CN113493729A

CN113493729A - Vinasse processing method, vinegar and preparation method thereof

Info

Publication number: CN113493729A
Application number: CN202010190284.0A
Authority: CN
Inventors: 石小和
Original assignee: Individual
Current assignee: Individual
Priority date: 2020-03-18
Filing date: 2020-03-18
Publication date: 2021-10-12

Abstract

The application belongs to the technical field of biology, and particularly relates to a vinasse processing method, which comprises the following steps: soaking elution vinasse by using a leaching solvent to separate husk and skin substances from the vinasse, wherein the rest substances in the vinasse and the leaching solvent form an elution suspension; filtering the chaff, the bark material and the elution suspension from the whole stillage; distilling off the leaching solvent in the elution suspension to obtain a distillation residue; solves the problems of resource waste and environmental pollution caused by the prior vinasse processing technology, and realizes high-value utilization and clean production of the vinasse.

Description

Vinasse processing method, vinegar and preparation method thereof

Technical Field

The invention belongs to the technical field of biology, and particularly relates to a vinasse processing method, vinegar and a preparation method of the vinegar.

Background

Vinasse is solid waste generated in the brewing process, and the yield of the vinasse is huge. In 2016, the total yield of Chinese liquor reaches 1358.4 ten thousand tons, in 2017 to 2018, and the production capacity is increased by 172.14 ten thousand tons per year. By conservative calculation, the yield of only white spirit vinasse in 2020 can reach 5 million tons. Fresh vinasse contains a large amount of nutrient substances and is extremely easy to decay rapidly under the action of microorganisms due to high moisture. The storage period of the fresh grains is generally not longer than 2-3 days, otherwise a series of deterioration characteristics such as smelling and hair growing are generated. The accumulation of a large amount of vinasse not only occupies land resources, but also generates stink after the vinasse is decayed, and the stink acts on human olfactory organs through air media, so that the human health is harmed; in addition, leachate produced from the rotten vinasse is acidic, and if the leachate enters soil, the soil is also acidified. Due to various pollution problems caused by the fresh lees, the fresh lees need to be treated timely and effectively.

The main application directions for vinasse recycling at present include: producing middle-low quality wine; fermenting to produce methane or fuel ethanol; fermenting to produce biological feed as culture medium of edible fungus, extracting dietary fiber and fragrant components, and producing organic fertilizer. However, the existing treatment process for the utilization direction of the vinasse has low treatment efficiency and long time consumption, and is not suitable for timely treatment and storage of a large batch of vinasse.

Therefore, obtaining a vinasse processing method which can realize large-scale industrialization of vinasse and has high resource utilization rate becomes a problem to be solved in the field.

Disclosure of Invention

In view of the above, the present invention aims to provide a vinasse processing method, vinegar and a preparation method thereof, so as to solve the problems of resource waste and environmental pollution caused by the existing vinasse processing technology, and realize high-value utilization and clean production of vinasse.

In order to achieve the above object, the first aspect of the present invention provides the following technical solutions: a vinasse processing method comprises the following steps:

soaking elution vinasse by using a leaching solvent to separate husk and skin substances from the vinasse, wherein the rest substances in the vinasse and the leaching solvent form an elution suspension;

filtering the chaff, the bark material and the elution suspension from the whole stillage;

the leaching solvent in the elution suspension is distilled off to obtain a distillation residue.

Optionally, the step of soaking an elution stillage with a leaching solvent to separate hulls and skin species from the stillage, the remaining species in the stillage forming an elution suspension with the leaching solvent, comprises:

soaking and eluting the vinasse by using a leaching and desolventizing agent, and stirring the vinasse at intervals of preset time; and when the husk and the skin substances in the vinasse are separated, the rest substances in the vinasse and the leaching solvent form an elution suspension, and the stirring treatment operation is finished.

Optionally, in the step of soaking and eluting the distiller's grains by using the leaching and desolventizing agent, the weight part ratio of the leaching and desolventizing agent to the distiller's grains is 1-30: 1.

optionally, the leaching and removing solvent is any one of ethanol, acetic acid, methanol, acetone, acetonitrile, petroleum ether, benzene, toluene, chloroform, diethyl ether, ethyl acetate, dichloroethane, n-butanol, propanol or isopropanol or a mixture of at least two of the above in any proportion.

Optionally, the leaching and desolventizing agent is ethanol, and in the step of leaching and eluting the vinasse by using the leaching and desolventizing agent, the weight part ratio of the leaching and desolventizing agent to the vinasse is 1-8: 1.

the second aspect of the invention provides the technical scheme that: a method for preparing vinegar by using vinasse comprises the following steps:

collecting the chaff and the distillation residue obtained by the above-mentioned spent grain treatment method;

fermenting the chaff and the distillation residue with a carrier comprising a microorganism to obtain a fermentation product;

sequentially carrying out fermented grains, fermented grains smoking and vinegar pouring treatment on the fermentation product to obtain vinegar liquid;

freezing the vinegar liquid until the surface of the vinegar liquid is solidified to obtain vinegar blocks;

melting the vinegar blocks, and collecting melted concentrated vinegar liquid;

aging the concentrated vinegar liquid to obtain vinegar;

wherein the carrier containing the microorganism is one or more than two of famous wine yeast, famous wine fermented grains and famous vinegar fermented grains.

Preferably, the carrier containing the microorganisms is fermented famous vinegar, and the fermented famous vinegar is fermented aspongopus savory ester vinegar.

Preferably, the step of fermenting the chaff and the distillation residue with a carrier containing a microorganism to obtain a fermentation product comprises:

adding a carrier containing microorganisms and grain processing skin substances into the rice husks and the distillation residues, uniformly mixing, and fermenting for 0-15 days to obtain a fermentation product; wherein the weight part ratio of the distillation residue, the chaff, the carrier containing the microorganism and the grain processing skin substance is 100: 30-70: 50-200: 0 to 60.

adding grain raw materials to be fermented and carriers containing microorganisms after soaking, steaming and stewing into the distillation residues and the rice husks, uniformly mixing, carrying out anaerobic fermentation, adding grain processing skin substances as loose materials after fermenting for 15-730 days, carrying out aerobic fermentation after uniformly mixing, and fermenting for 8-15 days to obtain fermentation products;

wherein the distillation residue, the chaff, the grain raw material to be fermented, the carrier containing the microorganism and the grain processing skin substance are mixed according to the following weight part ratio of 100: 30-70: 30-150: 55-180: 80-300.

The third aspect of the invention provides the technical scheme that: edible vinegar is prepared by the method for preparing edible vinegar from distiller's grains.

Compared with the prior art, the invention has the following beneficial effects:

according to the embodiment of the application, the vinasse is soaked by the soaking solvent, so that large batches of vinasse can be treated in a centralized manner, the treated materials can be stored in the closed container for a long time, and the storage time can be prolonged.

According to the application, for example, the vinasse is soaked by the alcohol, the vinasse can be effectively prevented from being rotten due to the bacteriostatic action of the alcohol, the storage time is further prolonged, and the alcohol can be recycled by distilling and recovering the alcohol; the vinasse also contains rich aroma substances, and the aroma substances are enriched in the edible alcohol through multiple soaking and distillation treatments, so that the secondary vinasse wine containing rich aroma substances is finally formed. After the vinasse is subjected to alcohol treatment, volatile aroma substances of the vinasse are enriched in alcohol, the remaining non-volatile part also comprises protein, amino acid, lipid, fiber, microorganism, trace elements and the like, and the vinasse is fermented based on a carrier containing the microorganism, so that the nutrient substances in the vinasse are fully utilized, the waste of resources is avoided, and the high-valued utilization and clean production of the vinasse are realized. The obtained secondary vinasse wine and vinegar are high-quality and high-value products.

Detailed Description

In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which embodiments of the invention belong. If a definition set forth in this section is contrary to or otherwise inconsistent with a definition set forth in the patents, patent applications, published patent applications, and other publications that are herein incorporated by reference, the definition set forth in this section prevails over the definition that is incorporated herein by reference.

In addition, the weight of the related components mentioned in the description of the embodiments of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, it is within the scope of the disclosure of the description of the embodiments of the present invention to scale up or down the content of the related components according to the description of the embodiments of the present invention. Specifically, the weight described in the description of the embodiments of the present invention may be a unit of weight known in the chemical industry, such as μ g, mg, g, and kg.

The first aspect of the embodiment of the invention provides a vinasse processing method, which comprises the following steps:

s101, soaking and eluting vinasse by using a leaching solvent to separate husk and skin substances in the vinasse, wherein the rest substances in the vinasse and the alcohol form an elution suspension;

wherein the skin material can be bran, sorghum peel, etc.; the leaching solvent can be hydrophilic solvent or lipophilic solvent, the leaching solvent can be used for soaking and separating chaff and skin substances in the vinasse, and can be used for soaking, eluting and separating usable substances such as lipid substances in the vinasse, and the lipid substances can be used for medicinal products, such as medicines for resisting malignant cell proliferation, scavenging free radicals, resisting oxidation, resisting virus cell proliferation, copying virus nucleic acid and the like.

By way of example only, and not limitation, the leaching solvent may be any one of ethanol, acetic acid, methanol, acetone, acetonitrile, petroleum ether, benzene, toluene, chloroform, diethyl ether, ethyl acetate, dichloroethane, n-butanol, propanol, or isopropanol, or a mixture of at least two or more thereof mixed in any ratio. For example, the leaching and removing solvent can be acetic acid, the leaching and removing solvent can be a mixture of ethanol and methanol mixed in any proportion, the leaching and removing solvent can be a mixture of petroleum ether, benzene and toluene mixed in any proportion, and the leaching and removing solvent can be a mixture of methanol, acetone, acetonitrile, petroleum ether and benzene mixed in any proportion; the weight part ratio of the leaching and desolventizing agent to the vinasse is 1-30: 1, preferably, the weight part ratio of the leaching and desolventizing agent to the vinasse is 1: 1,2: 1,3: 1,4: 1,5: 1,6: 1,7: 1,8: 1,10: 1,15: 1,20: 1,25: 1 or 30: 1.

Preferably, the leaching and desolventizing agent can be ethanol, and the weight part ratio of the ethanol to the vinasse is 1-8: 1; if the soaking solvent can be edible alcohol, the weight part ratio of the alcohol to the vinasse can be 1-8: 1, preferably, the weight part ratio of the alcohol to the vinasse is 1: 1,2: 1,3: 1,4: 1,5: 1,6: 1,7: 1, or 8:

the step of soaking and eluting the vinasse by using the leaching and desolventizing agent comprises the following steps of,

soaking and eluting the vinasse by using a leaching and desolventizing agent, and stirring the vinasse at intervals of preset time; and when the husk and the skin substances in the vinasse are separated, the rest substances in the vinasse and the alcohol form an elution suspension, and the stirring treatment operation is finished.

The preset time can be set according to the scale of the vinasse, such as 100t of vinasse, the preset time can be 1 day, the vinasse needs to be stirred every other day, and the vinasse does not need to be stirred after 1 week; for example, for 1000t of distiller's grains, the preset time can be 3 days, and the distiller's grains need to be stirred every 3 days and do not need to be stirred after 2 weeks; the ethanol or the alcohol is used as the solvent for the vinasse elution, so that the husk and the skin substances in the vinasse can be separated to the maximum extent on the basis of not introducing other irrelevant substances.

S102, filtering and separating the chaff, the skin substances and the elution suspension in the vinasse; the separated chaff can be used for brewing vinegar and producing fertilizer; the separated peel can be used for brewing vinegar, and also can be used for producing food and high-end feed.

Specifically, the husk in the distiller's grains is filtered and separated firstly, and a fence type screen with the thickness of 0.8-2.5 mm or a round hole type screen with the thickness of 1.5-2.5 mm can be adopted for filtering and separating; then, the skin substances and the elution suspension are separated by filtration, and a round hole type screen or a square screen with the thickness of 0.5-1.2 mm can be adopted.

S103, distilling to remove the leaching solvent in the elution suspension to obtain a distillation residue. Wherein the distillation residue is impregnated with a desolvation agent such as alcohol in an amount of 0 to 20% by weight. The distillation may partially remove the leaching solvent such as alcohol from the elution suspension, e.g. 5%, 8%, 10% or 15% of the remaining distillation residue, or may completely remove the alcohol from the elution suspension. The alcohol removed by distillation can be recycled as solvent alcohol for soaking and eluting the vinasse in the step S101, the recycled alcohol is recovered after 5-15 times of soaking and eluting the vinasse, separation and distillation treatment, so that high-quality secondary vinasse wine is obtained, and the alcohol used for soaking and eluting the vinasse again can be replaced by new alcohol. The distillation residue can be used for high-value utilization of vinasse; the distillation residue can also be stored in a sealed manner, so that the storage time is further prolonged. The embodiment of the application adopts the alcohol or the ethanol to soak the vinasse, so that the vinasse can be effectively prevented from being rotten due to the bacteriostatic action, the storage time is correspondingly prolonged, and the alcohol can be recycled by distilling and recovering the alcohol; the vinasse also contains rich aroma substances, and the aroma substances are enriched in the edible alcohol through multiple soaking and distillation treatments, so that the secondary vinasse wine containing rich aroma substances is finally formed.

Due to the characteristics of the wine brewing process, the vinasse output time is usually concentrated within 1-2 months, large batches of vinasse need to be processed in time, the traditional processing method is limited in processing amount, low in processing efficiency and long in time consumption, the vinasse is soaked in the soaking solvent, large batches of vinasse can be processed in a concentrated mode, the processed materials can be stored in the closed container for a long time, and the storage time can be prolonged.

The second aspect of the embodiments of the present invention provides a method for preparing vinegar by using vinasse, including the following steps:

s201, fermenting the chaff obtained in the step S102 and the distillation residue obtained in the step S103 by using a carrier containing microorganisms to obtain a fermentation product;

wherein the carrier containing the microorganism is one or more than two of famous wine yeast, famous wine fermented grains and famous vinegar fermented grains. Preferably, the carrier containing the microorganisms is fermented substrate of the koji balsamiferous vinegar, wherein the fermented substrate of the koji balsamiferous vinegar is fermented substrate of the koji balsamiferous vinegar generated in the brewing process; the koji aromatic ester vinegar is a raw stock vinegar prepared by utilizing famous wine fungus series Daqu in alcohol fermentation.

In step S201, one of the fermentation methods is:

adding carriers containing microorganisms such as fermented grains of aspongopus fragrant ester vinegar and grain processing skins into the chaff and the distillation residues, uniformly mixing, and fermenting for 0-15 days to obtain fermentation products; wherein the weight part ratio of the distillation residue, the chaff, the carrier containing the microorganism and the grain processing skin substance is 100: 30-70: 50-200: 0 to 60. In this manner, the chaff and the distillation residue may be used as the main material.

When only a carrier containing microorganisms such as the fermented substrate of the kajixiangzhi vinegar is added into the chaff and the distillation residue, and the grain processing skin substances are not added, the chaff, the distillation residue and the carrier containing the microorganisms such as the fermented substrate of the kajixiangzhi vinegar can be uniformly mixed and then fermented without fermentation for 0 day.

The chaff and the distillation residue may be placed in a fermentation unit for fermentation. The fermentation device may be a glass tank or a ceramic jar, but the fermentation device is not limited to the above glass tank or ceramic jar, and may include any device that can ferment the chaff and the distillation residue.

Preferably, the koji balsam vinegar residue fermented for 6 to 8 days may be added to the chaff and the distillation residue.

In step S201, the other mode of fermentation is:

adding grain raw materials to be fermented after soaking, steaming and stewing and carriers containing microorganisms such as famous wine daqu or koji balsam vinegar mash into the distillation residues and the rice husks, uniformly mixing, carrying out anaerobic fermentation, adding grain processing leather substances as loose materials after fermenting for 15-730 days, carrying out aerobic fermentation after uniformly mixing, and fermenting for 8-15 days to obtain fermentation products; in this manner, the distillation residue and the chaff may be used as auxiliary materials.

In this way, the distillation residue and the chaff undergo more fermentation stages, longer fermentation times and more secondary metabolites produced by the microorganisms during fermentation; and the distillation residue reacts with crude protein and other substances contained in the chaff more fully, and the proportion of the generated small molecular peptides is larger.

Preferably, the koji balsam vinegar residue fermented for 6 to 8 days may be added to the distillation residue and the chaff.

S202, sequentially carrying out unstrained spirits, unstrained spirits smoking and vinegar pouring treatment on the fermentation product to obtain vinegar liquid;

specifically, the step of the fermented grains comprises the following steps:

carrying out unstrained spirits treatment on the fermentation product for 15-720 days under a sealed condition to obtain an unstrained spirits product; the temperature of the aging environment is not particularly limited, and may be generally performed at room temperature.

The fermentation product may be filled when placed in a sealed container, or may leave a small space to trap a small amount of air.

As a specific embodiment of the invention, the fermentation product can be placed into a glass jar and then compacted and filled, a cover with a sealing plug is screwed, and sealed by gypsum and glue, so as to ensure strict sealing, and the fermented grains are aged for 15-720 days in an environment of 2-25 ℃.

The steps of smoking the unstrained spirits comprise:

heating a part of the aged fermentation substrate product by slow fire, and smoking the fermentation substrate for 4-8 days at 70-90 ℃ to obtain a smoked fermentation substrate product.

The vinegar pouring method comprises the following steps:

adding water and light vinegar into the other part of the aged wine product, soaking for more than 12h, and leaching out the vinegar to obtain a first vinegar; wherein the total weight of the other part of the fermented grain product, water and light vinegar liquid is 2-3 times of the weight of the other part of the fermented grain product, and the water and the light vinegar liquid can be mixed in any proportion; the light vinegar liquid can be the light vinegar liquid of the last vinegar drenching and can also be the light vinegar liquid generated after the vinegar residue water separation.

Heating the first vinegar solution to boiling state such as 100 deg.C, injecting into the product of smoked grains, soaking for more than 10 hr, and leaching to obtain second vinegar solution.

S203, freezing the vinegar liquid until the surface of the vinegar liquid is solidified to obtain vinegar blocks;

in the step of freezing treatment, the freezing treatment can be carried out at-50 ℃ to-1 ℃; the freezing environment may preferably be a freezer, freezer or refrigerator, frozen to a substantially solid block of vinegar. Since the vinegar liquid has a complicated composition and contains acetic acid, lactic acid, amino acids, various aromatic substances, and the like, a partially thick liquid may be contained in the vinegar cake formed after freezing.

The vinegar block obtained by freezing is not required to be solid, and the coagulated state may be a vinegar block which is just coagulated on the surface and is substantially solid, may be a vinegar block which is completely coagulated from the inside to the outside, or may be a vinegar block which is in between the two states.

S204, melting the vinegar blocks, and collecting melted concentrated vinegar liquid;

and (3) putting the frozen product, namely the vinegar block, at 0-20 ℃ for melting treatment, and collecting melted concentrated vinegar liquid.

S205, ageing the concentrated vinegar liquid to obtain vinegar;

placing the concentrated vinegar liquid in a closed container such as a brewing jar, and aging in the open air for at least 12 months to obtain edible vinegar. In the open air environment, as the aging time is prolonged, the total amount of aroma components tends to be reduced due to volatilization loss of part of aroma components or aging conversion into other aroma components, but the types of the aroma components are increased, so that the aroma is softer.

After the vinasse is subjected to alcohol treatment, volatile aroma substances of the vinasse are enriched in alcohol, the remaining non-volatile part also comprises protein, amino acid, lipid, fiber, microorganism, trace elements and the like, and the vinasse is fermented based on a carrier containing the microorganism, so that the nutrient substances in the vinasse are fully utilized, the waste of resources is avoided, and the high-valued utilization and clean production of the vinasse are realized. The obtained secondary vinasse wine and vinegar are high-quality and high-value products.

In the embodiment of the invention, the famous wine refers to various types of white spirits of which the famous wine titles are obtained by five national wine evaluation meetings in China since 1952, and the famous wine comprises but is not limited to: maotai, wuliangye, Luzhou Laojiao, Jiannanchun, Fenjiu, Yanghe Daqu, Lang liquor, Gujing tribute liquor, Dong liquor, Xifeng liquor, Shuanggou Daqu and the like can be prepared in the environment of famous liquor production or can be directly purchased from local Daqu manufacturers. Preferably, the famous wine can be Maotai, wuliangye, Luzhou Laojiao, Jiannanchun wine, Dong wine, and Gujing tribute wine; further preferably, the famous wine refers to thatch, wuliangye and Luzhou Lao jiao.

Wherein the preparation of the aspongopus ester vinegar comprises the following steps: soaking the grain raw material in water, steaming, and stewing to obtain the raw material to be fermented; and sequentially carrying out alcoholic fermentation, acetic fermentation, fumigating, vinegar pouring and ageing on the raw materials to be fermented.

Preferably, between the vinegar pouring and the aging, the method further comprises the following steps: freezing vinegar; the frozen vinegar comprises: freezing the vinegar liquid into solid vinegar blocks, then melting the vinegar blocks, and collecting the melted thick vinegar liquid.

As a specific embodiment of the invention, the preparation of the aspongopus ester vinegar comprises the following steps:

s01, adding water accounting for 30-60% of the weight of the cereal raw material into the cereal raw material for infiltration to ensure that the cereal raw material fully absorbs water to obtain the infiltrated cereal raw material;

s02, steaming the grain raw material soaked in the S01 for 90-180 min to obtain a steamed material;

s03, adding water accounting for 180-350% of the weight of the grain raw material into the steamed material obtained in the step S02, and stewing for 15-80 min under the action of steam to obtain a raw material to be fermented;

s04, adding famous wine fungus series yeast strain which accounts for 20-120% of the weight of the cereal raw material into the raw material to be fermented obtained in the step S03, and uniformly mixing;

s05, adding water accounting for 40-70% of the weight of the cereal raw material, and carrying out alcohol fermentation for 15-730 days at 28-35 ℃ to obtain wine mash;

s06, adding grain processing peel substances accounting for 100-300% of the weight of the grain raw materials into the fermented glutinous rice obtained in the S05 to serve as loose materials, and uniformly mixing;

s07, adding 5-15% by weight of grain raw materials into the vinegar substrate which is fermented for 6-8 days, and carrying out acetic fermentation for 8-360 days to obtain vinegar substrate; the vinegar substrate fermented for 6-8 days refers to vinegar substrate fermented for 6-8 days in the previous acetic acid fermentation process, or vinegar substrate obtained by acetic acid fermentation for 6-8 days by adopting acetic acid strains; the original pulp vinegar prepared by acetic acid fermentation with acetic acid strain has light fragrance, and the active substances are reduced correspondingly. Therefore, in the embodiment of the invention, the vinegar substrate fermented for 6-8 days is preferably the vinegar substrate fermented for 6-8 days in the previous time, so that the acetic acid fermentation effect is better, and the material components are richer.

S08, smoking 25-75% of the vinegar residue obtained in the step S07 at 70-90 ℃ for 4-8 days to obtain a koji balsam vinegar smoking residue product;

s09, adding cold water and vinegar pouring light vinegar liquid into the residual vinegar grains in the step S08 to enable the total weight to be increased to 2-3 times of the original weight, soaking for more than 12 hours, and pouring out the vinegar liquid to obtain third vinegar liquid; heating the third vinegar solution to boiling state, adding into the product of fermented product of JIUQUXIANGZHI vinegar, soaking for more than 10 hr, and leaching out again to obtain fourth vinegar solution;

s10, freezing the fourth vinegar liquid obtained in the step S09 in a freezing environment to obtain a piece of koji balsam vinegar; then, placing the koji aromatic ester vinegar blocks in an environment with the temperature of 0-20 ℃ to naturally melt the koji aromatic ester vinegar blocks, and collecting flowing thick vinegar liquid; the freezing environment is preferably a freezer, freezer or refrigerator. The koji balsam vinegar block may be a vinegar block which is just solidified on the outer surface and is substantially solid, or a vinegar block which is completely solidified from the inside to the outside.

S11, putting the concentrated vinegar liquid collected in the step S10 into a brewing jar, and brewing in the open air for at least 12 months to obtain the aspongopus aromatic ester vinegar.

The above cereal raw materials include, but are not limited to, cereals, beans and potatoes, preferably cereals such as sorghum, rice, millet, wheat and the like.

Through detection, the acidity of the aspongopus aromaticus ester vinegar prepared by the method is not lower than 9.0g/100mL, the polysaccharide content is not less than 96.0mg/g, the polypeptide content is not less than 58.8mg/g, the total amount of free amino acids is not less than 4.21mg/g, the content of biological total flavonoids is not less than 5.60mg/g, and the polyphenol content is not less than 6.75 mg/g.

In accordance with a third aspect of the present invention, there is provided vinegar obtained by the above method for producing vinegar using lees.

Through detection, the total acid content of the vinegar prepared by the vinegar preparation method in any embodiment is not less than 10.0g/100mL, the non-volatile acid content is not less than 8.0g/100mL, the soluble salt-free solid content is not less than 30g/100mL, the total polysaccharide content is not less than 95.0mg/g, the total polypeptide content is not less than 80.0mg/g, the total amount of free amino acids is not less than 40.0mg/g, the biological total flavone content is not less than 7.0mg/g, the total polyphenol content is not less than 10.0mg/g, and the ligustrazine content is not less than 350 mg/L.

In addition, 16 free amino acids are detected in the vinegar, wherein the content of essential amino acids is not less than 17.0mg/g, and the detected essential amino acids comprise lysine, threonine, leucine, isoleucine, valine, methionine and phenylalanine; the content of semi-essential amino group (such as arginine and histidine) is not less than 6.0 mg/g; and detecting ferulic acid, chlorogenic acid, gamma-aminobutyric acid, choline, glycerophosphorylcholine, inositol, anthocyanin, catechin, epicatechin and other active substances.

The fourth aspect of the embodiments of the present invention provides a method for preparing a secondary fermented grain wine from distiller's grains, comprising the steps of:

wherein the leaching and desolventizing agent in the step S101 is alcohol;

s301, collecting the alcohol of the soaking solvent distilled and removed in the step S103 as recovered alcohol for soaking and eluting the vinasse;

s302, sequentially carrying out soaking elution, filtering separation and distillation for a plurality of times to obtain distilled and removed alcohol, namely the side wine.

And (3) soaking the recycled alcohol for 5-15 times, eluting the vinasse, separating, distilling, and then recycling to obtain the high-quality secondary vinasse wine.

The fifth aspect of the embodiment of the invention provides a secondary distilled grain prepared by the method for preparing the secondary distilled grain by using the distilled grains.

The present invention will be described in further detail below with reference to specific examples.

Example 1

A vinasse processing method comprises the following steps:

1) soaking the vinasse by using alcohol, stirring the vinasse at intervals of 1 day for 2 weeks, and then not stirring the vinasse to separate husk and peel substances from the vinasse, wherein the rest substances in the vinasse and the leaching solvent form an elution suspension;

2) filtering the chaff, the bark material and the elution suspension from the whole stillage;

3) distilling off the alcohol from the elution suspension to obtain a distillation residue. Wherein the weight percentage of the alcohol in the distillation residue is 5%.

Example 2

The distillation residue obtained in example 1 was subjected to detection analysis and storage time test. The distillation residue was placed in a sealed container and stored at room temperature. The respective indices before and after 2 years of storage were measured, and the results are shown in Table 1.

From the results, it can be seen that the distillation residue after 2 years of storage had no difference in appearance and was not deteriorated; the content of the nutrient substances contained in the distiller's grains is not obviously changed, so that the distiller's grains treated in the embodiment 1 can be stored for at least 2 years, and the later high-value utilization is not influenced.

TABLE 1

Example 3

A method for preparing vinegar by using vinasse comprises the following steps:

putting the distillation residue and the chaff obtained in the example 1 into a fermentation device, wherein the weight ratio of the distillation residue to the chaff is 1:0.4, adding 150% of the distillation residue by weight of the koji balsam vinegar fermented grains fermented for 6-8 days and 80% of the distillation residue by weight of grain processing peel substances, uniformly mixing, and fermenting for 12 days to obtain a fermentation product;

transferring the fermentation product into a glass jar, compacting and filling, screwing a cover with a sealing plug, sealing with gypsum and glue water to ensure strict sealing, and aging for 180 days at 2-25 ℃ to obtain an aged grain product;

heating 50% of the aged fermentation product in a fermentation vat with slow fire, and smoking at 85 deg.C for 5 days to obtain fermented product;

adding cold water and the light vinegar solution obtained by spraying vinegar last time into the rest of the aged substances to increase the total weight to 3 times of the original weight, soaking for more than 12h, and spraying out the vinegar solution to obtain a first vinegar solution; heating the first vinegar liquid to boiling state, injecting into the product of smoked grains, soaking for more than 10 hr, and leaching out again to obtain a second vinegar liquid;

freezing the second vinegar liquid in a cold storage to form vinegar blocks; then, placing the vinegar blocks in an environment with the temperature of 0-20 ℃ to naturally melt the vinegar blocks, and collecting flowing-down concentrated vinegar liquid;

when the color of the vinegar block becomes light, the color of the flowing vinegar liquid becomes light, and when the color of the vinegar block is close to white, the vinegar block is combined with the leached light vinegar liquid for the next use; putting the collected concentrated vinegar liquid into a brewing jar, and brewing in the open air for at least 12 months to obtain the edible vinegar.

Example 4

In this example, the vinegar obtained in example 3 was analyzed for its material composition, and the contents of each index are shown in Table 2.

TABLE 2

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims

1. A vinasse processing method is characterized by comprising the following steps:

2. The stillage processing method according to claim 1, wherein the step of soaking the eluted stillage with a leaching solvent to separate hulls and skin-like substances from the stillage, the remaining substances in the stillage forming an elution suspension with the leaching solvent comprises:

3. The method for processing the distiller's grains according to claim 1, wherein in the step of soaking and eluting the distiller's grains with the leaching solvent, the weight part ratio of the leaching solvent to the distiller's grains is 1-30: 1.

4. the method for treating distiller's grains according to any one of claims 1 to 3, wherein the leaching solvent is one of ethanol, acetic acid, methanol, acetone, acetonitrile, petroleum ether, benzene, toluene, chloroform, diethyl ether, ethyl acetate, dichloroethane, n-butanol, propanol, and isopropanol, or a mixture of at least two of them in any ratio.

5. The method for processing the distiller's grains according to claim 4, wherein the leaching solvent is ethanol, and in the step of leaching and eluting the distiller's grains by using the leaching solvent, the weight ratio of the leaching solvent to the distiller's grains is 1-8: 1.

6. the method for preparing vinegar by using vinasse is characterized by comprising the following steps of:

collecting the chaff and the distillation residue obtained from the stillage processing method of claim 5;

melting the vinegar blocks, and collecting melted concentrated vinegar liquid;

aging the concentrated vinegar liquid to obtain vinegar;

7. The method for producing vinegar using pot ale according to claim 6, wherein the carrier containing microorganisms is fermented famous vinegar, and the fermented famous vinegar is fermented murraya kouyama vinegar.

8. The method of manufacturing vinegar using pot ale according to claim 6, wherein the step of fermenting the chaff and the distillation residue using a carrier containing a microorganism to obtain a fermentation product comprises:

9. The method of manufacturing vinegar using pot ale according to claim 6, wherein the step of fermenting the chaff and the distillation residue using a carrier containing a microorganism to obtain a fermentation product comprises:

10. A vinegar produced by the method for producing a vinegar using the pot lees according to any one of claims 6 to 9.