CN111808713A - Method for recycling waste vinasse - Google Patents

Method for recycling waste vinasse Download PDF

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Publication number
CN111808713A
CN111808713A CN202010709475.3A CN202010709475A CN111808713A CN 111808713 A CN111808713 A CN 111808713A CN 202010709475 A CN202010709475 A CN 202010709475A CN 111808713 A CN111808713 A CN 111808713A
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vinasse
baking
grains
parts
distiller
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杨少勇
刘文汇
刘平
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Hebei Guxiangyang Wine Co ltd
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Hebei Guxiangyang Wine Co ltd
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12HPASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/02Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
    • C12H1/04Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material
    • C12H1/0416Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of organic added material
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12HPASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/003Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages by a biochemical process
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12HPASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/02Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
    • C12H1/04Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material
    • C12H1/0416Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of organic added material
    • C12H1/0424Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of organic added material with the aid of a polymer

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  • General Chemical & Material Sciences (AREA)
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  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)

Abstract

The invention belongs to the technical field of brewing, and particularly relates to a method for recycling waste vinasse, which comprises six steps of S1, separation, S2, primary feeding, S3, secondary feeding, S4, baking, S5, puffing and S6, purification. The invention has the following advantages: the finally formed puffed vinasse has an excellent high-strength reticular structure and is beneficial to adsorbing impurities in the purification process, the puffed vinasse needs to be put into turbid wine, under the impact of a large amount of ethanol, the combination of polydimethylsiloxane and gellan gum-protein reticular structure can be partially dissociated, so that flavor substances in the puffed vinasse are fully released, the quality of wine is improved, meanwhile, the bentonite, grain powder, tricalcium silicate and polydimethylsiloxane are added to form firm puffed vinasse, the storage of the vinasse is simple and easy, the puffed vinasse in the wine is not easy to disintegrate, and the separation effect of the puffed vinasse and the wine is beneficial to ensuring.

Description

Method for recycling waste vinasse
Technical Field
The invention belongs to the technical field of brewing, and particularly relates to a method for recycling waste vinasse.
Background
The solid-state white spirit, i.e. pure grain spirit, is made up by using grain as raw material, adopting solid (or semi-solid) saccharification, fermentation and distillation, ageing and blending, and has no addition of edible alcohol and flavouring material produced by non-white spirit fermentation.
Nowadays, the utilization mode of the distiller's grains is generally used as feed for the aquaculture industry, particularly for fish and cattle, and has remarkable effect on the fattening of animals, for example, a patent document with the patent publication number of "CN 103005147B" and the name of "distiller's grain-based biological feed" provides the method, but the utilization mode of the distiller's grains only utilizes the nutrient substances of the distiller's grains, and the valuable flavor substances contained in the distiller's grains are not utilized sufficiently.
Disclosure of Invention
The invention aims to provide a method for recycling waste vinasse, which can be used for preparing durable puffed vinasse, can be used for removing turbidity of low-quality turbid white spirit, and can release flavor substances to improve the quality of low-degree turbid white spirit.
The technical purpose of the invention is realized by the following technical scheme: a method for recycling waste vinasse comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing wet distiller's grains until ice crystals appear in the center, grinding in a food-grade grinder, repeatedly freezing and grinding for 3-5 times, and adding grain powder, food-grade polydimethylsiloxane and food-grade bentonite during grinding to obtain mixed distiller's grains;
s3, secondary feeding: placing the mixed vinasse obtained in the step S2 in a container to be frozen into blocks, then breaking the blocks into small blocks, and placing the frozen small blocks of vinasse in a gellan gum solution to be frozen to obtain composite vinasse;
s4, baking: placing the composite distiller 'S grains obtained in the step S3 into a baking oven, baking while stirring at 80-90 deg.C until the water content is below 45%, and finally obtaining pasty distiller' S grains;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for at least 1 hour, and filtering to obtain pure white wine.
By adopting the technical scheme, the vinasse is frozen and ground, and the agglomerated protein precipitate in the vinasse is separated by utilizing the sharp edge of fine ice crystals, so that the problem that the vinasse can be ground only by drying in the traditional vinasse recycling process is solved, and more flavor substances are reserved; and finally, the puffed vinasse is prepared, can be used for purifying low-quality turbid liquor, can release flavor substances contained in the puffed vinasse while adsorbing flocculent impurities in the liquor, and improves the quality of the low-quality liquor.
The invention is further provided with: the addition amounts of the components in the steps S1-S6 are respectively as follows by mass parts:
wet vinasse: 15-20 parts of a solvent;
grain powder: 8-10 parts;
food-grade bentonite: 3-5 parts;
food grade polydimethylsiloxane: 1-1.5 parts;
gellan gum: 2-4 parts;
wherein, the wet vinasse, the polydimethylsiloxane and the gellan gum are all dry weight basis.
By adopting the technical scheme, the bentonite has the functions of providing a base point for attaching a substance and containing a part of flavor substances, the gellan gum has the functions of coagulating the substance into a mass on one hand and partially degrading the substance during baking to expose the reducing sugar residue and crosslinking the reducing sugar residue with macromolecular protein in vinasse to form a reticular structure, the polydimethylsiloxane is a substance which does not dehydrate and is difficult to degrade under the whole process environment and aims to provide a long-acting framework and is connected with the gellan gum-protein reticular structure through a secondary bond to form a polydimethylsiloxane-gellan gum-protein composite structure, the polydimethylsiloxane does not dehydrate and does not react in the baking and puffing processes and provides a certain supporting force for the dehydration and shrinkage of the gellan gum-protein reticular structure, similar to steel bars in reinforced concrete, the composite structure is beneficial to keeping microscopic shape of vinasse, not only can retain more flavor substances by the gellan gum-protein network structure, but also can improve the adsorption capacity of the gellan gum-protein network structure, and the composite structure of the polydimethylsiloxane-gellan gum-protein is partially decomposed by being impacted by a large amount of alcohol in the subsequent purification process, so that the flavor substances can be released from the vinasse.
The invention is further provided with: the cereal powder is prepared by baking husk and straw of cereal to water content of 10-15%, and grinding with 10 mesh sieve.
By adopting the technical scheme, the grain powder mainly contains substances such as hard organic silicon, hemicellulose, long-chain cellulose and the like, has the main functions of serving as an abrasive on one hand and supplementing certain hemicellulose and cellulose on the other hand, the hemicellulose and the cellulose have certain reducing ends and can be combined into a gellan gum-protein reticular structure, untreated cellulose has large internal acting force and is easy to agglomerate, a plurality of hard particles embedded into the gellan gum-protein reticular structure can be formed, the stability of the gellan gum-protein reticular structure is improved, in a general embodiment, the grain powder needs to be baked to be free of any plant odor so as not to influence the quality of the final puffed vinasse, but in some special embodiments, if some crops with fragrance are used for preparing the grain powder, a certain odor can be retained as required, so that the aroma finally enters the wine body through the puffed vinasse.
The invention is further provided with: the calcium stearoyl lactylate is added into the cereal powder in the grinding process, and the adding amount of the calcium stearoyl lactylate is 0.1 part by mass of the calcium stearoyl lactylate added into each part by mass of the cereal powder.
By adopting the technical scheme: the stearoyl calcium lactate connects crude protein, crude starch and protein in the vinasse in the grain powder to increase the connecting sites of the grain powder and the vinasse, and can connect gellan gum and the protein in the vinasse to enhance the strength of the gellan gum-protein network structure, so that the durability of the gellan gum-protein network structure is improved when the gellan gum-protein network structure is soaked in wine, and the puffed wine vinasse cannot collapse too early.
The invention is further provided with: in step S3, pullulan is also dissolved in the gellan gum solution, and the pullulan is added in an amount of 0.1 part by mass per part of gellan gum.
By adopting the technical scheme, the pullulan and the gellan gum are compounded to be used, so that the gellan gum is smoother and more soaked in vinasse, and on the other hand, the pullulan has excellent film forming property and can help the gellan gum-protein net structure to keep flavor substances.
The invention is further provided with: in the step S4, in the baking process, 0.01 part by mass of tricalcium silicate is added into each part by mass of wet distiller 'S grains according to dry weight, the tricalcium silicate is added in a mode that the tricalcium silicate is evenly divided into at least 3 parts, each part is evenly scattered on the surface of the distiller' S grains, and the time interval between every two parts is at least 15 minutes.
By adopting the technical scheme, the tricalcium silicate can be rapidly hydrated to release silicon-calcium-water hard particles and calcium hydroxide particles, and the vinasse contains a large amount of hydroxyl groups, so that the silicon-calcium-water hard particles are not hydrated into a cluster form like tricalcium silicate in cement, but are combined with gellan gum, protein and other long-chain polysaccharides to form a hard central point, the structural strength of the vinasse can be greatly improved, and on the other hand, a small amount of released calcium hydroxide particles can form a local high-pH environment to promote the breakage of the long-chain polysaccharides to expose more reducing ends so as to be combined with the protein, so that the combination between the protein and the polysaccharides is more stable.
The invention is further provided with: and S4, in the baking process, the temperature is increased to 55 ℃ at the heating rate of 2 ℃/min, the temperature is kept for at least 10min, and then the baking is carried out in a baking oven, wherein the baking time is not less than 45 min.
By adopting the technical scheme, the vinasse is prevented from being gelatinized by excessively fast temperature rise, and unpleasant smell is generated.
The invention has the beneficial effects that: .
1. Through the compound cross-linking between the gellan gum and the protein, a gellan gum-protein reticular structure is formed, then stable polydimethylsiloxane is used as a framework to support the gellan gum-protein reticular structure to avoid excessive dehydration and shrinkage in the baking and puffing processes, the finally formed puffed vinasse is ensured to have a structure with excellent high-strength reticular morphology, impurities are favorably adsorbed in the purifying process, the polydimethylsiloxane and the gellan gum-protein reticular structure are connected through a secondary bond, the bonding strength is high, the puffed vinasse needs to be put into turbid wine in the purifying process, the bonding between the polydimethylsiloxane and the gellan gum-protein reticular structure is partially dissociated under the impact of a large amount of ethanol, so that flavor substances in the puffed vinasse are fully released, and the gellan gum-protein reticular structure is fully expanded, so that the dissociation does not affect the adsorption of the puffed vinasse.
2. According to the scheme, the cereal husk is added in the one-step charging process, the tricalcium silicate is added in the baking process, the hard structure centers are respectively formed at different periods, and the cross-linked reticular structure between the protein and the polysaccharide is strengthened, so that the finally formed puffed vinasse has an excellent and firm appearance structure, the storage of the puffed vinasse is convenient, the puffed vinasse is not easy to disintegrate in use, the puffed vinasse is not easy to fall off, and the dirty wine to be purified is not polluted; meanwhile, a local high pH environment is formed near the hard particles of a hydration product silicon-calcium-water of tricalcium silicate due to the addition of tricalcium silicate, and the high molecular polysaccharide is promoted to break to expose the reducing end at the baking temperature, so that more cross links are generated near the hard particles of silicon-calcium-water, and the overall strength of the puffed vinasse and the capability of wrapping flavor molecules are improved.
3. The scheme is different from the traditional utilization mode of filtering, drying and mixing materials, adopts the freezing-grinding process, utilizes the sharp edge grinding of ice crystals to decompose protein groups in the vinasse and expose more flavor substances, so that the finally supported puffed vinasse flavor substances are released more quickly, simultaneously, the problem of excessive loss of the flavor substances caused by baking before a reticular structure is formed is avoided, and the problem of continuous vinasse fermentation of yeast residual in the vinasse is also avoided.
4. According to the scheme, the vinasse is finally treated through the puffing process, so that the vinasse is subjected to primary high-temperature sterilization, and meanwhile, the bentonite, the grain powder, the tricalcium silicate and the polydimethylsiloxane are added to form firm puffed vinasse, so that the storage of the vinasse is simple and easy to implement, the puffed vinasse in the wine body is not easy to disintegrate, and the separation effect of the puffed vinasse and the wine body is favorably ensured.
Detailed Description
The technical solutions in the examples will be clearly and completely described below.
The parts in all the following examples and comparative examples are calculated as the same parts by mass.
Example 1
A method for recycling waste vinasse comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing 18 parts of wet distiller grains until ice crystals appear in the center part, grinding the wet distiller grains in a food-grade grinding machine, repeatedly freezing and grinding the wet distiller grains for 4 times, adding 9 parts of grain powder, 1.3 parts of food-grade polydimethylsiloxane and 3.8 parts of food-grade bentonite in the grinding process to obtain mixed distiller grains, wherein the grain powder is obtained by baking the shells and the straws of grains until the water content is 14 percent and grinding the grains with a 10-mesh screen, and 0.9 part of calcium stearoyl lactate is also added in the grinding process of the grain powder;
s3, secondary feeding: placing the mixed vinasse obtained in the step S2 in a container to be frozen into blocks, then breaking the blocks into small blocks, and placing the frozen small blocks of vinasse into a solution prepared from 3.4 parts of gellan gum and 0.34 part of pullulan to be frozen, so as to obtain compound vinasse;
s4, baking: heating the composite vinasse obtained in the step S3 to 55 ℃ at a heating rate of 2 ℃/min, then keeping the temperature for 15min, then placing the composite vinasse into a baking oven for baking, placing the composite vinasse into the baking oven, then baking the composite vinasse while stirring at a temperature of 83 ℃, adding 0.18 part of tricalcium silicate in the baking process, uniformly distributing 3 parts of tricalcium silicate, uniformly scattering one part of tricalcium silicate on the surface of the vinasse every 20 minutes, baking for 60min, finally baking until the water content of the vinasse is 41%, and finally obtaining pasty vinasse;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for at least 1 hour, and filtering to obtain pure white wine.
Example 2
A method for recycling waste vinasse comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing 15 parts of wet distiller grains until ice crystals appear in the center part, grinding the wet distiller grains in a food-grade grinding machine, repeatedly freezing and grinding the wet distiller grains for 5 times, adding 8 parts of grain powder, 1.5 parts of food-grade polydimethylsiloxane and 3 parts of food-grade bentonite in the grinding process to obtain mixed distiller grains, wherein the grain powder is obtained by baking the shells and the straws of grains until the water content is 10 percent and grinding the grains with a 10-mesh screen, and 0.8 part of calcium stearoyl lactate is also added into the grain powder in the grinding process;
s3, secondary feeding: placing the mixed vinasse obtained in the step S2 in a container to be frozen into blocks, then breaking the blocks into small blocks, and placing the frozen small blocks of vinasse into a solution prepared from 4 parts of gellan gum and 0.4 part of pullulan to be frozen, so as to obtain composite vinasse;
s4, baking: heating the composite vinasse obtained in the step S3 to 55 ℃ at a heating rate of 2 ℃/min, then preserving heat for 10min, then placing the composite vinasse into a baking oven for baking, placing the composite vinasse into the baking oven, then baking the composite vinasse while stirring at a temperature of 90 ℃, adding 0.15 part of tricalcium silicate in the baking process, uniformly distributing one part of tricalcium silicate on the surface of the vinasse every 15 minutes, baking for 60min, and finally baking until the water content of the vinasse is 37%, thereby finally obtaining pasty vinasse;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for 1 hour, and filtering to obtain pure white wine.
Example 3
A method for recycling waste vinasse comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing 20 parts of wet distiller's grains until ice crystals appear in the center part, grinding the wet distiller's grains in a food-grade grinding machine, repeatedly freezing and grinding the wet distiller's grains for 3 times, adding 10 parts of grain powder, 1 part of food-grade polydimethylsiloxane and 5 parts of food-grade bentonite in the grinding process to obtain mixed distiller's grains, wherein the grain powder is obtained by baking the shells and straws of grains until the water content is 15 percent and grinding the grains with a 10-mesh screen, and 1 part of calcium stearoyl lactylate is also added into the grain powder in the grinding process;
s3, secondary feeding: placing the mixed vinasse obtained in the step S2 in a container to be frozen into blocks, then breaking the blocks into small blocks, and placing the frozen small blocks of vinasse into a solution prepared from 2 parts of gellan gum and 0.2 part of pullulan to be frozen, so as to obtain composite vinasse;
s4, baking: heating the composite vinasse obtained in the step S3 to 55 ℃ at a heating rate of 2 ℃/min, then preserving heat for 20min, then placing the composite vinasse into a baking oven for baking, placing the composite vinasse into the baking oven, then baking the composite vinasse while stirring at a temperature of 80 ℃, adding 0.2 part of tricalcium silicate in the baking process, uniformly distributing 3 parts of tricalcium silicate, uniformly spreading one part of tricalcium silicate on the surface of the vinasse every 15 minutes, baking for 45min, and finally baking until the water content of the vinasse is 45%, thereby finally obtaining pasty vinasse;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for 2 hours, and filtering to obtain pure white wine.
Example 4
A method for recycling waste vinasse comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing 18 parts of wet distiller's grains until ice crystals appear in the central part, grinding the wet distiller's grains in a food-grade grinding machine, repeatedly freezing and grinding the wet distiller's grains for 4 times, adding 9 parts of grain powder, 1.3 parts of food-grade polydimethylsiloxane and 3.8 parts of food-grade bentonite in the grinding process to obtain mixed distiller's grains, wherein the grain powder is the powder of shells and straws of grains which are roasted until the water content is 14 percent and ground by a 10-mesh screen;
s3, secondary feeding: placing the mixed vinasse obtained in the step S2 in a container to be frozen into blocks, then breaking the blocks into small blocks, and placing the frozen small blocks of vinasse into a solution prepared from 3.4 parts of gellan gum and 0.34 part of pullulan to be frozen, so as to obtain compound vinasse;
s4, baking: heating the composite vinasse obtained in the step S3 to 55 ℃ at a heating rate of 2 ℃/min, then keeping the temperature for 15min, then placing the composite vinasse into a baking oven for baking, placing the composite vinasse into the baking oven, then baking the composite vinasse while stirring at a temperature of 83 ℃, adding 0.18 part of tricalcium silicate in the baking process, uniformly distributing 3 parts of tricalcium silicate, uniformly scattering one part of tricalcium silicate on the surface of the vinasse every 20 minutes, baking for 60min, finally baking until the water content of the vinasse is 42%, and finally obtaining pasty vinasse;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for 1.5 hours, and filtering to obtain pure white wine.
Example 5
A method for recycling waste vinasse comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing 18 parts of wet distiller grains until ice crystals appear in the center part, grinding the wet distiller grains in a food-grade grinding machine, repeatedly freezing and grinding the wet distiller grains for 4 times, adding 9 parts of grain powder, 1.3 parts of food-grade polydimethylsiloxane and 3.8 parts of food-grade bentonite in the grinding process to obtain mixed distiller grains, wherein the grain powder is obtained by baking the shells and the straws of grains until the water content is 14 percent and grinding the grains with a 10-mesh screen, and 0.9 part of calcium stearoyl lactate is also added in the grinding process of the grain powder;
s3, secondary feeding: placing the mixed vinasse obtained in the step S2 in a container to be frozen into blocks, then breaking the blocks into small blocks, and placing the frozen small blocks of vinasse into a solution prepared from 3.4 parts of gellan gum to be thawed to obtain composite vinasse;
s4, baking: heating the composite vinasse obtained in the step S3 to 55 ℃ at a heating rate of 2 ℃/min, then keeping the temperature for 15min, then placing the composite vinasse into a baking oven for baking, placing the composite vinasse into the baking oven, then baking the composite vinasse while stirring at a temperature of 83 ℃, adding 0.18 part of tricalcium silicate in the baking process, uniformly distributing 3 parts of tricalcium silicate, uniformly scattering one part of tricalcium silicate on the surface of the vinasse every 20 minutes, baking for 60min, finally baking until the water content of the vinasse is 40%, and finally obtaining pasty vinasse;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for 1.5 hours, and filtering to obtain pure white wine.
Example 6
A method for recycling waste vinasse comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing 18 parts of wet distiller grains until ice crystals appear in the center part, grinding the wet distiller grains in a food-grade grinding machine, repeatedly freezing and grinding the wet distiller grains for 4 times, adding 9 parts of grain powder, 1.3 parts of food-grade polydimethylsiloxane and 3.8 parts of food-grade bentonite in the grinding process to obtain mixed distiller grains, wherein the grain powder is obtained by baking the shells and the straws of grains until the water content is 14 percent and grinding the grains with a 10-mesh screen, and 0.9 part of calcium stearoyl lactate is also added in the grinding process of the grain powder;
s3, secondary feeding: placing the mixed vinasse obtained in the step S2 in a container to be frozen into blocks, then breaking the blocks into small blocks, and placing the frozen small blocks of vinasse into a solution prepared from 3.4 parts of gellan gum and 0.34 part of pullulan to be frozen, so as to obtain compound vinasse;
s4, baking: heating the composite vinasse obtained in the step S3 to 55 ℃ at a heating rate of 2 ℃/min, then preserving heat for 15min, then placing the composite vinasse into a baking oven for baking, placing the composite vinasse into the baking oven, and then baking the composite vinasse while stirring at a temperature of 83 ℃ for 60min until the water content of the vinasse is 41%, thus finally obtaining pasty vinasse;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for 1.5 hours, and filtering to obtain pure white wine.
Comparative example 1
A method for recycling waste vinasse comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing 18 parts of wet distiller grains until ice crystals appear in the center part, grinding the wet distiller grains in a food-grade grinding machine, repeatedly freezing and grinding the wet distiller grains for 4 times, adding 9 parts of grain powder and 3.8 parts of food-grade bentonite in the grinding process to obtain mixed distiller grains, wherein the grain powder is obtained by baking the shells and straws of grains until the water content is 14 percent and grinding the grains with a 10-mesh screen, and 0.9 part of calcium stearoyl lactylate is also added in the grinding process;
s3, secondary feeding: placing the mixed vinasse obtained in the step S2 in a container to be frozen into blocks, then breaking the blocks into small blocks, and placing the frozen small blocks of vinasse into a solution prepared from 3.4 parts of gellan gum and 0.34 part of pullulan to be frozen, so as to obtain compound vinasse;
s4, baking: heating the composite vinasse obtained in the step S3 to 55 ℃ at a heating rate of 2 ℃/min, then keeping the temperature for 15min, then placing the composite vinasse into a baking oven for baking, placing the composite vinasse into the baking oven, then baking the composite vinasse while stirring at a temperature of 83 ℃, adding 0.18 part of tricalcium silicate in the baking process, uniformly distributing 3 parts of tricalcium silicate, uniformly scattering one part of tricalcium silicate on the surface of the vinasse every 20 minutes, baking for 60min, finally baking until the water content of the vinasse is 41%, and finally obtaining pasty vinasse;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for at least 1 hour, and filtering to obtain pure white wine.
Comparative example 2
A method for recycling waste vinasse comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing 18 parts of wet distiller grains until ice crystals appear in the center part, grinding the wet distiller grains in a food-grade grinding machine, repeatedly freezing and grinding the wet distiller grains for 4 times, adding 9 parts of grain powder, 1.3 parts of food-grade polydimethylsiloxane and 3.8 parts of food-grade bentonite in the grinding process to obtain mixed distiller grains, wherein the grain powder is obtained by baking the shells and the straws of grains until the water content is 14 percent and grinding the grains with a 10-mesh screen, and 0.9 part of calcium stearoyl lactate is also added in the grinding process of the grain powder;
s3, secondary feeding: placing the mixed distiller 'S grains obtained in the step S2 in a container to be frozen into blocks, then crushing the blocks into small blocks, and freezing the frozen small blocks of distiller' S grains with the same amount of water as that of the distiller 'S grains obtained in the step S3 in the embodiment 1 to obtain composite distiller' S grains;
s4, baking: heating the composite vinasse obtained in the step S3 to 55 ℃ at a heating rate of 2 ℃/min, then keeping the temperature for 15min, then placing the composite vinasse into a baking oven for baking, placing the composite vinasse into the baking oven, then baking the composite vinasse while stirring at a temperature of 83 ℃, adding 0.18 part of tricalcium silicate in the baking process, uniformly distributing 3 parts of tricalcium silicate, uniformly scattering one part of tricalcium silicate on the surface of the vinasse every 20 minutes, baking for 60min, finally baking until the water content of the vinasse is 41%, and finally obtaining pasty vinasse;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for at least 1 hour, and filtering to obtain pure white wine.
Comparative example 3
A method for recycling waste vinasse comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing 18 parts of wet distiller grains until ice crystals appear in the center part, grinding the wet distiller grains in a food-grade grinding machine, repeatedly freezing and grinding the wet distiller grains for 4 times, adding 9 parts of grain powder, 1.3 parts of food-grade polydimethylsiloxane and 3.8 parts of food-grade bentonite in the grinding process to obtain mixed distiller grains, wherein the grain powder is obtained by baking the shells and the straws of grains until the water content is 14 percent and grinding the grains with a 10-mesh screen, and 0.9 part of calcium stearoyl lactate is also added in the grinding process of the grain powder;
s3, secondary feeding: placing the mixed distiller 'S grains obtained in the step S2 in a container to be frozen into blocks, then crushing the blocks into small blocks, and freezing the frozen small blocks of distiller' S grains with the same amount of water as that of the distiller 'S grains obtained in the step S3 in the embodiment 1 to obtain composite distiller' S grains;
s4, baking: heating the composite vinasse obtained in the step S3 to 55 ℃ at a heating rate of 2 ℃/min, then keeping the temperature for 15min, then placing the composite vinasse into a baking oven for baking, placing the composite vinasse into the baking oven, then baking the composite vinasse while stirring at a temperature of 83 ℃, adding 0.18 part of tricalcium silicate in the baking process, uniformly distributing 3 parts of tricalcium silicate, uniformly scattering one part of tricalcium silicate on the surface of the vinasse every 20 minutes, baking for 60min, finally baking until the water content of the vinasse is 41%, and finally obtaining pasty vinasse;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for at least 1 hour, and filtering to obtain pure white wine.
Comparative example 4 (starch adsorption method)
Adding starch according to the proportion that 0.001 part by mass of starch is added into each part by mass of the turbid liquor, standing until the turbid liquor is clear, and filtering to obtain pure white liquor.
Comparative example 5 (freezing impurity removal method)
Reducing the temperature of the turbid liquor to-13 ℃, adding a small amount of flocculant, refrigerating until the turbid liquor is clear, and filtering to obtain pure white liquor.
Comparative example 6
No treatment is carried out on the turbid wine.
For each example and comparative example, the purified muddy liquor adopts the low-alcohol muddy white liquor produced by the same batch brewed by the applicant in the current year, and the adopted vinasse is the vinasse remained in the same batch for producing high-quality white liquor. Total acids, total esters, solid matters and ethyl caproate after treatment of each example and comparative example are respectively recorded according to GB/T10781.1-2006 Luzhou-flavor liquor and GB/T10345-2007 liquor analysis methods, liquor body clarification is observed every 1 hour until no suspended matter is visible to naked eyes, time of last observation is recorded, total purification time is calculated, and recorded results are shown in Table 1. Meanwhile, 10 appraisers are invited to comment on the color, aroma and taste of the white spirit, wherein the aroma and taste are graded by taking the top-grade white spirit manufactured by the applicant in the same year as 10 grades, a highest grade and a lowest grade are removed from the grades, the average of other values is taken as a final grade, and the recorded results are shown in table 2.
TABLE 1 results of physical and chemical tests
Figure BDA0002588637520000101
TABLE 2 sensory test results
Fragrance Taste of the product Evaluation of color and luster
Example 1 8.4 7.7 Colorless, clear and transparent, and has no suspended matter and precipitate
Example 2 8.0 7.5 Colorless, clear and transparent, and has no suspended matter and precipitate
Example 3 7.4 8.0 Colorless, clear and transparent, and has no suspended matter and precipitate
Example 4 7.3 7.4 Colorless, clear and transparent, and has no suspended matter and precipitate
Example 5 6.8 6.9 Colorless, clear and transparent, and has no suspended matter and precipitate
Example 6 6.8 6.3 Colorless, clear and transparent, and has no suspended matter and precipitate
Comparative example 1 7.1 7.3 YellowishWith suspended turbid matter
Comparative example 2 7.1 7.4 Yellowish, suspended turbidity
Comparative example 3 7.0 7.0 Yellowish, suspended turbidity
Comparative example 4 6.2 6.1 Yellowish, clear and transparent, and has no suspended matter and precipitate
Comparative example 5 7.2 7.0 Colorless, clear and transparent, and has no suspended matter and precipitate
Comparative example 6 7.1 7.2 Yellow with suspended turbidity
Comparative example 6 is a raw wine without any treatment and is used as a blank for other treatment methods, and in comparative example 4 using a commercially available starch adsorption method, comparative example 5 using a freezing impurity removal method and examples 4 to 6, total acids and total esters representing flavor are lost to some extent, wherein the loss by the cooling impurity removal method is small, and the loss by the examples 4 to 6 is not much different from the loss by the cooling impurity removal method and is far superior to the loss by the starch adsorption method, while in the preferred examples 1 to 3, the contents of total acids, total esters and ethyl caproate are rather increased to some extent, and sensory scores of aroma and taste are also increased, which indicates that in the preferred examples, flavor substances contained in distiller's grains are sufficiently released.
In the actual process of adsorbing and removing turbidity, the better examples 1-3 keep good appearance in the wine body, and can not collapse and deform in the subsequent filtering and separating process, while the examples 4 without adding stearoyl calcium lactate and 6 without adding tricalcium silicate can still keep a certain shape in the wine body, but the whole puffed vinasse is already collapsed softly, which causes a certain obstacle to the separating process, while the comparative example 3 without adding cereal husk has basically disintegrated puffed vinasse, and although a certain adsorbing and flocculating effect still exists, the disintegrated puffed vinasse can return to the wine body instead, and can pollute the wine body again, so that the wine body carries suspended turbidity again.
In the comparative examples 1 and 2, an effective reticular microstructure cannot be formed, so that adsorption and flocculation effects cannot be generated, and the turbid wine cannot be purified basically.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.

Claims (7)

1. A method for recycling waste vinasse is characterized by comprising the following steps: the method comprises the following steps:
s1, separation: filtering the liquor to obtain wet distiller's grains and crude liquor;
s2, primary feeding: freezing wet distiller's grains until ice crystals appear in the center, grinding in a food-grade grinder, repeatedly freezing and grinding for 3-5 times, and adding grain powder, food-grade polydimethylsiloxane and food-grade bentonite during grinding to obtain mixed distiller's grains;
s3, secondary feeding: placing the mixed vinasse obtained in the step S2 in a container to be frozen into blocks, then breaking the blocks into small blocks, and placing the frozen small blocks of vinasse in a gellan gum solution to be frozen to obtain composite vinasse;
s4, baking: placing the composite distiller ' S grains obtained in the step S3 into a baking oven, baking while stirring at 80-90 deg.C until the water content of distiller ' S grains is below 45%, and finally obtaining pasty distiller ' S grains;
s5, puffing: putting the pasty vinasse obtained in the step S4 into an extruder, and extruding the vinasse into expanded vinasse;
s6, purification: and putting the puffed vinasse into turbid crude wine, slowly stirring until the turbid wine becomes transparent, standing for at least 1 hour, and filtering to obtain pure white wine.
2. The method of claim 1, wherein the method comprises: the addition amounts of the components in the steps S1-S6 are respectively as follows by mass parts:
wet vinasse: 15-20 parts of a solvent;
grain powder: 8-10 parts;
food-grade bentonite: 3-5 parts;
food grade polydimethylsiloxane: 1-1.5 parts;
gellan gum: 2-4 parts;
wherein, the wet vinasse, the polydimethylsiloxane and the gellan gum are all dry weight basis.
3. The method of claim 1, wherein the method comprises: the cereal powder is prepared by baking husk and straw of cereal to water content of 10-15%, and grinding with 10 mesh sieve.
4. The method of claim 2, wherein the method comprises: the calcium stearoyl lactylate is added into the cereal powder in the grinding process, and the adding amount of the calcium stearoyl lactylate is 0.1 part by mass of the calcium stearoyl lactylate added into each part by mass of the cereal powder.
5. The method of claim 1, wherein the method comprises: in step S3, pullulan is also dissolved in the gellan gum solution, and the pullulan is added in an amount of 0.1 part by mass per part of gellan gum.
6. The method of claim 1, wherein the method comprises: in the step S4, in the baking process, 0.01 part by mass of tricalcium silicate is added into each part by mass of wet distiller 'S grains according to dry weight, the tricalcium silicate is added in a mode that the tricalcium silicate is evenly divided into at least 3 parts, each part is evenly scattered on the surface of the distiller' S grains, and the time interval between every two parts is at least 15 minutes.
7. The method of claim 1, wherein the method comprises: and S4, in the baking process, the temperature is increased to 55 ℃ at the heating rate of 2 ℃/min, the temperature is kept for at least 10min, and then the baking is carried out in a baking oven, wherein the baking time is not less than 45 min.
CN202010709475.3A 2020-07-17 2020-07-17 Method for recycling waste vinasse Withdrawn CN111808713A (en)

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Application publication date: 20201023