 good primary yeasts of activation in the fermentor tank: candiyeast, spore debaryomyces hansenii, pichia spp, Ke Leke yeast and yeast saccharomyces cerevisiae, stir, inoculum size is controlled at respectively 1%~10%, adopt temperature controlled fermentation, leavening temperature is controlled at 20~25 ℃, and fermentation time is 10~20d;
(8) ageing: after the fermentation former wine being packed into is placed with in the container of oak chip, and former wine is carried out supersound process, and ultrasonic frequency is 20~30kHz, and power is 40~60W, and the time is 5~15min;
(9) clarification: the wine liquid after the ageing is filtered the red date wine that to clarify at last by diatomite filter.
2. many strain compound fermentation type jujube wines brewing method according to claim 1 is characterized in that,
(1) select materials, wash: select complete, without the red date of canker insect pest, rinse well with water purification;
(2) steam treatment: the red date steam treatment 10min after cleaning;
(3) protect look, hot dipping: red date that steam treatment is crossed adds 8 times water, then adds parts by weight and be the composite phosphate of 0.05% citric acid and 0.15% as colour protecting agent, processes 90min for 80 ℃; Described composite phosphate is sodium hexametaphosphate: the mixture of sodium polyphosphate=1: 1;
(4) making beating, filtration: the red date of above-mentioned processing is pulled an oar, and screenings separates, and removes jujube nuclear, then filters to get jujube juice a and jujube slag b;
(5) enzymolysis: add respectively citric acid among jujube juice a and the jujube slag b, regulate pH to 3, the control temperature is at 40 ℃, then adds parts by weight among the jujube juice a and be 0.10% polygalacturonase and 0.02% α-amylase, and enzymolysis 35min filters to get jujube juice c; The cellulase of adding 0.05% and 0.06% hemicellulase carry out ultrasonic enzymolysis processing 20min with the probe type ultrasonic extraction apparatus among the jujube slag b under strength of current 1.5A/275w, then filter to get jujube juice d, and jujube juice c and jujube juice d are mixed;
(6) sterilization: the SO that is filled with 90mg/L in the above-mentioned mixing jujube juice 2, stir, 100 ℃ are carried out germicidal treatment 30min;
(7) inoculation, fermentation: will be cooled to 20 ℃ of mixing jujube juice and squeeze into fermentor tank, access respectively 5 good primary yeasts of activation in the fermentor tank: candiyeast, spore debaryomyces hansenii, pichia spp, Ke Leke yeast and yeast saccharomyces cerevisiae, stir, inoculum size is controlled at respectively 1%, adopt temperature controlled fermentation, leavening temperature is controlled at 20 ℃, and fermentation time is 20d;
(8) ageing: after the fermentation former wine being packed into is placed with in the container of oak chip, and former wine is carried out supersound process, and ultrasonic frequency is 20kHz, and power is 60W, and the time is 5min;
(9) clarification: the wine liquid after the ageing is filtered the red date wine that to clarify at last by diatomite filter.
3. many strain compound fermentation type jujube wines brewing method according to claim 2 is characterized in that,
(1) select materials, wash: select complete, without the red date of canker insect pest, rinse well with water purification;
(2) steam treatment: the red date steam treatment 30min after cleaning;
(3) protect look, hot dipping: red date that steam treatment is crossed adds 4 times water, then adds parts by weight and be the composite phosphate of 0.10% citric acid and 0.05% as colour protecting agent, processes 150min for 60 ℃; Described composite phosphate is sodium hexametaphosphate: the mixture of sodium polyphosphate=1: 1.5;
(4) making beating, filtration: the red date of above-mentioned processing is pulled an oar, and screenings separates, and removes jujube nuclear, then filters to get jujube juice a and jujube slag b;
(5) enzymolysis: add respectively citric acid among jujube juice a and the jujube slag b, regulate pH to 4, the control temperature is at 60 ℃, then adds parts by weight among the jujube juice a and be 0.02% polygalacturonase and 0.08% α-amylase, and enzymolysis 15min filters to get jujube juice c; The cellulase of adding 0.10% and 0.06% hemicellulase carry out ultrasonic enzymolysis processing 40min with the probe type ultrasonic extraction apparatus among the jujube slag b under strength of current 0.6A/25w, then filter to get jujube juice d, and jujube juice c and jujube juice d are mixed;
(6) sterilization: the SO that is filled with 140mg/L in the above-mentioned mixing jujube juice 2, stir, 100 ℃ are carried out germicidal treatment 15min;
(7) inoculation, fermentation: will be cooled to 30 ℃ of mixing jujube juice and squeeze into fermentor tank, access respectively 5 good primary yeasts of activation in the fermentor tank: candiyeast, spore debaryomyces hansenii, pichia spp, Ke Leke yeast and yeast saccharomyces cerevisiae, stir, inoculum size is controlled at respectively 10%, adopt temperature controlled fermentation, leavening temperature is controlled at 25 ℃, and fermentation time is 10d;
(8) ageing: after the fermentation former wine being packed into is placed with in the container of oak chip, and former wine is carried out supersound process, and ultrasonic frequency is 30kHz, and power is 40W, and the time is 5min;
(9) clarification: the wine liquid after the ageing is filtered the red date wine that to clarify at last by diatomite filter.
4. many strain compound fermentation type jujube wines brewing method according to claim 2 is characterized in that,
(1) select materials, wash: select complete, without the red date of canker insect pest, rinse well with water purification;
(2) steam treatment: the red date steam treatment 20min after cleaning;
(3) protect look, hot dipping: red date that steam treatment is crossed adds 6 times water, then adds parts by weight and be the composite phosphate of 0.08% citric acid and 0.10% as colour protecting agent, processes 120min for 75 ℃; Described composite phosphate is sodium hexametaphosphate: the mixture of sodium polyphosphate=1: 1.2;
(4) making beating, filtration: the red date of above-mentioned processing is pulled an oar, and screenings separates, and removes jujube nuclear, then filters to get jujube juice a and jujube slag b;
(5) enzymolysis: add respectively citric acid among jujube juice a and the jujube slag b, regulate pH to 3.5, the control temperature is at 50 ℃, then adds parts by weight among the jujube juice a and be 0.06% polygalacturonase and 0.05 α-amylase, and enzymolysis 25min filters to get jujube juice c; The cellulase of adding 0.07% and 0.03% hemicellulase carry out ultrasonic enzymolysis processing 30min with the probe type ultrasonic extraction apparatus among the jujube slag b under strength of current 0.9A/75w, then filter to get jujube juice d, and jujube juice c and jujube juice d are mixed;
(6) sterilization: the SO that is filled with 110mg/L in the above-mentioned mixing jujube juice 2, stir, 100 ℃ are carried out germicidal treatment 20min;
(7) inoculation, fermentation: will be cooled to 25 ℃ of mixing jujube juice and squeeze into fermentor tank, access respectively 5 good primary yeasts of activation in the fermentor tank: candiyeast, spore debaryomyces hansenii, pichia spp, Ke Leke yeast and yeast saccharomyces cerevisiae, stir, inoculum size is controlled at respectively 3%, adopt temperature controlled fermentation, leavening temperature is controlled at 22 ℃, and fermentation time is 15d;
(8) ageing: after the fermentation former wine being packed into is placed with in the container of oak chip, and former wine is carried out supersound process, and ultrasonic frequency is 25kHz, and power is 50W, and the time is 10min;
(9) clarification: the wine liquid after the ageing is filtered the red date wine that to clarify at last by diatomite filter.
5. red date wine, it is characterized in that according to claim 1~4 arbitrary described methods make.
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