Device and method for preparing non-alcoholic wine or high-alcohol wine
The double-membrane method separates and processes raw wine, which solves the problems of heat-sensitive substances and easily oxidized components in the preparation of non-alcoholic or high-alcohol wine, and achieves high-quality wine preparation and effective utilization of resources.
Patent Information
- Application Number
- CN202111589151.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-12-23
- Publication Date
- 2025-01-21
- Estimated Expiration
- 2041-12-23
AI Technical Summary
In the prior art, when preparing alcohol-free or high-alcohol wine, heat-sensitive substances are easily destroyed and the components are easily deteriorated, resulting in poor quality of the wine.
The double-membrane method is used to separate the original wine at low temperature or normal temperature through the filter membrane component, intercepting pigments, residual sugar, protein, amino acids and a small amount of macromolecular aroma components, and using the alcohol-permeable membrane component to process the colorless wine on the permeation side to form high-quality wine and alcohol-free wine. Water, dilute the colored wine on the retentate side to prepare non-alcoholic wine.
It effectively avoids the destruction of heat-sensitive substances and the deterioration of easily oxidized components, ensuring the quality and taste of wine, while maximizing the utilization of resources, and is suitable for industrial production.
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Figure CN114181791B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of wine making, and in particular relates to a device and method for preparing non-alcoholic wine or high-proof wine by a double-membrane method. Background Art
[0002] In recent years, low-alcohol and non-alcoholic beverages have shown a clear growth trend worldwide. The low-alcohol craze has begun to show signs, and at the same time, more and more non-alcoholic wines are entering China. On the other hand, brandy is often called the "soul of wine". It is expensive and there are few types of domestic brandy. Because brandy has a fashionable appearance and the connotation of white wine, it can meet people's pursuit of life taste and will become a substitute for white wine consumption to some extent. Against this background, brandy will usher in a new era of development in the Chinese market.
[0003] Patent CN109593619A proposes a system and method for simultaneously preparing non-alcoholic wine and strong wine. The non-alcoholic wine in this patent is prepared at a temperature of about 40°C, which greatly damages the heat-sensitive substances in the original wine and partially deteriorates the easily oxidized components in the original wine. Summary of the invention
[0004] The purpose of the present invention is to provide a device and method for preparing alcohol-free wine or strong wine by a double membrane method. The method uses a filter membrane to separate raw wine at low temperature or room temperature, intercepts pigments, residual sugar, protein, amino acids and a small amount of other macromolecular flavor components, and the heat-sensitive substances in the raw wine are mainly concentrated on the retentate side of the filter membrane. The colorless wine on the permeation side of the filter membrane is treated with an alcohol permeation membrane to form strong wine and alcohol-free water. The alcohol-free water dilutes the colored wine on the retentate side of the filter membrane to finally prepare alcohol-free wine, solving the problems of easy destruction of heat-sensitive substances and deterioration of easily oxidized components. The method has the characteristics of simple and effective operation, safety and environmental protection, small wine loss, reliable process, and applicability to industrial production.
[0005] To achieve the above purpose, the technical solution adopted by the present invention is as follows:
[0006] A device for preparing non-alcoholic wine or strong wine, comprising a raw material tank, an intermediate tank, a filter membrane assembly and an alcohol permeation membrane assembly.
[0007] The outlet of the raw material tank is connected to the filter membrane assembly, the outlet of the filter membrane assembly on the permeate side is connected to the intermediate tank, the outlet of the filter membrane assembly on the retentate side is connected to the raw material tank, and the filter membrane assembly includes a nanofiltration membrane or a decolorization membrane.
[0008] The outlet of the intermediate tank is connected to the raw material tank and the alcohol permeation membrane assembly through valves, and the retentate side outlet of the alcohol permeation membrane assembly is connected to the intermediate tank.
[0009] The filter membrane assembly can use nanofiltration membrane or decolorization membrane. After the nanofiltration membrane is filtered, the ethanol concentration in the permeate changes to a certain extent, while the decolorization membrane has no interception effect on alcohols and alcohol-soluble flavor components such as esters, acids, ketones and other small molecules, thus ensuring that the alcohol content before and after the membrane is unchanged. In specific applications, it can be selected according to actual needs.
[0010] Furthermore, the base membrane of the decolorization membrane is prepared by phase conversion of polyethyleneimine (PEI), N-methylpyrrolidone (NMP) and LiCl, the active layer of the decolorization membrane is polyvinyl alcohol (PVA) and polyacrylic acid (PAA) cross-linked by tetraethyl orthosilicate (TEOS), and the decolorization membrane also includes a pore blocking layer between the base membrane and the active layer. The base membrane prepared by phase conversion of polyethyleneimine (PEI), N-methylpyrrolidone (NMP) and LiCl has a larger permeation flux than the traditional PEI base membrane.
[0011] Furthermore, the pore-blocking layer material includes γ-aminopropyltriethoxysilane.
[0012] The decolorizing membrane is a beer decolorizing membrane, which can be used for decolorizing beer or wine.
[0013] Furthermore, the permeation side of the alcohol permeation membrane assembly is connected to a high wine tank.
[0014] Furthermore, a heater is provided before the inlet of the alcohol permeation membrane assembly, and the permeation side outlet of the alcohol permeation membrane assembly is connected to a condenser.
[0015] Furthermore, the alcohol permeation membrane assembly is driven by a vacuum pump.
[0016] Furthermore, a circulation pump is provided between the raw material tank and the filter membrane assembly or between the intermediate tank and the alcohol permeable membrane assembly.
[0017] Furthermore, a pump is provided between the intermediate tank and the raw material tank for conveying the retentate of the alcohol membrane.
[0018] Furthermore, the nanofiltration membrane is a solvent-resistant nanofiltration membrane, and the molecular weight cutoff of the nanofiltration membrane is 200-700 Daltons.
[0019] Furthermore, the alcohol permeation membrane assembly adopts an anti-pollution pervaporation membrane, which is a composite membrane that preferentially permeates organic matter. The composite membrane is composed of a base membrane layer and an active layer. The base membrane layer is composed of one or more of cellulose acetate, polytetrafluoroethylene, and polyvinylidene fluoride, and the active layer is composed of one or more of polydimethylsiloxane, polymethyloctylsiloxane, hexamethyldisilazane, and hydrophobic nano-titanium dioxide.
[0020] Preferably, the alcohol permeation membrane assembly or the filtration membrane assembly is composed of one membrane separator or at least two membrane separators connected in series, in parallel, or in a series-parallel mixture.
[0021] Preferably, the membrane separator of the alcohol permeation membrane module is of a scroll type.
[0022] Preferably, the membrane separator of the membrane filter assembly is in the form of a tube.
[0023] The present invention also provides a method for preparing non-alcoholic wine or high-proof wine using the above device, comprising the following steps:
[0024] (1) The raw liquor is sent to the filter membrane assembly for separation, and the liquid obtained on the retentate side of the filter membrane assembly is refluxed to the raw material tank for cyclic separation, and finally a primary filtration retentate is obtained in the raw material tank; the primary filtration permeate obtained on the permeate side of the filter membrane assembly enters the intermediate tank;
[0025] (2) sending the primary filtered permeate to the alcohol permeate membrane module for separation, and the liquid obtained on the retentate side of the alcohol permeate membrane module is refluxed to the intermediate tank for cyclic separation, and finally obtaining the primary alcohol permeate retentate in the intermediate tank; and obtaining the first strong liquor on the retentate side of the alcohol permeate membrane module;
[0026] (3) The first alcohol permeate is sent from the intermediate tank to the raw material tank to be mixed with the first filtration permeate to obtain low-alcohol wine.
[0027] The low-alcohol wine has a low alcohol content, but contains residual sugar, protein, amino acids and a small amount of other macromolecular flavor components. If the non-alcohol wine is obtained by diluting with water, the taste of the non-alcohol wine deteriorates due to the large amount of water used for dilution. Therefore, the method of the present invention can ensure that the concentration of pigments and the like of the original wine and the low-alcohol wine remains unchanged, and only the alcohol content is reduced to the target range.
[0028] The filter membrane mainly intercepts pigments, residual sugars, proteins, amino acids and a small amount of other macromolecular flavor components.
[0029] Preferably, the alcohol content of the original liquor in step (1) is 8-13°. The alcohol content of the first high-alcohol liquor obtained in step (2) is 35-45°.
[0030] Preferably, the operating temperature of the filter membrane assembly is 0.5~25°C.
[0031] When a decolorizing membrane is used, the alcohol content of the original wine, the filtered retentate, and the filtered permeate remains unchanged before and after separation by the membrane assembly.
[0032] Preferably, the alcohol content of the first alcohol permeate in step (2) is 0.1-0.3°.
[0033] Preferably, the operating conditions of the alcohol permeable membrane module are a temperature of 40-45° C., a membrane surface flow rate of 0.1-0.6 m / s, and a vacuum degree of 2000-6000 Pa.
[0034] Preferably, the alcohol content of the low-alcohol wine is 4-6°.
[0035] Preferably, the weight ratio of the primary filtered permeate to the original wine is 0.8~0.9:1.
[0036] Preferably, the method for preparing non-alcoholic wine or high-proof wine further comprises step (5):
[0037] (5) The low-alcohol wine is sent to the filter membrane assembly for separation, and the liquid obtained on the retentate side of the filter membrane assembly is returned to the raw material tank for circulation and separation, and finally a secondary filtration retentate is obtained in the raw material tank; the secondary filtration permeate obtained on the permeate side of the filter membrane assembly enters the intermediate tank;
[0038] The secondary filtered permeate is sent to the alcohol permeate membrane module for separation, and the liquid obtained on the retentate side of the alcohol permeate membrane module is refluxed to the intermediate tank for cyclic separation, and finally a secondary alcohol permeate retentate is obtained in the intermediate tank; the second alcohol liquor is obtained on the retentate side of the alcohol permeate membrane module;
[0039] The secondary alcohol permeate is sent from the intermediate tank to the raw material tank to be mixed with the secondary filtration permeate or the primary alcohol permeate to obtain alcohol-free wine.
[0040] When the alcohol-free wine is obtained, the specific mixing ratio of the secondary alcohol permeate, the primary alcohol permeate and the secondary filtration permeate can be formulated according to actual product standards.
[0041] The original liquor processed only through steps (1) to (4) can only produce a first-proof liquor that meets actual needs, but the alcohol content of the low-alcohol liquor is often not low enough to meet the requirements of alcohol-free liquor. The alcohol-free liquor produced through step (5) can further reduce the alcohol content to 0.1-0.5° while maintaining the taste of the liquor.
[0042] The second high-proof liquor obtained by the treatment in step (5) has an alcohol content of 25-35°.
[0043] Preferably, in step (5), the weight ratio of the secondary filtered permeate to the low-alcohol wine is 0.7-0.85:1.
[0044] The present invention proposes a device and method for preparing alcohol-free wine or high-proof wine by using a double membrane method. First, a filter membrane assembly is used to separate the original wine at low temperature. The filter membrane mainly intercepts pigments, residual sugar, protein, amino acids and a small amount of other macromolecular flavor components. The heat-sensitive substances in the original wine are mainly concentrated on the retentate side of the filter membrane, while the permeate side is colorless and transparent. After the permeate on the permeate side is treated by the alcohol permeation membrane assembly, most of the alcohols and alcohol-soluble flavor components therein are enriched on the permeate side of the membrane, and the permeate side obtains the enriched high-proof wine; while the retained retentate is an alcohol-free aqueous solution. In the process of step (5), the alcohol-free water dilutes the filtered retentate to reduce the degree, and then passes through the filter membrane assembly again. The permeate of the filter membrane assembly is treated by the alcohol permeation membrane assembly. The permeate of the alcohol permeation membrane assembly is a high-proof wine with a temperature of more than 25°, and the retentate is an alcohol-free aqueous solution. The alcohol-free water obtained twice and the retentate of the filter membrane assembly (secondary filtration retentate) are mixed and reduced in degree, and finally an alcohol-free wine with a temperature of less than 0.5° is formed.
[0045] The beneficial effects of the present invention are:
[0046] The present invention adopts a double membrane method, that is, a nanofiltration membrane or a decolorization membrane and an alcohol permeation membrane combination technology to separate various substances in the original wine. The non-alcoholic wine is prepared by a filter membrane at room temperature or low temperature, which causes minimal damage to the heat-sensitive substances in the original wine and prevents the easily oxidized components in the original wine from deteriorating.
[0047] The alcohol-free water on the retentate side of the alcohol permeation membrane is used as dilution and alcohol reduction water, without introducing new components from the outside. Moreover, this alcohol-free water comes entirely from the fermentation of grains or fruits themselves. The alcohol-free wine produced has a refreshing and natural taste without watery taste, while achieving the maximum resource utilization of the original wine.
[0048] (3) The present invention not only avoids the use of organic solvents or other third-party substances, but also realizes a green extraction process. It has the characteristics of simple and effective operation, safety and environmental protection, small wine loss, reliable process, and applicability to industrial production. BRIEF DESCRIPTION OF THE DRAWINGS
[0049] Figure 1 It is a schematic diagram of the device for preparing non-alcoholic wine or strong wine according to the present invention.
[0050] Among them, 1 is the raw material tank, 2 is the first circulation pump, 3 is the filter membrane assembly, 4 is the pump, 5 is the intermediate tank, 6 is the second circulation pump, 7 is the heater, 8 is the alcohol permeation membrane assembly, 9 is the condenser, 10 is the high wine tank, and 11 is the vacuum pump. DETAILED DESCRIPTION
[0051] The present invention is further described below in conjunction with specific implementation modes.
[0052] like Figure 1 The device for preparing non-alcoholic wine or high-alcohol wine shown in the figure comprises a raw material tank, an intermediate tank, a filter membrane assembly and an alcohol permeation membrane assembly.
[0053] The outlet of the raw material tank is connected to the filter membrane assembly, the outlet of the filter membrane assembly on the permeate side is connected to the intermediate tank, the outlet of the filter membrane assembly on the retentate side is connected to the raw material tank, and the filter membrane assembly includes a nanofiltration membrane or a decolorization membrane.
[0054] The outlet of the intermediate tank is connected to the raw material tank and the alcohol permeation membrane assembly through valves, and the retentate side outlet of the alcohol permeation membrane assembly is connected to the intermediate tank.
[0055] The base film of the decolorizing film is a composite base film of polyethyleneimine (PEI), N-methylpyrrolidone (NMP) and LiCl, the active layer of the decolorizing film is polyvinyl alcohol (PVA) and polyacrylic acid (PAA) cross-linked with tetraethyl orthosilicate (TEOS), and the decolorizing film also includes a pore blocking layer between the base film and the active layer.
[0056] The pore-blocking layer material includes γ-aminopropyltriethoxysilane.
[0057] The decolorizing membrane is a beer decolorizing membrane, which can be used for decolorizing beer or wine.
[0058] The permeation side of the alcohol permeation membrane assembly is connected to a height wine tank.
[0059] A heater is arranged before the inlet of the alcohol permeation membrane assembly, and the permeation side outlet of the alcohol permeation membrane assembly is connected to a condenser.
[0060] The alcohol permeation membrane assembly is driven by a vacuum pump.
[0061] A circulation pump is provided between the raw material tank and the filter membrane assembly or between the intermediate tank and the alcohol permeable membrane assembly.
[0062] A pump is provided between the intermediate tank and the raw material tank for conveying alcohol-free water.
[0063] The nanofiltration membrane is a solvent-resistant nanofiltration membrane, and the molecular weight cutoff of the nanofiltration membrane is 200-700 Daltons.
[0064] The alcohol permeation membrane assembly adopts an anti-pollution pervaporation membrane, which is a composite membrane that preferentially permeates organic matter. The composite membrane consists of a base membrane layer and an active layer. The base membrane layer consists of one or more of cellulose acetate, polytetrafluoroethylene, and polyvinylidene fluoride, and the active layer consists of one or more of polydimethylsiloxane, polymethyloctylsiloxane, hexamethyldisilazane, and hydrophobic nano-titanium dioxide.
[0065] Example 1
[0066] The original wine with an alcohol content of 8° was separated by a filter membrane assembly at an operating temperature of 0.5°C. After the separation was completed, a first-filter permeate with an alcohol content of 8.2° was formed on the permeate side, and a first-filter permeate with an alcohol content of 7.2° was formed on the retentate side. The weight of the first-filter permeate / the weight of the original wine was 0.8. The first-filter permeate was separated by a pervaporation alcohol permeation membrane assembly. Alcohols and alcohol-soluble flavor components preferentially permeated the membrane. The first high-alcohol wine with an alcohol content of 35° was obtained on the permeate side, and the first-filter permeate with an alcohol content of 0.1° was obtained on the retentate side. The first-filter permeate permeate and the first-filter permeate were mixed and diluted to form a low-alcohol wine with an alcohol content of 4°.
[0067] The low-alcohol wine is then separated through a filter membrane assembly, and finally a secondary filtration permeate with an alcohol content of 4.2° is formed on the permeate side, and a secondary filtration permeate with an alcohol content of 3.5° is formed on the retentate side. The weight of the secondary filtration permeate / the weight of the low-alcohol wine is 0.7. The secondary filtration permeate is passed through an alcohol permeation membrane assembly, and ethanol preferentially passes through the membrane. A second high-alcohol wine with an alcohol content of 25° is obtained on the permeate side, and a secondary alcohol permeate permeate with an alcohol content of 0.1° is obtained on the retentate side. The alcohol permeate permeate and the secondary filtration permeate obtained in the two steps are mixed and reduced to form a finished non-alcoholic wine with an alcohol content of 0.1°.
[0068] The membrane filter assembly in this embodiment 1 adopts a tubular solvent-resistant nanofiltration membrane with a molecular weight cutoff of 200 Daltons, which mainly intercepts pigments, residual sugars, proteins, amino acids and a small amount of other macromolecular flavor components, and the ethanol concentration of the filtered permeate is higher than that of the original wine. The anti-pollution pervaporation roll membrane used in the alcohol permeation membrane assembly is a composite membrane that preferentially permeates alcohol-soluble substances such as alcohols, esters, ketones, and acids, and is composed of a base membrane layer and an active layer, wherein the base membrane layer is composed of polytetrafluoroethylene and polyvinylidene fluoride, and the active layer is composed of polymethyloctylsiloxane, hexamethyldisilazane, and hydrophobic nano-titanium dioxide. The operating conditions of the alcohol permeation membrane assembly are a temperature of 40°C, a membrane surface flow rate of 0.1 m / s, and a vacuum degree of 6000 Pa.
[0069] Example 2
[0070] The original wine with an alcohol content of 12.5° was separated by a membrane filter assembly at an operating temperature of 10°C. After the separation was completed, a first-filter permeate with an alcohol content of 12.8° was formed on the permeate side, and a first-filter permeate with an alcohol content of 10.8° was formed on the retentate side. The weight of the first-filter permeate / the weight of the original wine was 0.85. The first-filter permeate was separated by a pervaporation alcohol permeation membrane assembly. Alcohols and alcohol-soluble flavor components preferentially permeated the membrane. The first high-alcohol wine with an alcohol content of 40° was obtained on the permeate side, and the first-filter permeate with an alcohol content of 0.2° was obtained on the retentate side. The first-filter permeate permeate and the first-filter permeate were mixed and diluted to form a low-alcohol wine with an alcohol content of 5°.
[0071] The low-alcohol wine is then separated through a filter membrane assembly, and a secondary filtration permeate with an alcohol content of 5.2° is formed on the permeate side, and a secondary filtration permeate with an alcohol content of 4.2° is formed on the retentate side. The weight of the secondary filtration permeate / the weight of the low-alcohol wine is 0.8. The secondary filtration permeate is passed through an alcohol permeation membrane assembly, and a second high-alcohol wine with an alcohol content of 30° is obtained on the permeate side, and a secondary alcohol permeate permeate with an alcohol content of 0.1° is obtained on the retentate side. The alcohol permeate permeate and the secondary filtration permeate obtained in the two steps are mixed and reduced to form a finished non-alcoholic wine with an alcohol content of 0.3°.
[0072] The nanofiltration membrane assembly in this embodiment 2 adopts a tubular solvent-resistant nanofiltration membrane with a nanofiltration membrane cutoff molecular weight of 500 Daltons, which mainly intercepts pigments, residual sugars, proteins, amino acids and a small amount of other macromolecular flavor components, and the ethanol concentration of the filtered permeate is higher than that of the original wine. The anti-pollution pervaporation roll membrane used in the alcohol permeation membrane assembly is a composite membrane that preferentially permeates alcohol-soluble substances such as alcohols, esters, ketones, and acids, and is composed of a base membrane layer and an active layer, wherein the base membrane layer is composed of polytetrafluoroethylene, and the active layer is composed of polydimethylsiloxane, hexamethyldisilazane, and hydrophobic nano-titanium dioxide. The operating conditions of the alcohol permeation membrane assembly are a temperature of 42°C, a membrane surface flow rate of 0.3 m / s, and a vacuum degree of 5000 Pa.
[0073] Example 3
[0074] The original wine with an alcohol content of 13° was separated by a membrane filter assembly at an operating temperature of 25°C. After the separation was completed, a first-filter permeate with an alcohol content of 13.5° was formed on the permeate side, and a first-filter permeate with an alcohol content of 8.5° was formed on the retentate side. The weight of the first-filter permeate / the weight of the original wine was 0.9. The first-filter permeate was separated by a pervaporation alcohol permeation membrane assembly. Alcohols and alcohol-soluble flavor components preferentially permeated the membrane. The first high-alcohol wine with an alcohol content of 45° was obtained on the permeate side, and the first-filter permeate with an alcohol content of 0.3° was obtained on the retentate side. The first-filter permeate permeate and the first-filter permeate were mixed and diluted to form a low-alcohol wine with an alcohol content of 6°.
[0075] The low-alcohol wine is then separated through a filter membrane assembly, and a secondary filtration permeate with an alcohol content of 6.3° is formed on the permeate side, and a secondary filtration permeate with an alcohol content of 4.3° is formed on the retentate side. The weight of the secondary filtration permeate / the weight of the low-alcohol wine is 0.85. The secondary filtration permeate is passed through an alcohol permeation membrane assembly, and ethanol preferentially permeates the membrane. A second high-alcohol wine with an alcohol content of 35° is obtained on the permeate side, and a secondary alcohol permeate with an alcohol content of 0.1° is obtained on the retentate side. The alcohol permeate retentate and the secondary filtration retentate obtained in the two steps are mixed and reduced to form a finished non-alcoholic wine with an alcohol content of 0.5°.
[0076] In this embodiment 3, the nanofiltration membrane assembly adopts a tubular solvent-resistant nanofiltration membrane with a molecular weight cutoff of 700 Daltons, which mainly intercepts pigments, residual sugars, proteins, amino acids and a small amount of other macromolecular flavor components. The ethanol concentration on the permeate side after filtration is higher than that of the original wine. The anti-pollution pervaporation roll membrane used in the alcohol permeation membrane assembly is a composite membrane that preferentially permeates alcohol-soluble substances such as alcohols, esters, ketones, and acids, and is composed of a base membrane layer and an active layer, wherein the base membrane layer is composed of cellulose acetate and polyvinylidene fluoride, and the active layer is composed of polydimethylsiloxane and hydrophobic nano titanium dioxide. The operating conditions of the alcohol permeation membrane assembly are a temperature of 45°C, a membrane surface flow rate of 0.6 m / s, and a vacuum degree of 2000 Pa.
[0077] Example 4
[0078] Dissolve PVA powder in 95℃ hot water to prepare 8% PVA solution; dissolve PAA powder in 90℃ hot water to prepare 3% PAA solution; mix the above two solutions in a ratio of 1:5 and stir for 24 hours until evenly mixed. Add TEOS to the mixed solution, TEOS accounts for 3% of the total solution, and stir evenly to obtain a hydrophilic coating solution. Mix γ-aminopropyltriethoxysilane, water, and ethanol in a weight ratio of 15:35:50 to prepare a plugging solution. Prepare PEI, NMP, and LiCl in a weight ratio of 20:70:10 to prepare a base film solution, apply it on the surface of the non-woven fabric, and then immerse it in 25℃ deionized water to prepare a base film. The base film is then immersed in the above-mentioned plugging solution for 15 minutes, and the membrane surface is wiped dry. The hydrophilic coating liquid was then coated on the surface of the PEI base film by slit extrusion coating at a solution extrusion rate of 1.5 mL / min, and placed in a 150°C oven for interfacial polymerization reaction for 8 hours to obtain a decolorized film.
[0079] The original wine with an alcohol content of 13° was separated by a filter membrane assembly at an operating temperature of 20°C. After the separation was completed, a first-filter permeate with an alcohol content of 13° was formed on the permeate side, and a first-filter permeate with an alcohol content of 13° was formed on the retentate side. The weight of the first-filter permeate / the weight of the original wine was 0.9. The first-filter permeate was separated by a pervaporation alcohol permeation membrane assembly, and a first-alcohol permeate with an alcohol content of 45° was obtained on the permeate side, and a first-filter permeate with an alcohol content of 0.3° was obtained on the retentate side. The first-filter permeate permeate and the first-filter permeate were mixed and diluted to form a low-alcohol wine with an alcohol content of 6°.
[0080] Then the low alcohol wine is separated by a filter membrane assembly, and a secondary filtration permeate with an alcohol content of 6° is formed on the permeate side, and a secondary filtration retentate with an alcohol content of 6° is formed on the retentate side. The weight of the secondary filtration permeate / the weight of the low alcohol wine is 0.8. The secondary filtration permeate is passed through an alcohol permeation membrane assembly, and ethanol preferentially permeates the membrane. A second high alcohol with an alcohol content of 30° is obtained on the permeate side, and a secondary alcohol permeate retentate with an alcohol content of 0.1° is obtained on the retentate side. The alcohol permeate retentate and the secondary filtration retentate obtained in the two steps are mixed and reduced to form a finished non-alcoholic wine with an alcohol content of 0.5°.
[0081] In this embodiment 4, the filter membrane assembly adopts a tubular decolorizing membrane with a molecular weight cutoff of 200 Daltons, which mainly intercepts pigments, residual sugars, proteins, amino acids and a small amount of other macromolecular flavor components. The anti-pollution pervaporation roll membrane used in the alcohol permeation membrane assembly is a composite membrane that preferentially permeates alcohol-soluble substances such as alcohols, esters, ketones, and acids, and is composed of a base membrane layer and an active layer, wherein the base membrane layer is composed of cellulose acetate and polyvinylidene fluoride, and the active layer is composed of polydimethylsiloxane and hydrophobic nano titanium dioxide. The operating conditions of the alcohol permeation membrane assembly are a temperature of 45°C, a membrane surface flow rate of 0.6 m / s, and a vacuum degree of 2000Pa.
[0082] Example 5
[0083] Dissolve PVA powder in 85℃ hot water to prepare a 5% PVA solution; dissolve PAA powder in 90℃ hot water to prepare a 1% PAA solution; mix the above two solutions in a 1:1 ratio and stir for 36 hours until they are evenly mixed. Add TEOS to the mixed solution, TEOS accounts for 1% of the total solution, and stir evenly to obtain a hydrophilic coating solution. Mix γ-aminopropyltriethoxysilane, water, and ethanol in a weight ratio of 10:30:60 to prepare a plugging solution. Prepare PEI, NMP, and LiCl in a weight ratio of 12:60:28 to prepare a base membrane solution, apply it on the surface of the non-woven fabric, and then immerse it in 25℃ deionized water to prepare a base membrane. The base membrane is then immersed in the above-mentioned plugging solution for 10 minutes, and the membrane surface is wiped dry. The hydrophilic coating liquid was then applied on the surface of the PEI base film by slit extrusion coating at a solution extrusion rate of 0.8 mL / min, and placed in a 130° C. oven for interfacial polymerization reaction for 4 hours to obtain a decolorized film.
[0084] The original wine with an alcohol content of 10° was separated by a filter membrane assembly at an operating temperature of 25°C. After the separation was completed, a first-filter permeate with an alcohol content of 10° was formed on the permeate side, and a first-filter permeate with an alcohol content of 10° was formed on the retentate side. The weight of the first-filter permeate / the weight of the original wine was 0.85. The first-filter permeate was separated by a pervaporation alcohol permeation membrane assembly, and a first-alcohol permeate with an alcohol content of 38° was obtained on the permeate side, and a first-filter permeate with an alcohol content of 0.2° was obtained on the retentate side. The first-filter permeate permeate and the first-filter permeate were mixed and diluted to form a low-alcohol wine with an alcohol content of 6°.
[0085] Then the low alcohol wine is separated by a filter membrane assembly, and a secondary filtration permeate with an alcohol content of 6° is formed on the permeate side, and a secondary filtration retentate with an alcohol content of 6° is formed on the retentate side. The weight of the secondary filtration permeate / the weight of the low alcohol wine is 0.85. The secondary filtration permeate is passed through an alcohol permeation membrane assembly, and ethanol preferentially passes through the membrane. A second high alcohol with an alcohol content of 32° is obtained on the permeate side, and a secondary alcohol permeate retentate with an alcohol content of 0.1° is obtained on the retentate side. The alcohol permeate retentate and the secondary filtration retentate obtained in the two steps are mixed and reduced to form a finished non-alcoholic wine with an alcohol content of 0.5°.
[0086] In this embodiment 5, the filter membrane assembly adopts a tubular decolorizing membrane with a molecular weight cutoff of 200 Daltons, which mainly intercepts pigments, residual sugars, proteins, amino acids and a small amount of other macromolecular flavor components. The anti-pollution pervaporation roll membrane used in the alcohol permeation membrane assembly is a composite membrane that preferentially permeates alcohol-soluble substances such as alcohols, esters, ketones, and acids, and is composed of a base membrane layer and an active layer, wherein the base membrane layer is composed of cellulose acetate and polyvinylidene fluoride, and the active layer is composed of polydimethylsiloxane and hydrophobic nano-titanium dioxide. The operating conditions of the alcohol permeation membrane assembly are a temperature of 45°C, a membrane surface flow rate of 0.6 m / s, and a vacuum degree of 2000Pa.
[0087] The filter membranes of Examples 1 to 3 are solvent-resistant nanofiltration membranes. Although they have a decolorization effect, the ethanol concentration on the permeate side is higher than that of the original wine. The filter membranes of Examples 4 to 5 are decolorization membranes, which only have a decolorization effect and have no interception effect on the alcohols and alcohol-soluble flavor components of the original wine, such as esters, acids, ketones and other small molecules. Therefore, the alcohol content before and after the filter membrane can be guaranteed to remain unchanged.
Claims
1. A device for preparing non-alcoholic wine or strong wine, characterized in that: Including raw material tank, intermediate tank, filter membrane assembly and alcohol permeation membrane assembly, The outlet of the raw material tank is connected to the filter membrane assembly, the outlet of the filter membrane assembly on the permeate side is connected to the intermediate tank, the outlet of the filter membrane assembly on the retentate side is connected to the raw material tank, and the filter membrane assembly includes a nanofiltration membrane or a decolorization membrane. The outlet of the intermediate tank is connected to the raw material tank and the alcohol permeation membrane assembly through valves, and the retentate side outlet of the alcohol permeation membrane assembly is connected to the intermediate tank; the alcohol permeation membrane assembly adopts an anti-pollution pervaporation membrane; The nanofiltration membrane is a solvent-resistant nanofiltration membrane, and the molecular weight cutoff of the nanofiltration membrane is 200-700 Daltons; The base film of the decolorizing film is prepared by phase conversion of polyethyleneimine, N-methylpyrrolidone and LiCl, the active layer of the decolorizing film is polyvinyl alcohol and polyacrylic acid cross-linked with tetraethyl orthosilicate, and the decolorizing film also includes a pore-blocking layer between the base film and the active layer; the material of the pore-blocking layer includes γ-aminopropyltriethoxysilane; The anti-pollution pervaporation membrane is a composite membrane that preferentially permeates organic matter. The composite membrane consists of a base membrane layer and an active layer. The base membrane layer consists of one or more of cellulose acetate, polytetrafluoroethylene, and polyvinylidene fluoride, and the active layer consists of one or more of polydimethylsiloxane, polymethyloctylsiloxane, hexamethyldisilazane, and hydrophobic nano-titanium dioxide.
2. The device for preparing non-alcoholic wine or strong wine according to claim 1, characterized in that: The alcohol permeable membrane assembly or the filter membrane assembly is composed of one membrane separator or at least two membrane separators connected in series, in parallel or in a series-parallel mixture.
3. The device for preparing non-alcoholic wine or strong wine according to claim 1, characterized in that: The membrane separator of the alcohol permeation membrane assembly is of a roll type; the membrane separator of the filtration membrane assembly is of a tube type.
4. A method for preparing non-alcoholic wine or strong wine using the device for preparing non-alcoholic wine or strong wine according to any one of claims 1 to 3, characterized in that: The steps include: (1) The raw liquor is sent to the filter membrane assembly for separation, and the liquid obtained on the retentate side of the filter membrane assembly is refluxed to the raw material tank for cyclic separation, and finally a primary filtration retentate is obtained in the raw material tank; the primary filtration permeate obtained on the permeate side of the filter membrane assembly enters the intermediate tank; (2) sending the primary filtered permeate to the alcohol permeate membrane module for separation, and the liquid obtained on the retentate side of the alcohol permeate membrane module is refluxed to the intermediate tank for cyclic separation, and finally obtaining the primary alcohol permeate retentate in the intermediate tank; and obtaining the first strong liquor on the retentate side of the alcohol permeate membrane module; (3) The first alcohol permeate is sent from the intermediate tank to the raw material tank to be mixed with the first filtration permeate to obtain low-alcohol wine.
5. The method according to claim 4, characterized in that The alcohol content of the original wine in step (1) is 8-13°.
6. The method according to claim 4, characterized in that The operating temperature of the filter membrane assembly is 0.5~25°C.
7. The method according to claim 4, characterized in that The operating conditions of the alcohol permeation membrane assembly are a temperature of 40-45°C, a membrane surface flow rate of 0.1-0.6 m / s, and a vacuum degree of 2000-6000 Pa.
8. The method according to claim 4, characterized in that The method for preparing non-alcoholic wine or high-proof wine further comprises step (5): (5) The low-alcohol wine is sent to the filter membrane assembly for separation, and the liquid obtained on the retentate side of the filter membrane assembly is returned to the raw material tank for circulation and separation, and finally a secondary filtration retentate is obtained in the raw material tank; the secondary filtration permeate obtained on the permeate side of the filter membrane assembly enters the intermediate tank; The secondary filtered permeate is sent to the alcohol permeate membrane module for separation, and the liquid obtained on the retentate side of the alcohol permeate membrane module is refluxed to the intermediate tank for cyclic separation, and finally a secondary alcohol permeate retentate is obtained in the intermediate tank; the second alcohol liquor is obtained on the retentate side of the alcohol permeate membrane module; The secondary alcohol permeate is sent from the intermediate tank to the raw material tank to be mixed with the secondary filtration permeate or the primary alcohol permeate to obtain alcohol-free wine.
Citation Information
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