CN115074206A - Method for preparing acetified esterified liquid by using vinegar residue and application - Google Patents

Method for preparing acetified esterified liquid by using vinegar residue and application Download PDF

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CN115074206A
CN115074206A CN202210787121.XA CN202210787121A CN115074206A CN 115074206 A CN115074206 A CN 115074206A CN 202210787121 A CN202210787121 A CN 202210787121A CN 115074206 A CN115074206 A CN 115074206A
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vinegar
acetified
esterified
enzymolysis
fermentation
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CN115074206B (en
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张旭姣
夏瑶瑶
周景丽
郎繁繁
田莉
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Shanxi Zilin Vinegar Industry Co ltd
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12JVINEGAR; PREPARATION OR PURIFICATION THEREOF
    • C12J1/00Vinegar; Preparation or purification thereof
    • C12J1/04Vinegar; Preparation or purification thereof from alcohol
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00Technologies relating to agriculture, livestock or agroalimentary industries
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Abstract

The invention provides a method for preparing acetified esterified liquid by using vinegar residue and application and a method thereof in an alcohol/acetic acid fermentation stage, which specifically comprises the following steps: carrying out enzymolysis on the vinegar residue; performing enzymolysis on vinegar precipitated mud, yellow wine lees and trickle, preparing a culture solution, and inoculating; preparing acetified esterified solution and carrying out continuous culture; the prepared acetified and esterified solution can be independently applied to the alcohol or acetic acid fermentation stage, and can also be applied to the alcohol and acetic acid fermentation stage. The invention not only can improve the product quality, but also solves the problem of surplus vinegar residue which is a byproduct of solid fermentation vinegar.

Description

Method for preparing acetified esterified liquid by using vinegar residue and application
Technical Field
The invention relates to the technical field of vinegar brewing, in particular to a method for preparing acetified esterification liquid by using vinegar residues and application.
Background
The fragrant components of the grain vinegar mainly comprise various volatile components such as acid, aldehyde, alcohol, ester, phenol, furan, pyrazine and the like. They are contained in a very small amount in vinegar, but can impart a special flavor to vinegar at an appropriate ratio. The aroma characteristics of various kinds of vinegar are the expression of the balance of the aroma components. Among them, esters have fruity odor and are important components for forming the peculiar aroma of vinegar. In the research of the aroma components of mature vinegar, the contents of high-quality vinegar and medium-quality vinegar ethyl acetate are obviously different.
The mature vinegar is prepared by taking sorghum as a main raw material, taking bran, chaff and rice husk as auxiliary materials, taking Daqu made from barley and peas as a saccharification leavening agent, fermenting by alcohol, fermenting by solid acetic acid, and brewing by smoking, aging and other processes. A large amount of vinegar residues are generated after the vinegar pouring link, and the components in the vinegar residues mainly comprise insoluble cellulose, macromolecular protein and fat, and a small amount of residual organic acid and trace elements.
At present, a lot of research reports about recycling of vinegar residue exist, one type is to process the vinegar residue into feed, fertilizer, edible fungus culture medium and nutrient additive, or convert the vinegar residue into energy through microbial fermentation, but the vinegar residue has strong acidity and needs to be recycled after acid reduction pretreatment through fermentation or addition of alkaline substances, so that the method is not applied in large scale; the other method is to treat the vinegar residue as a part of the filling auxiliary material for reuse in the acetic acid fermentation stage, but the vinegar residue has poor water retention property and needs to be compounded with other raw materials for use as the filling auxiliary material. The increase of the yield of the vinegar is accompanied by the generation of more vinegar residue, and how the vinegar residue is used as a necessary byproduct of solid-state fermentation vinegar and can be applied more scientifically and reasonably is a great problem faced by the vinegar industry.
Therefore, how to use vinegar residue to prepare acetified esterified liquid and apply the acetified esterified liquid to mature vinegar brewing is a technical problem which needs to be solved urgently by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a method for preparing acetified esterified liquid by using vinegar residue, and an application and a method thereof in an alcohol/acetic acid fermentation stage, which not only can improve the product quality, but also solve the problem of surplus vinegar residue as a byproduct of solid state fermentation vinegar.
In order to achieve the above effects, one of the objects of the present invention is to provide a method for preparing acetified esterified liquid by using vinegar residue, comprising the steps of:
1) enzymolysis of vinegar residues: adding a proper amount of water into fresh vinegar residue to enable the water content of the fresh vinegar residue to be 80-85%, grinding into vinegar residue thick slurry, adding a proper amount of cellulase into the vinegar residue thick slurry, and performing enzymolysis to obtain vinegar residue zymolyte;
wherein the addition amount of the cellulase is 3.0-5.0 per mill of the mass of the vinegar residue thick slurry;
2) carrying out enzymolysis on vinegar precipitation mud, yellow wine lees and drenched water: uniformly mixing to obtain a mixture, adding acid amylase, and carrying out enzymolysis to obtain a mixed zymolyte;
wherein the addition amount of the acid amylase is 0.6-1.0 per mill of the total mass of the mixture;
3) preparation of a culture solution: uniformly mixing the vinegar residue zymolyte and the mixed zymolyte, adding protease, and performing enzymolysis to obtain a culture solution;
wherein the adding amount of the protease is 1.0-2.0 ‰ of the total mass of the vinegar residue zymolyte and the mixed zymolyte;
4) inoculation: inoculating aroma-producing active dry yeast, esterified red yeast and liquid fermented vinegar precipitate into the culture solution;
wherein, the adding amount of the aroma-producing active dry yeast, the esterified red yeast and the liquid fermented vinegar precipitate respectively accounts for 2.0-4.0 per mill, 1.0-2.0 per mill and 0.5-1.0 percent of the volume of the culture solution;
5) preparation of acetified esterified liquid: step 4), after inoculation, carrying out open fermentation at 28-30 ℃ for 1-3 d; ventilating and stirring once every 2-3d at the temperature of 4-15d and 32-34 ℃, and obtaining acetified esterified mash after fermentation is finished, wherein the liquid part of the acetified esterified mash is acetified esterified liquid; continuously adding the culture solution in the step 3) for continuous culture.
The beneficial effects of adopting the above technical scheme at least include: because a large amount of vinegar residues are generated after the vinegar pouring link of the solid state fermentation vinegar is finished, after physical grinding and enzymolysis, the invention decomposes the insoluble macromolecular fibers and macromolecular organic matters into micromolecular compounds which can be used by microorganisms and then carries out targeted fermentation culture. On one hand, the fresh vinegar residue is treated in time without any storage treatment, so that the cost is reduced; on the other hand, the method is applied to the solid state fermentation vinegar process again, is more beneficial to environmental protection, provides a new mode for post-treatment of the solid state fermentation vinegar residue, and realizes waste utilization.
Preferably, the mass content of the crude fiber after the fresh vinegar residue is air-dried in the step 1) is 28-35%;
the enzymolysis temperature is 45 ℃, the enzymolysis time is 1.5-2.0h, and the mixture is stirred once every 30 min.
Preferably, the mass ratio of the vinegar precipitated mud, the yellow wine lees and the drenching water in the step 2) is 0.8-1.4:1: 2;
the enzymolysis temperature is normal temperature, the enzymolysis time is 1.5-2.0h, and the mixture is stirred once every 30 min.
The beneficial effects of adopting above-mentioned technical scheme include at least: the invention utilizes the waste yellow wine lees, vinegar sediment mud and liquid fermentation vinegar sediment generated in production, and realizes the full utilization of the waste.
Preferably, the vinegar precipitated mud in the step 2) is a precipitated substance generated in the aging process of the mature vinegar, and the main components of the vinegar precipitated mud comprise saccharides, crude fat and protein, and the mass ratio of the saccharides to the crude fat to the protein is 16-20%, 15-18% and 16-20%, respectively.
The beneficial effects of adopting the above technical scheme at least include: the substances are subjected to enzymolysis, so that the nutrients required by fermentation can be provided for microorganisms for producing fragrance, ester and acid, and the like, and the substances with fragrance flavor improve the sensory quality of the mature vinegar. The finished vinegar has softer and more mellow taste.
Preferably, the yellow wine lees in the step 2) are byproducts obtained by squeezing yellow wine, and the main components of the yellow wine lees comprise: starch, protein and ethanol, the mass ratio of which is respectively 10-15%, 20-30% and 6-9%.
Preferably, the mass ratio of the vinegar residue zymolyte to the mixed zymolyte in the step 3) is 5:2.5-4.0, the enzymolysis temperature is 40 ℃, the enzymolysis time is 2-3h, and the pH value is adjusted to 4.5-5.5 after the enzymolysis is finished.
The invention also aims to provide the application of the acetified and esterified liquid, in particular to the application in the alcoholic fermentation stage.
The invention also aims to provide a method for applying the acetified and esterified liquid to the alcoholic fermentation stage, which comprises the following steps:
(1) carrying out puffing treatment on sorghum serving as a main material at the puffing temperature of 110-120 ℃;
(2) feeding the puffed sorghum after puffing is finished, adding the puffed sorghum into water with the temperature raised to 60-65 ℃, wherein the mass ratio of the material to the water is 1: 4.2, adding bran koji, wherein the adding amount of the bran koji is 20-40% of the mass of the sorghum, stirring while adding, and keeping the temperature for 20-30min at 60-65 ℃ after feeding is finished;
(3) rapidly cooling to 28-32 ℃, adding the yeast for making hard liquor, and fermenting, wherein the adding amount of the yeast for making hard liquor is 15-20% of the mass of the sorghum;
the initial fermentation stage comprises open fermentation for 3 days, then sealing fermentation for 10 days, and controlling the temperature at 32 + -2 deg.C during the fermentation stage.
(4) After fermentation, adding acetified esterified liquid, wherein the adding amount of the acetified esterified liquid is 10-20% of the mass of the sorghum, continuously controlling the temperature to be 32 +/-2 ℃, carrying out open fermentation for 2-4d, and finishing the alcoholic fermentation.
(5) After the alcoholic fermentation is finished, adding auxiliary materials to prepare the new fermented grains, wherein the addition amount of the auxiliary materials is based on sorghum, 100% of bran, 100% of rice husk and 40% of rice husk, the moisture content of the new fermented grains is 64-70%, and the alcoholic strength is 4.2-4.5% vol. And (3) firing the fermented grains, wherein the firing amount is 10-15% of the amount of the acetic fermentation fermented grains, and entering an acetic fermentation stage. Turning over the fermented grains every day, fermenting for 1-3 days, controlling the temperature at 38-42 deg.C, fermenting for 4-7 days, controlling the temperature at 42-48 deg.C, controlling the temperature at 38-40 deg.C for 8-9 days, fermenting for 8-9 days, ending the acetic acid fermentation stage when the alcohol content of the vinegar grains is less than or equal to 0.2 vol%, and performing smoking, vinegar pouring and aging stages.
The fourth purpose of the invention is to provide an application of the acetified and esterified liquid, in particular to an application in an acetic acid fermentation stage.
The fifth purpose of the invention is to provide a method for applying the acetified and esterified liquid to the acetic acid fermentation stage, which comprises the following steps:
s1, performing puffing treatment on sorghum serving as a main material at the puffing temperature of 110-120 ℃;
s2, feeding the puffed sorghum after puffing is finished, adding the puffed sorghum into water with the temperature raised to 60-65 ℃, wherein the material-water ratio is 1: 4.2, adding bran koji, wherein the adding amount of the bran koji accounts for 20-40% of the mass of the sorghum, stirring while adding, and preserving heat for 30min after feeding is finished;
s3, rapidly cooling to 28-32 ℃, adding Daqu, and fermenting, wherein the adding amount of the Daqu is 15-20% of the mass of the sorghum;
firstly carrying out open fermentation for 3 days at the initial stage of fermentation, then carrying out closed fermentation for 10 days, and controlling the temperature at 32 +/-2 ℃ at the fermentation stage;
s4, adding auxiliary materials after the alcoholic fermentation is finished, and preparing new fermented grains;
wherein, the auxiliary materials comprise bran, chaff and rice hull, and the addition amounts of the bran, the chaff and the rice hull are respectively 100 percent, 100 percent and 40 percent of the mass of the sorghum; the water content of the new fermented grains is 64-70%, and the alcoholic strength is 4.2-4.5% vol;
s5, adding fire, wherein the fire adding amount is 10-15% of the mass of acetic acid fermentation culture, entering an acetic acid fermentation stage, turning over the culture every day, fermenting for 1-3d, controlling the temperature at 38-42 ℃, fermenting for 4-6 days, controlling the temperature at 42-48 ℃, adding acetified esterification liquid at 7 days of fermentation, wherein the adding amount is 4-6% of the mass of the acetic acid culture, and fermenting for 7-9 days, and controlling the temperature at 35-38 ℃; after fermenting for 8-9 days, when the alcoholic strength of the fermented grains of vinegar is less than or equal to 0.2 vol%, the acetic acid fermentation stage is finished, and the steps of fumigating the fermented grains, pouring vinegar and ageing are carried out.
In order to further optimize the above technical solution, after step S3, the method further includes: adding acetified esterification solution, wherein the addition amount of the acetified esterification solution is 10-20% of the mass of the sorghum, continuously controlling the temperature to be 32 +/-2 ℃, and carrying out open fermentation for 2-4d until the fermentation is finished, and then entering step S4.
In summary, the present invention has at least the following advantages:
(1) because a large amount of vinegar residues are generated after the last vinegar pouring link of the solid state fermentation vinegar, after physical grinding and enzymolysis, the invention decomposes insoluble macromolecular fibers and macromolecular organic matters into micromolecular compounds which can be used by microorganisms and then carries out targeted fermentation culture; the treatment of the fresh vinegar residue is more timely and effective, and no storage treatment is needed, so that the method is applied to the solid state fermentation vinegar process again, is more beneficial to environmental protection, and provides a new mode for the subsequent treatment of the solid state fermentation vinegar residue. Meanwhile, the comprehensive utilization of the waste yellow wine lees, vinegar precipitation mud and liquid fermentation vinegar precipitate is realized.
(2) The invention uses the vinegar residue to prepare the acetified esterified liquid in a continuous culture mode, and is applied to the production of mature vinegar, so that the vinegar residue is efficiently recycled, the content of total esters in the mature vinegar can be effectively increased, and the recycling of the vinegar residue does not depend on modes except vinegar fermentation.
(3) The invention also applies yellow wine lees, vinegar precipitated mud, drenching and liquid fermented vinegar precipitates which are fermentation byproducts, and other nutrient components are not required to be added for microbial fermentation to prepare acetified esterification liquid.
Wherein the yellow wine lees is a byproduct for brewing yellow wine, mainly comprises ethanol, starch, protein, various amino acids and flavor substances, and simultaneously carries various microorganisms beneficial to fermentation, such as yeast, monascus and the like;
the main components of the vinegar precipitated mud are macromolecular starch, protein and various complexes;
the liquid fermented vinegar precipitate is mainly cracked thallus and surviving acetic acid bacteria in the fermentation process, contains rich thallus protein, can provide high acid and alcohol resistance acetic acid bacteria on one hand, and is beneficial to the acetic acid fermentation on the other hand.
The substances can be used in the invention after enzymolysis, provide nutrient substances required by fermentation for microorganisms such as producing fragrance, ester and acid, and the like, and meanwhile, the fragrant flavor substances of the substances further improve the sensory quality of the mature vinegar, so that the finished vinegar has softer and more mellow taste.
(4) The acetified esterified liquid prepared from the vinegar residue is applied to the mature vinegar production process, the advantages of the fermentation process are fully utilized, the acetified esterified liquid is applied to the later stage of the alcoholic fermentation stage, and as aroma-producing yeast and esterified red yeast are used, high acid-resistant and alcohol-resistant acetic acid bacteria in the liquid fermented vinegar are added, the generation of total ester can be continuously improved by using ethanol produced by the fermentation of the alcoholic fermentation stage, the subsequent acetic fermentation process is accelerated, and the acetic fermentation period is shortened;
further, in the later stage of acetic acid fermentation, ethanol with higher concentration still remains in the vinegar culture, and the acetic acid concentration in the vinegar culture is higher at the moment, so that the esterification reaction of aroma-producing yeast and esterified red yeast is facilitated, the total ester content is further improved, the high acid resistance and the high wine resistance acetic acid bacteria can further accelerate the fermentation process, and the fermentation period is shortened.
(5) On one hand, the acetified and esterified liquid prepared by the invention can be independently applied to the alcoholic fermentation stage, the total ester content in the fermented mash is improved by about 25-38%, the total acid content is improved by about 2-5%, and finally, the total ester content in newly drenched vinegar is improved by 15-28%, and the total acid content is improved by 5-10%;
on the other hand, the method can be independently applied to the acetic fermentation stage, the total ester content in the vinegar grains is improved by about 10-20%, the total acid content is improved by about 10-15%, and finally, the total ester content in newly-drenched vinegar is improved by 15-25%, and the total acid content is improved by 18-25%.
If the method is applied to the alcohol fermentation stage and the acetic acid fermentation stage at the same time, the total ester content is improved by 30-40% and the total acid content is improved by 20-35% in the newly sprayed vinegar finally.
(6) After the acetified and esterified liquid prepared by the invention is applied to the mature vinegar fermentation process, compared with the newly drenched vinegar which is not obtained, the same quality can be achieved through the aging process, the aging time is shortened by about 1/5, and the production efficiency of the mature vinegar is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment 1 of the invention provides a method for preparing acetified esterified liquid by using vinegar residues, which comprises the following steps:
1) enzymolysis of vinegar residues: adding a proper amount of water into fresh vinegar residue to enable the water content of the fresh vinegar residue to be 80-85%, grinding into vinegar residue thick slurry, adding a proper amount of cellulase into the vinegar residue thick slurry, and performing enzymolysis to obtain vinegar residue zymolyte;
wherein the addition amount of the cellulase is 3.0-5.0 per mill of the mass of the vinegar residue thick slurry;
2) carrying out enzymolysis on vinegar precipitation mud, yellow wine lees and drenched water: uniformly mixing to obtain a mixture, adding acid amylase, and carrying out enzymolysis to obtain a mixed zymolyte;
wherein the addition amount of the acid amylase is 0.6-1.0 per mill of the total mass of the mixture;
3) preparation of a culture solution: uniformly mixing the vinegar residue zymolyte and the mixed zymolyte, adding protease, and performing enzymolysis to obtain a culture solution;
wherein the adding amount of the protease is 1.0-2.0 ‰ of the total mass of the vinegar residue zymolyte and the mixed zymolyte;
4) inoculation: inoculating aroma-producing active dry yeast, esterified red yeast and liquid fermented vinegar precipitate into the culture solution;
wherein, the adding amount of the aroma-producing active dry yeast, the esterified red yeast and the liquid fermented vinegar precipitate respectively accounts for 2.0-4.0 per mill, 1.0-2.0 per mill and 0.5-1.0 percent of the volume of the culture solution;
5) preparation of acetified esterified liquid: step 4), after inoculation, carrying out open fermentation at 28-30 ℃ for 1-3 d; ventilating and stirring once every 2-3d at the temperature of 4-15d and 32-34 ℃, and obtaining acetified esterified mash after fermentation is finished, wherein the liquid part of the acetified esterified mash is acetified esterified liquid; continuously adding the culture solution in the step 3) for continuous culture.
In order to further optimize the technical scheme, the mass content of the crude fiber after the fresh vinegar residue is air-dried in the step 1) is 28-35 percent;
the enzymolysis temperature is 45 deg.C, the enzymolysis time is 2.0h, and the mixture is stirred once every 30 min.
In order to further optimize the technical scheme, the mass ratio of the vinegar precipitated mud, the yellow wine lees and the drenching water in the step 2) is 0.8-1.4:1: 2;
the enzymolysis temperature is normal temperature, the enzymolysis time is 2.0h, and the mixture is stirred once every 30 min.
In order to further optimize the technical scheme, the vinegar precipitated mud in the step 2) is a precipitated substance generated in the aging process of the mature vinegar, and the main components of the vinegar precipitated mud comprise saccharides, crude fat and protein, wherein the mass percentages of the saccharides, the crude fat and the protein are respectively 16-20%, 15-18% and 16-20%.
In order to further optimize the technical scheme, the yellow wine lees are byproducts obtained by squeezing yellow wine, and the main components of the yellow wine lees comprise: starch, protein and ethanol, the mass ratio of which is respectively 10-15%, 20-30% and 6-9%.
In order to further optimize the technical scheme, the mass ratio of the vinegar residue zymolyte to the mixed zymolyte in the step 3) is 5:2.5-4.0, the enzymolysis temperature is 40 ℃, the enzymolysis time is 2-3h, and the pH value is adjusted to 4.5-5.5 after the enzymolysis is finished.
The procedure of example 1 was repeated to prepare a three-time acetified and esterified liquid, and the results of the examination of the obtained acetified and esterified liquid are shown in Table 1.
TABLE 1 detection results of acetified esterification solution
Figure BDA0003729149300000091
As can be seen from the data in table 1; in addition to the total acid and ester contents, the amount of microorganisms in the acetified and esterified solution can directly affect the fermentation process and the quality of the final new vinegar.
Example 2
Embodiment 2 of the present invention provides a method for applying an esterified solution of acetic acid to alcoholic fermentation based on embodiment 1, which specifically comprises the following steps:
(1) carrying out puffing treatment on sorghum serving as a main material at the puffing temperature of 110-120 ℃;
(2) feeding the puffed sorghum after the puffing is finished, adding the puffed sorghum into water with the temperature raised to 60-65 ℃, wherein the material-water ratio is 1: 4.2, adding bran koji, wherein the adding amount of the bran koji is 20-40% of the mass of the sorghum while stirring, and keeping the temperature for 20-30min at 60-65 ℃ after the feeding is finished;
(3) rapidly cooling to 28-32 ℃, adding the yeast for making hard liquor, and fermenting, wherein the adding amount of the yeast for making hard liquor is 15-20% of the mass of the sorghum;
the initial fermentation stage comprises open fermentation for 3 days, then sealing fermentation for 10 days, and controlling the temperature at 32 + -2 deg.C during the fermentation stage.
(4) After fermentation, adding acetified esterified liquid, wherein the adding amount of the acetified esterified liquid is 10-20% of the mass of the sorghum, continuously controlling the temperature to be 32 +/-2 ℃, carrying out open fermentation for 2-4d, and finishing the alcoholic fermentation.
(5) After the alcoholic fermentation is finished, adding auxiliary materials to prepare the new fermented grains, wherein the addition amount of the auxiliary materials is based on sorghum, 100% of bran, 100% of rice husk and 40% of rice husk, the moisture content of the new fermented grains is 64-70%, and the alcoholic strength is 4.2-4.5% vol. And (3) firing the fermented grains, wherein the firing amount is 10-15% of the amount of the acetic fermentation fermented grains, and entering an acetic fermentation stage. Turning over the fermented grains every day, fermenting for 1-3 days, controlling the temperature at 38-42 deg.C, fermenting for 4-7 days, controlling the temperature at 42-48 deg.C, controlling the temperature at 35-38 deg.C for 8-9 days, fermenting for 8-9 days, ending the acetic acid fermentation stage when the alcohol content of the vinegar grains is less than or equal to 0.2 vol%, and performing smoking, vinegar pouring and aging stages.
The results of physico-chemical measurements of the mash and the freshly poured vinegar after the acetified and esterified liquid prepared in example 1 was applied to the alcoholic fermentation stage in example 2 are shown in tables 2 and 3.
Both the mash of the control group and the mature vinegar of the control group are the condition without adding acetified esterification liquid in the step (4);
table 2 example 2 effect of acetified esterified liquid on beer mash in alcohol fermentation stage
Figure BDA0003729149300000101
TABLE 3 influence of acetified esterified liquid applied to alcoholic fermentation stage on quality of new vinegar
Figure BDA0003729149300000102
Example 3
Embodiment 3 of the present invention provides a method for applying an esterified acetic acid solution to an acetic acid fermentation stage based on embodiment 1, which specifically includes the following steps:
s1, performing puffing treatment on sorghum serving as a main material at the puffing temperature of 110-120 ℃;
s2, feeding after the puffing is finished, adding the puffed sorghum into water with the temperature being raised to 60-65 ℃, wherein the material-water ratio is 1: 4.2, simultaneously adding bran koji, wherein the adding amount of the bran koji is 20-40% of the mass of the sorghum, stirring while adding, and preserving heat for 30min after the feeding is finished;
s3, rapidly cooling to 28-32 ℃, adding Daqu, and fermenting, wherein the adding amount of the Daqu is 15-20% of the mass of the sorghum;
firstly carrying out open fermentation for 3 days at the initial stage of fermentation, then carrying out closed fermentation for 10 days, and controlling the temperature at 32 +/-2 ℃ at the fermentation stage;
s4, adding auxiliary materials after the alcoholic fermentation is finished, and preparing new fermented grains;
wherein, the auxiliary materials comprise bran, chaff and rice hull, and the addition amounts of the bran, the chaff and the rice hull are respectively 100 percent, 100 percent and 40 percent of the mass of the sorghum; the water content of the new fermented grains is 64-70%, and the alcoholic strength is 4.2-4.5% vol;
s5, fermented grains: the ignition amount is 10-15% of the mass of the acetic acid fermentation grains, the acetic acid fermentation stage is started, the grains are turned over every day, the fermentation is carried out for 1-3 days, the temperature is controlled at 38-42 ℃, the fermentation is carried out for 4-6 days, the temperature is controlled at 42-48 ℃, the acetified esterification solution is added in the fermentation for 7 days, the addition amount is 4-6% of the amount of the vinegar grains, the fermentation is carried out for 7-9 days, and the temperature is controlled at 35-38 ℃; after fermenting for 8-9 days, when the alcoholic strength of the fermented grains of vinegar is less than or equal to 0.2 vol%, the acetic acid fermentation stage is finished, and the steps of fumigating the fermented grains, pouring vinegar and ageing are carried out.
The results of physicochemical measurements of the fermented grains of vinegar and the newly poured vinegar after the acetified and esterified solution prepared in example 1 was applied to the acetic fermentation stage in example 3 are shown in tables 4 and 5:
the control group vinegar culture and the control group mature vinegar are both the case of not adding the acetified and esterified solution in the step S5.
TABLE 4 EXAMPLE 3 Effect of the acetified esterified liquid applied to the fermented grains of vinegar in the acetic acid fermentation stage
Figure BDA0003729149300000111
Figure BDA0003729149300000121
TABLE 5 EXAMPLE 3 Effect of the acetified esterification liquid used in the acetic fermentation stage on the quality of new vinegar
Figure BDA0003729149300000122
Example 4
Embodiment 4 of the present invention provides a method for applying an esterified acetic acid solution to alcoholic fermentation based on embodiment 3, and the specific differences are as follows:
further included after step S3 is: adding acetified esterified liquid, wherein the adding amount of the acetified esterified liquid is 10-20% of the mass of the sorghum, continuously controlling the temperature to be 32 +/-2 ℃, and carrying out open fermentation for 2-4d until the fermentation is finished, and then entering step S4.
Example 4 physical and chemical detection results of the fermented grains, the vinegar grains and the newly drenched vinegar are shown in tables 6, 7 and 8:
the control fermented mash and the control vinegar mash are not included after the step S3, and the method further comprises the following steps: adding acetified esterified liquid, wherein the adding amount of the acetified esterified liquid is 10-20% of the mass of the sorghum, continuously controlling the temperature to be 32 +/-2 ℃, and carrying out open fermentation for 2-4d until the fermentation is finished, and then carrying out the operation of step S4.
TABLE 6 results of physico-chemical measurements of the mash
Figure BDA0003729149300000123
TABLE 7 physicochemical detection results of fermented grains of vinegar
Figure BDA0003729149300000124
Figure BDA0003729149300000131
TABLE 8 physicochemical detection results of new drenched vinegar
Figure BDA0003729149300000132
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed in the embodiment corresponds to the method disclosed in the embodiment, so that the description is simple, and the relevant points can be referred to the description of the method part.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. A method for preparing acetified esterified liquid by using vinegar residue is characterized by comprising the following steps:
1) enzymolysis of vinegar residues: adding a proper amount of water into fresh vinegar residue to enable the water content of the fresh vinegar residue to be 80-85%, grinding into vinegar residue thick slurry, adding a proper amount of cellulase into the vinegar residue thick slurry, and performing enzymolysis to obtain vinegar residue zymolyte;
wherein the addition amount of the cellulase is 3.0-5.0 per mill of the mass of the vinegar residue thick slurry;
2) carrying out enzymolysis on vinegar precipitation mud, yellow wine lees and drenched water: uniformly mixing the vinegar precipitation mud, the yellow wine lees and the drenching water to obtain a mixture, adding acid amylase for enzymolysis to obtain a mixed zymolyte;
wherein the addition amount of the acid amylase is 0.6-1.0 per mill of the mass of the mixture;
3) preparation of culture solution: uniformly mixing the vinegar residue zymolyte and the mixed zymolyte, adding protease, and carrying out enzymolysis to obtain a culture solution;
wherein the adding amount of the protease is 1.0-2.0 ‰ of the total mass of the vinegar residue zymolyte and the mixed zymolyte;
4) inoculation: inoculating aroma-producing active dry yeast, esterified red yeast and liquid fermented vinegar precipitate into the culture solution;
wherein, the adding amount of the aroma-producing active dry yeast, the esterified red yeast and the liquid fermented vinegar precipitate respectively accounts for 2.0-4.0 per mill, 1.0-2.0 per mill and 0.5-1.0 percent of the volume of the culture solution;
5) preparation of acetified esterified liquid: step 4), after inoculation, carrying out open fermentation at 28-30 ℃ for 1-3 d; ventilating and stirring once every 2-3d at the temperature of 4-15d and 32-34 ℃, and obtaining acetified esterified mash after fermentation is finished, wherein the liquid part of the acetified esterified mash is acetified esterified liquid; continuously adding the culture solution in the step 3) for continuous culture.
2. The method for preparing acetified esterified liquid by using vinegar residue as claimed in claim 1, wherein the mass content of crude fiber after air drying of the fresh vinegar residue in the step 1) is 28-35%;
the enzymolysis temperature is 45 ℃, the enzymolysis time is 1.5-2.0h, and the mixture is stirred once every 30 min.
3. The method for preparing acetified esterified liquid by utilizing vinegar residues as claimed in claim 1, wherein the mass ratio of the vinegar precipitated mud, the yellow wine lees and the water in the step 2) is 0.8-1.4:1: 2;
the enzymolysis temperature is normal temperature, the enzymolysis time is 1.5-2.0h, and the mixture is stirred once every 30 min.
4. The method as claimed in claim 1, wherein the vinegar precipitated sludge in step 2) is a precipitated substance produced during aging of mature vinegar, and the precipitated substances mainly comprise saccharides, crude fats and proteins, and the mass ratio of the precipitated substances is 16-20%, 15-18% and 16-20%, respectively.
5. The method for preparing acetified esterified liquid by utilizing vinegar residue as claimed in claim 1, wherein the yellow wine residue in step 2) is a byproduct obtained by squeezing yellow wine, and comprises the following main components: starch, protein and ethanol, the mass ratio of which is respectively 10-15%, 20-30% and 6-9%.
6. The method for preparing acetified esterified liquid by using vinegar residue as claimed in claim 1, wherein the mass ratio of the vinegar residue zymolyte and the mixed zymolyte in the step 3) is 5:2.5-4.0, the enzymolysis temperature is 40 ℃, the enzymolysis time is 2-3h, and the pH value is adjusted to 4.5-5.5 after the enzymolysis is finished.
7. Use of an acetified and esterified liquid, wherein the acetified and esterified liquid prepared by the method according to any one of claims 1 to 6 is used in an alcoholic fermentation stage.
8. A method for applying acetified liquor to alcoholic fermentation, which is characterized in that the acetified liquor prepared by the method of any one of claims 1 to 6 is added in the alcoholic fermentation stage at the temperature of 32 +/-2 ℃ with the addition of 10 to 20 percent and is subjected to open fermentation.
9. Use of an acetylated esterification solution prepared according to the process of any of claims 1 to 6 in an acetic fermentation stage.
10. A method for applying acetified liquor to acetic fermentation stage is characterized in that the acetified liquor prepared by the method of any one of claims 1 to 6 is added in the acetic fermentation stage, and the addition amount of the acetified liquor is 4-6% of the mass of the fermented grains of vinegar.
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