A method for preparing rice-flavor liquor and rice vinegar by using yellow rice wine

Abstract

The application discloses a method for preparing rice-flavor liquor and rice vinegar by using yellow rice wine, which comprises the following steps: conveying the yellow rice wine in a raw material tank to a preferential organic matter membrane separation unit; controlling the vacuum degree of the permeation side of the preferential organic matter membrane separation unit to be 1500-9500 Pa, so that the organic matters in the yellow rice wine selectively permeate the membrane and are vaporized into organic matter steam, and the retentate returns to the raw material tank and participates in the cyclic separation; obtaining the rice-flavor liquor by condensing the organic matter steam; and preparing the retentate in the raw material tank into rice vinegar after the separation process is stopped. The rice-flavor liquor obtained by the method retains various beneficial substances and effects of the yellow rice wine, and the content of harmful components including higher alcohols in the liquor is reduced; the remaining low-alcohol-content yellow rice wine can also be used to prepare rice vinegar. The method has the characteristics of high efficiency, reliable process and suitability for industrial production.

Description

Technical Field

[0001] This invention belongs to the field of pervaporation membrane separation technology, specifically relating to a method for preparing rice-fragrant white wine and rice vinegar using yellow rice wine. Background Technology

[0002] Yellow wine originated in China and is one of the world's oldest traditional brewed alcoholic beverages, ranking alongside beer and wine as one of the world's three major fermented alcoholic beverages. Yellow wine is made from rice (including glutinous rice, indica rice, japonica rice, and black rice), millet, corn, sorghum, wheat, buckwheat, and other grains through specific processing techniques (steaming, adding yeast, saccharification, fermentation, pressing, filtering, heating, storage, and blending). It is brewed through the combined action of various molds, yeasts, and bacteria. Baijiu (white liquor) was developed based on yellow wine, incorporating stills. The production and consumption of yellow wine in the Jiangsu, Zhejiang, and Shanghai regions account for over 70% of the national total, making it one of my country's major yellow wine production and consumption areas.

[0003] Currently, the quality of rice wine on the market varies greatly, with the following shortcomings: unstable color, strong bitterness, and excessively high levels of higher alcohols. Data shows that among all brewed alcoholic beverages, rice wine has the highest content of higher alcohols, far exceeding that of beer and wine. Excessive higher alcohol content can easily lead to intoxication, affecting consumer acceptance and recognition. Furthermore, due to its high sugar content, rice wine generally has a shelf life of only three to five years, making long-term storage difficult. These factors combined have resulted in consistently low sales of rice wine. Therefore, innovative processing methods for rice wine, aiming to reduce harmful components, increase alcohol content, and decrease sugar content to extend shelf life, while maximizing the extraction of beneficial substances, are crucial for improving its quality and enhancing drinking comfort. Traditional distillation techniques can be used to prepare high-proof rice wine, distilling out beneficial components and alcohol. In this process, organic substances such as alcohols and esters with low boiling points are more likely to volatilize, while beneficial components such as acids and aldehydes with high boiling points are released in smaller quantities, resulting in a stronger wine produced by traditional distillation.

[0004] Pervaporation is an energy-saving and environmentally friendly separation technology. Pervaporation membranes can be functionally categorized into water-preferential permeable membranes and organic-preferential permeable membranes. Organic-preferential permeable membranes are mainly used for the separation of organic-water systems or organic-organic systems. Compared to other separation methods such as distillation, extraction, and adsorption, they offer advantages such as low energy consumption, simple equipment, high recovery rate, easy operation, and high safety. For rice wine, the pervaporation membrane method utilizes the membrane's preferential permeability to concentrate organic components. Ethanol, among alcohols, permeates through the membrane more easily through dissolution and diffusion than higher alcohols such as isobutanol and isoamyl alcohol. Thus, most of the ethanol and a small amount of higher alcohols enter the permeate. A suitable amount of higher alcohols gives the wine its mellow flavor, while excessive amounts result in a bitter taste and are toxic to the human body. Wine produced using the pervaporation membrane method has richer nutritional components, a smoother taste, and better balance. Summary of the Invention

[0005] The purpose of this invention is to provide a method for preparing rice-aroma baijiu and rice vinegar using huangjiu (yellow rice wine). This method solves the problem of high higher alcohol content in huangjiu by using a preferential organic permeation vaporization membrane technology, reducing harmful components in the wine and maximizing the extraction of various beneficial substances from huangjiu. By increasing the alcohol content and reducing the sugar content, its shelf life is extended. The rice-aroma baijiu obtained using this method retains various beneficial substances and effects of huangjiu while reducing the content of harmful components, including higher alcohols. The remaining low-alcohol huangjiu can be used to produce rice vinegar. This method is characterized by high efficiency, reliable process, and applicability to industrial production.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows: A method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine includes the following steps: (1) The rice wine in the raw material tank is transported to the organic matter membrane separation unit; (2) The vacuum degree on the permeate side of the preferential organic matter membrane separator is controlled to be 1500-9500 Pa. Organic matter in rice wine selectively permeates through the membrane and vaporizes into organic matter vapor. The residual liquid is returned to the raw material tank and participates in the circulation separation. (3) The organic vapor obtained in step (2) is condensed to obtain rice-fragrant baijiu; (4) After the separation process is stopped, the residual liquid in the raw material tank is prepared into rice vinegar.

[0007] Preferably, in step (1), the volume fraction of alcohol in the rice wine is 12% to 18%.

[0008] Preferably, in step (3), the volume fraction of alcohol in the rice-aroma baijiu is 28%~40%.

[0009] Preferably, the separation process described in step (4) is stopped when the volume fraction of alcohol in the raw material tank is 4% to 8%.

[0010] Preferably, the method for preparing rice vinegar from the leachate in step (4) is as follows: add acetic acid bacteria solution to the leachate, and then ferment, press, filter, and blend to obtain rice vinegar.

[0011] Preferably, the preferential organic permeate membrane separator unit is composed of at least one preferential organic permeate membrane separator connected in series, in parallel, or in a mixed series-parallel configuration.

[0012] Preferably, the preferred organic membrane separator is of tubular or spiral type.

[0013] Furthermore, the organic-permeable membrane in the organic-permeable membrane separation unit is a functional membrane that preferentially permeates volatile aromatic compounds including alcohols, esters, aldehydes, and acids.

[0014] Further, the alcohols are one or more of ethanol, phenethyl alcohol, isoamyl alcohol, isobutylmethanol, isobutanol, or sec-butanol; the esters are one or more of ethyl lactate, ethyl acetate, ethyl formate, ethyl propionate, or ethyl acetate; the aldehydes are one or more of furfural, benzaldehyde, acetaldehyde, isobutyraldehyde, isovaleraldehyde, or acetal; and the volatile aromatic acids are one or two of lactic acid or acetic acid.

[0015] Furthermore, the organic-permeable membrane in the organic-permeable membrane separator is a composite membrane composed of a base membrane layer and an active layer. The base membrane layer is made of cellulose acetate, dimethylacetamide, ethylenediaminopropylmethyldimethoxysilane, and polyethylene glycol 400, while the active layer is made of hydroxyl-terminated fluorosilicone oil, di(dimethylamino)methylvinylsilane, hydrogen-containing silicone oil, and chloroplatinic acid.

[0016] Preferably, the organic-permeable membrane in the organic-permeable membrane separator is prepared by the following method: (0-1) Mix vinyl-terminated fluorosilicone oil with hydrogen-containing silicone oil, chloroplatinic acid, reaction solvent n-heptane and reaction inhibitor maleic acid, stir at 30~45℃, and stop stirring when the viscosity reaches 40~80 mPa·s to obtain fluoromodified silicone rubber solution. (0-2) Mix cellulose acetate, dimethylacetamide, ethylenediaminopropylmethyldimethoxysilane and polyethylene glycol 400, stir at 55℃~70℃ for 18~36 hours, coat the mixture onto the surface of a nonwoven fabric, and invert the phase in a water bath to obtain a base film. (0-3) The fluorine-modified silicone rubber solution obtained in step (0-1) is uniformly coated on the surface of the base film prepared in step (0-2), and crosslinked at 80~100℃ for 3~5h to obtain the composite film.

[0017] Preferably, in step (1), the rice wine is pumped to the preferential organic membrane separator unit via a feed pump. Preferably, the head range of the feed pump is 10~50m.

[0018] Preferably, in step (2), the vacuum level on the permeate side of the organic membrane separator is controlled by a vacuum pump.

[0019] Preferably, in step (2), the feed temperature on the raw material side of the preferred organic membrane separator is 25-50°C, and the membrane flow rate is 0.08-2 m / s.

[0020] This invention proposes a method for preparing rice-aroma baijiu and rice vinegar using huangjiu (yellow rice wine). It creatively employs a preferential organic permeation membrane. Because preferential organic permeation membranes exhibit different selective permeability to different substances, the preferential organic permeation membrane in this invention is specifically designed to preferentially permeate volatile aromatic compounds, including alcohols, esters, aldehydes, and acids. After treatment with the preferential organic permeation membrane, some of the volatile aromatic compounds of alcohols, esters, aldehydes, and acids in the huangjiu raw materials permeate through the membrane and are enriched in gaseous form on the permeate side. After condensation, the permeate is obtained, which is rice-aroma baijiu. The retained permeate is a mixture containing water, higher alcohols, higher acids, etc. After the separation process is complete, this mixture can be fermented, pressed, filtered, and blended by adding a certain amount of acetic acid bacteria solution to finally obtain rice vinegar.

[0021] The beneficial effects of this invention are: 1. This invention separates various substances in rice wine using a preferential organic permeation membrane separator. This separator employs a specific functional membrane that preferentially permeates volatile aromatic compounds, including alcohols, esters, aldehydes, and acids. This membrane effectively reduces the content of harmful components, including higher alcohols, and maximizes the extraction of various beneficial substances from the rice wine. By increasing the alcohol content and reducing the sugar content, the shelf life of this novel rice-aroma baijiu is extended. As an innovative product, it not only possesses the functions of ordinary baijiu but also retains the various beneficial substances and effects of rice wine. The remaining low-alcohol rice wine can be used to prepare rice vinegar, achieving maximum resource utilization of rice wine.

[0022] 2. This invention employs a novel membrane separation technology, which not only avoids the use of organic solvents or other third-party substances, achieving a green extraction process, but also features simple and efficient operation, low energy consumption, safety and environmental protection, reducing harmful components including higher alcohols while lowering costs. Detailed Implementation

[0023] The present invention will be further described below with reference to specific embodiments.

[0024] Example 1 The rice wine with an alcohol content of 12% (v / v) in the raw material tank is pumped to the preferential organic permeate membrane separator unit via a feed pump with a head of 10m. The preferential organic permeate membrane separator unit consists of two spiral wound preferential organic permeate membrane separators connected in series. The preferential organic permeate membrane separator includes a preferential organic permeate membrane, which is a specific functional membrane that preferentially permeates volatile aromatic compounds such as alcohols (ethanol, phenylethanol, isoamyl alcohol, isobutylmethanol, isobutanol or sec-butanol), esters (ethyl lactate, ethyl acetate, ethyl formate, ethyl propionate or ethyl acetate), aldehydes (furfural, benzaldehyde, acetaldehyde, isobutyraldehyde, isopentaldehyde or acetal), and acids (lactic acid or acetic acid). The organic-permeable membrane was prepared by the following method: Vinyl-terminated fluorosilicone oil was mixed with hydrogen-containing silicone oil, chloroplatinic acid, the reaction solvent n-heptane, and the reaction inhibitor maleic acid. The mixture was stirred at 30–45°C until the viscosity reached 40–80 mPa·s, at which point stirring was stopped to obtain a fluorinated silicone rubber solution. Cellulose acetate, dimethylacetamide, ethylenediaminepropylmethyldimethoxysilane, and polyethylene glycol 400 were mixed and stirred at 55–70°C for 18–36 hours. The mixture was then coated onto a nonwoven fabric surface and subjected to phase inversion in a water bath to obtain a base membrane. The obtained fluorinated silicone rubber solution was uniformly coated onto the surface of the prepared base membrane and crosslinked at 80–100°C for 3–5 hours to obtain the composite membrane. A vacuum of 1500 Pa was applied to the permeate side of the organic-permeable membrane separator. The feed temperature on the feed side of the organic-permeable membrane separator was 25°C, and the membrane surface flow rate was 0.08 m / s. Some organic compounds in rice wine, including alcohols, esters, aldehydes, and volatile aromatic compounds such as acids, selectively permeate through the membrane and vaporize into organic vapor. After condensation in a condenser, the permeate is obtained, which is a rice-aroma type of rice wine with an alcohol volume fraction of 28%. Other substances that do not permeate through the membrane, including water, higher alcohols, and higher acids, are returned to the rice wine raw material tank for further circulation and separation. The separation process stops when the alcohol volume fraction of the permeate in the raw material tank reaches 4%. This mixture can be fermented, pressed, filtered, and blended by adding a certain amount of acetic acid bacteria solution to finally obtain rice vinegar.

[0025] Example 2 Yellow rice wine with an alcohol content of 14% (v / v) from the raw material tank is pumped to a preferential organic permeate membrane separator unit via a feed pump with a head of 30m. The preferential organic permeate membrane separator unit consists of one spiral wound preferential organic permeate membrane separator and one tubular membrane separator connected in parallel. The preferential organic permeate membrane separator includes preferential organic permeate membranes, all of which are specific functional membranes that preferentially permeate volatile aromatic compounds including alcohols, esters, aldehydes, and acids. The preparation method of the preferential organic permeate membrane is the same as in Example 1. A vacuum is applied to the permeate side of the preferential organic permeate membrane separator unit, with a vacuum degree of 3500 Pa. The feed temperature on the raw material side of the preferential organic permeate membrane separator unit is 40℃, and the membrane surface flow rate is 1.2 m / s. Some organic compounds in rice wine, including alcohols, esters, aldehydes, and volatile aromatic compounds such as acids, selectively permeate through the membrane and vaporize into organic vapor. After condensation in a condenser, the permeate is obtained, which is a rice-aroma type of rice wine with an alcohol volume fraction of 35%. Other substances that do not permeate through the membrane, including water, higher alcohols, and higher acids, are returned to the rice wine raw material tank for further circulation and separation. The separation process stops when the alcohol volume fraction of the permeate in the raw material tank reaches 8%. This mixture can be fermented, pressed, filtered, and blended after adding a certain amount of acetic acid bacteria solution to finally obtain rice vinegar.

[0026] Example 3 Yellow rice wine with an alcohol content of 18% (v / v) from the raw material tank is pumped to a preferential organic permeate membrane separator unit via a feed pump with a head of 50m. The preferential organic permeate membrane separator unit consists of two spiral wound preferential organic permeate membrane separators connected in series and one tubular preferential organic permeate membrane separator connected in parallel. The preferential organic permeate membrane separator includes preferential organic permeate membranes, all of which are specific functional membranes that preferentially permeate volatile aromatic compounds including alcohols, esters, aldehydes, and acids. The preparation method of the preferential organic permeate membranes is the same as in Example 1. A vacuum is applied to the permeate side of the preferential organic permeate membrane separator unit, with a vacuum degree of 9500 Pa. The feed temperature on the raw material side of the preferential organic permeate membrane separator unit is 50℃, and the membrane surface flow rate is 2 m / s. Some organic compounds in rice wine, including alcohols, esters, aldehydes, and volatile aromatic compounds such as acids, selectively permeate through the membrane and vaporize into organic vapor. After condensation in a condenser, the permeate is obtained, which is a rice-aroma type of rice wine with an alcohol volume fraction of 40%. Other substances that do not permeate through the membrane, including water, higher alcohols, and higher acids, are returned to the rice wine raw material tank for further circulation and separation. The separation process stops when the alcohol volume fraction of the permeate in the raw material tank reaches 5%. This mixture can be fermented, pressed, filtered, and blended by adding a certain amount of acetic acid bacteria solution to finally obtain rice vinegar.

Claims

1. A method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine, characterized in that, Includes the following steps: (1) The rice wine in the raw material tank is transported to the preferential organic permeate membrane separation unit; the preferential organic permeate membrane in the preferential organic permeate membrane separation unit is a composite membrane composed of a base membrane layer and an active layer, wherein the base membrane layer is prepared by cellulose acetate, dimethylacetamide, ethylenediaminopropylmethyldimethoxysilane and polyethylene glycol 400, and the active layer is prepared by hydroxyl-terminated fluorosilicone oil, di(dimethylamino)methylvinylsilane, hydrogen-containing silicone oil and chloroplatinic acid; The organic-permeable membrane in the organic-permeable membrane separator is prepared by the following method: a. Mix vinyl-terminated fluorosilicone oil with hydrogen-containing silicone oil, chloroplatinic acid, reaction solvent n-heptane and reaction inhibitor maleic acid, stir at 30~45℃, and stop stirring when the viscosity reaches 40~80 mPa·s to obtain fluoromodified silicone rubber solution. b. Mix cellulose acetate, dimethylacetamide, ethylenediaminopropylmethyldimethoxysilane and polyethylene glycol 400, stir at 55℃~70℃ for 18~36 hours, coat the mixture onto the surface of a nonwoven fabric, and invert the phase in a water bath to obtain a base film. c. The fluorine-modified silicone rubber solution obtained in step a is uniformly coated on the surface of the base film prepared in step b, and crosslinked at 80~100℃ for 3~5h to obtain the composite film; (2) The vacuum degree on the permeate side of the preferential organic matter membrane separator is controlled to be 1500-9500 Pa. Organic matter in rice wine selectively permeates through the membrane and vaporizes into organic matter vapor. The residual liquid is returned to the raw material tank and participates in the circulation separation. (3) The organic vapor obtained in step (2) is condensed to obtain rice-fragrant baijiu; (4) After the separation process is stopped, the residual liquid in the raw material tank is prepared into rice vinegar.

2. The method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine according to claim 1, characterized in that: The volume fraction of alcohol in the rice wine in step (1) is 12%~18%; the volume fraction of alcohol in the rice-flavored baijiu in step (3) is 28%~40%.

3. The method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine according to claim 1, characterized in that: The separation process described in step (4) is stopped when the volume fraction of alcohol in the raw material tank is 4% to 8%.

4. The method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine according to claim 1, characterized in that: The method for preparing rice vinegar from the residual liquid in step (4) is as follows: add acetic acid bacteria solution to the residual liquid, and then ferment, press, filter, and blend to obtain rice vinegar.

5. The method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine according to claim 1, characterized in that: The preferred organic permeable membrane separation unit consists of at least one preferred organic permeable membrane separator connected in series, parallel, or a combination of series and parallel.

6. The method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine according to claim 5, characterized in that: The preferred organic membrane separator is either tubular or spiral wound.

7. The method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine according to claim 1, characterized in that: The preferred organic permeation membrane in the preferred organic permeation membrane separator is a functional membrane that preferentially permeates volatile aromatic compounds including alcohols, esters, aldehydes, and acids.

8. The method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine according to claim 7, characterized in that: The alcohols are one or more of ethanol, phenethyl alcohol, isoamyl alcohol, isobutylmethanol, isobutanol, or sec-butanol; the esters are one or more of ethyl lactate, ethyl formate, ethyl propionate, or ethyl acetate; the aldehydes are one or more of furfural, benzaldehyde, acetaldehyde, isobutyraldehyde, isovaleraldehyde, or acetal; and the volatile aromatic acids are one or two of lactic acid or acetic acid.

9. The method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine according to claim 1, characterized in that: In step (1), the rice wine is transported to the preferential organic permeate membrane separator unit via a feed pump; in step (2), the vacuum level on the permeate side of the preferential organic permeate membrane separator unit is controlled by a vacuum pump; in step (2), the feed temperature on the raw material side of the preferential organic permeate membrane separator unit is 25-50℃, and the membrane surface flow rate is 0.06-2 m / s.

10. The method for preparing rice-aroma type white wine and rice vinegar using yellow rice wine according to claim 9, characterized in that: The head range of the feed pump is 10~50m.