A device for removing off-flavor and higher fatty acid esters from liquor

Abstract

The utility model discloses a device for removing the miscellaneous smell and senior fatty acid ester in the white spirit, the outlet of raw material tank is connected with membrane separator and chromatographic column through valve respectively, the permeation side outlet of membrane separator is connected with first product tank through condenser, the retentate side outlet of membrane separator is connected with raw material tank, and the outlet of chromatographic column is connected with second product tank. The utility model realizes the removal of the miscellaneous smell and senior fatty acid ester in the white spirit, makes the wine body more coordinated, improves the quality of white spirit, reduces the waste of resources, and has wide application prospect in the white spirit industry.

Description

Technical Field

[0001] This utility model belongs to the field of brewing technology, specifically relating to a device for removing off-flavors and higher fatty acid esters from baijiu (Chinese white liquor). Background Technology

[0002] In the traditional solid-state fermentation process of baijiu production, the lipases of microorganisms break down the fat in the grains into higher fatty acids. These higher fatty acids then undergo esterification with ethanol to produce higher fatty acid esters such as ethyl palmitate, ethyl oleate, and ethyl linoleate. When the content of these substances is too high, the overall taste of the liquor will be heavy and lacking in freshness, producing a noticeable greasy feeling, which seriously affects the sensory quality of the baijiu.

[0003] In addition, various off-flavor substances are produced during the fermentation and distillation of baijiu, with furfural being a typical example. Furfural has a strong, pungent odor and a bitter taste, and even extremely low concentrations can affect the overall flavor of the liquor. Other off-flavor components, such as sulfides, may also be present, severely compromising the flavor harmony of the baijiu. To address this, distilleries typically resort to methods like low-temperature freezing and activated carbon adsorption. However, these methods can lead to the loss of aroma components and excessive energy consumption. Improving the added value of defective baijiu and enhancing its overall quality is a pressing issue for many distilleries. Utility Model Content

[0004] The purpose of this invention is to provide a device for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor). This device combines membrane separation technology with column chromatography adsorption technology and is effectively used in defective liquor to address the problem of excessive off-flavors and higher fatty acid esters, thereby solving the problem of defective liquor, reducing resource waste, and creating good economic value and social benefits.

[0005] To achieve the above objectives, the present invention adopts the following technical solution: A device for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor). The outlet of feed tank 1 is connected to membrane separator 4 and chromatography column 3 via valves. The permeate-side outlet of membrane separator 4 is connected to first product tank 6 via condenser 5, and the residual outlet of membrane separator 4 is connected to feed tank 1. The outlet of the chromatography column 3 is connected to the second product tank 7.

[0006] Furthermore, a heat exchanger 2 is also provided between the outlet of the raw material tank 1 and the membrane separator 4.

[0007] Furthermore, a pump is also provided between the outlet of the raw material tank 1 and the heat exchanger 2.

[0008] Furthermore, a pump is also provided between the outlet of the raw material tank 1 and the chromatography column 3.

[0009] Furthermore, the condenser 5 is connected to a vacuum pump 8. By employing a vacuuming and condensation method, a vapor pressure difference is created between the upstream and downstream of the membrane, allowing for the separation of effective components and impurity components.

[0010] Furthermore, the first product tank 6 is connected to the second product tank 7.

[0011] Furthermore, the membrane of the membrane separator 4 is prior art, as described in CN113214947A.

[0012] Furthermore, the membrane is composed of a base film layer and an active layer; the base film layer is composed of one or more of cellulose acetate, polytetrafluoroethylene, polyvinylidene fluoride, or inorganic ceramics; the active layer is composed of one or more of polydimethylsiloxane, hydrophobic nano-titanium dioxide, or polyvinyl alcohol.

[0013] Furthermore, the membrane separator 4 is either spiral wound or tubular.

[0014] Furthermore, a pump is also provided between the chromatography column 3 and the second product tank 7.

[0015] This invention can be operated by those skilled in the art using general methods as needed. To achieve better product quality, it can also be operated as follows: (1) The raw material is heated to about 45°C by the heater 2 from the raw material tank 1 and sent to the membrane separator 4. Under the action of the vacuum pump 8 and the condenser 5, alcohol-soluble components such as ethyl hexanoate and ethyl acetate preferentially pass through the membrane. Pure wine is obtained by permeation and stored in the first product tank. The liquid on the permeate side is returned to the raw material tank 1.

[0016] (2) When the alcohol content of the osmotic liquid drops to 30°, the pervaporation membrane separation process is stopped, and the osmotic liquid in the raw material tank 1 is sent to the chromatography column for adsorption. The off-flavors and higher fatty acid esters are adsorbed, and the aroma liquid is obtained at the outlet of the chromatography column and sent to the second product tank 7.

[0017] (3) Mix the pure wine in the first product tank 6 with the flavor liquid in the second product tank 7 to obtain a white wine product with the impurities and high fatty acid esters removed.

[0018] The beneficial effects of this utility model are as follows: (1) The membrane separator used can effectively retain off-flavor substances and higher fatty acid esters, and the operating temperature is suitable, which is conducive to preserving the aroma components of the wine and provides convenient conditions for the next step of column adsorption.

[0019] (2) Membrane separators and chromatography column adsorption equipment occupy little space, are automatically controlled, are easy to operate, and are easy to industrialize.

[0020] (3) The adsorption of membrane separator and chromatography column is a purely physical process that will not introduce other components and will not generate secondary pollution.

[0021] (4) This utility model uses membrane separation technology to solve the problem of defective wine, realizes the removal of off-flavors and higher fatty acid esters in defective wine, makes the wine more harmonious, improves the quality of baijiu, reduces the waste of resources, and gives defective wine more room and ways to be used. Attached Figure Description

[0022] Figure 1 This is a schematic diagram of the device for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor) according to this utility model.

[0023] Among them, 1 is the raw material tank, 2 is the heat exchanger, 3 is the chromatography column, 4 is the membrane separator, 5 is the condenser, 6 is the first product tank, 7 is the second product tank, 8 is the vacuum pump, and 9, 10, 11 and 12 are all pumps. Detailed Implementation

[0024] The technical solution of this utility model is further illustrated below with reference to specific embodiments. These embodiments should not be construed as limiting the technical solution.

[0025] like Figure 1 The apparatus shown is for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor). The outlet of the raw material tank 1 is connected to a membrane separator 4 and a chromatography column 3 via valves. The permeate-side outlet of the membrane separator 4 is connected to a first product tank 6 via a condenser 5. The osmotic-side outlet of the membrane separator 4 is connected to the raw material tank 1. The outlet of the chromatography column 3 is connected to a second product tank 7.

[0026] A heat exchanger 2 is also provided between the outlet of the raw material tank 1 and the membrane separator 4.

[0027] A pump is also installed between the outlet of the raw material tank 1 and the heat exchanger 2.

[0028] A pump is also installed between the outlet of the raw material tank 1 and the chromatography column 3.

[0029] The condenser 5 is connected to the vacuum pump 8. By using vacuuming and condensation, a vapor pressure difference is created between the upstream and downstream of the membrane, which can separate the effective components and impurity components.

[0030] The first product tank 6 is connected to the second product tank 7.

[0031] The membrane of the membrane separator 4 is prior art, as described in CN113214947A.

[0032] The 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, polyvinylidene fluoride or inorganic ceramics; the active layer is composed of one or more of polydimethylsiloxane, hydrophobic nano-titanium dioxide or polyvinyl alcohol.

[0033] The membrane separator 4 is either a spiral wound type or a tubular type.

[0034] A pump is also provided between the chromatography column 3 and the second product tank 7.

[0035] Example 1 The following operations are performed using the aforementioned apparatus for removing off-flavors and higher fatty acid esters from baijiu: (1) Heat exchange: 5L of defective liquor is pumped into the raw material tank by the raw material pump. The defective liquor is then pumped from the raw material tank into the heat exchanger for preheating to about 45℃. Defective liquor testing and analysis: Sensory evaluation: poor aroma components, serious off-flavors, poor taste. Physicochemical indicators: alcohol content 52° (under standard conditions of 20℃, the same below), total acid 1.66g / L, hexanoic acid 28.74mg / 100mL, acetic acid 115.4mg. / 100mL, Ethyl hexanoate 120.6mg / 100mL, Ethyl lactate 230.2mg / 100mL, Ethyl ethyl acetate 40.9mg / 100mL, Ethyl butyrate 10.3mg / 100mL, Ethyl palmitate 60.74mg / 100mL, Ethyl oleate 23.64mg / 100mL, Ethyl linoleate 33.24mg / 100mL, Furfural 35.1mg / 100mL.

[0036] (2) The defective liquor heated in step (1) is introduced into the membrane separator. Vacuuming and condensation are used to form a vapor pressure difference between the upstream and downstream of the membrane, separating the effective components and impurities. The product that permeates through the membrane to the downstream side of the membrane is vaporized into a gaseous form under vacuum. This gaseous form enters the condenser under the action of the vacuum machine. The condensation temperature is -20℃. After cooling, it enters the first product tank in the form of pure liquor. The permeate side is stored in the raw material tank in liquid form. The liquid on the permeate side contains obvious off-flavors and high fatty acid esters.

[0037] (3) Chromatography column treatment: When the alcohol content of the osmotic liquid drops from 52° to 30°, the pervaporation membrane separation process is stopped. The osmotic liquid in the feed tank is pumped to the chromatography column for further adsorption. After adsorption is complete, it is collected in the second product tank. Column chromatography can remove off-flavors and higher fatty acid esters.

[0038] (4) Product mixing: The liquor in the first product tank and the second product tank are mixed to obtain a liquor product with impurities and high fatty acid esters removed.

[0039] Sensory evaluation of the baijiu product after removing off-flavors and higher fatty acid esters: The alcohol content showed no significant change, the aroma components were basically collected and preserved, the aroma was pure, there were no obvious off-flavors, and the body was clean. Physicochemical indicators: alcohol content 51° (under standard conditions at 20℃, the same below), total acid 1.66g / L, hexanoic acid 29.74mg / 100mL, acetic acid 113.2mg / 100mL, ethyl hexanoate 117.4mg / 100mL, ethyl lactate 224.2mg / 100mL, ethyl acetate 42.9mg / 100mL, ethyl butyrate 12.3mg / 100mL, ethyl palmitate 10.3mg / 100mL, ethyl oleate 9.4mg / 100mL, ethyl linoleate 5.21mg / 100mL, furfural 5mg / 100mL.

[0040] Example 2 (1) Heat exchange: 40L of defective liquor is pumped into the raw material tank by the raw material pump. The defective liquor is then pumped from the raw material tank to the raw material tank. The original aroma components are poor, the off-flavors are serious, and the taste is poor. The physicochemical indicators are: alcohol content 52° (under standard conditions of 20℃, the same below), total acid 1.66g / L, hexanoic acid 28.74mg / 100mL, acetic acid 115.4mg / 100mL, ethyl hexanoate 120.6mg / 100mL, ethyl lactate 230.2mg / 100mL, ethyl acetate 40.9mg / 100mL, ethyl butyrate 10.3mg / 100mL, ethyl palmitate 60.74mg / 100mL, ethyl oleate 23.64mg / 100mL, ethyl linoleate 33.24mg / 100mL, furfural 34.6mg / 100ml.

[0041] (2) The defective liquor heated in step (1) is put into the membrane separator. Vacuuming and condensation are used to form a vapor pressure difference between the upstream and downstream of the membrane to separate the effective components and impurities. The product that permeates through the membrane to the downstream side of the membrane is vaporized into a gaseous form under vacuum. The gaseous form enters the condenser under the action of the vacuum machine. The condensation temperature is -20℃. After cooling, it enters the first product tank in the form of pure liquor. The permeate side is stored in the raw material tank in liquid form. The liquid on the permeate side contains obvious off-flavors and high fatty acid esters.

[0042] (3) Chromatography column treatment: When the alcohol content of the osmotic liquid drops from 52° to 30°, the pervaporation membrane separation process is stopped. The osmotic liquid in the feed tank is pumped to the chromatography column for further adsorption. After adsorption is complete, it is collected in the second product tank. Column chromatography can remove off-flavors and higher fatty acid esters.

[0043] (4) Product mixing: The liquor in the first product tank and the second product tank are mixed to obtain a liquor product with impurities and high fatty acid esters removed.

[0044] Sensory evaluation of the baijiu product after removing off-flavors and higher fatty acid esters: The alcohol content showed no significant change, the aroma components were basically collected and preserved, the aroma was pure, there were no obvious off-flavors, and the body was clean. Physicochemical indicators: alcohol content 50° (under standard conditions at 20℃, the same below), total acid 1.76g / L, hexanoic acid 30.24mg / 100mL, acetic acid 114.3mg / 100mL, ethyl hexanoate 119.6mg / 100mL, ethyl lactate 220.7mg / 100mL, ethyl acetate 44.9mg / 100mL, ethyl butyrate 11.2mg / 100mL, ethyl palmitate 11.2mg / 100mL, ethyl oleate 9.2mg / 100mL, ethyl linoleate 6.1mg / 100mL, furfural 4.5mg / 100mL.

[0045] Example 3 (1) Heat exchange: 500L of defective liquor is pumped into the raw material tank by the raw material pump. The defective liquor is then pumped from the raw material tank to the raw material tank. The original aroma components are poor, the off-flavors are serious, and the taste is poor. The physicochemical indicators are: alcohol content 52° (under standard conditions of 20℃, the same below), total acid 1.66g / L, hexanoic acid 28.74mg / 100mL, acetic acid 115.4mg / 100mL, ethyl hexanoate 120.6mg / 100mL, ethyl lactate 230.2mg / 100mL, ethyl acetate 40.9mg / 100mL, ethyl butyrate 10.3mg / 100mL, ethyl palmitate 60.74mg / 100mL, ethyl oleate 23.64mg / 100mL, ethyl linoleate 33.24mg / 100mL, furfural 34.4mg / 100mL.

[0046] (2) The defective liquor heated in step (1) is put into the membrane separator. Vacuuming and condensation are used to form a vapor pressure difference between the upstream and downstream of the membrane to separate the effective components and impurities. The product that permeates through the membrane to the downstream side of the membrane is vaporized into a gaseous form under vacuum. The gaseous form enters the condenser under the action of the vacuum machine. The condensation temperature is -20℃. After cooling, it enters the first product tank in the form of pure liquor. The permeate side is stored in the raw material tank in liquid form. The liquid on the permeate side contains obvious off-flavors and high fatty acid esters.

[0047] (3) Chromatography column treatment: When the alcohol content of the osmotic liquid drops from 52° to 30°, the pervaporation membrane separation process is stopped. The osmotic liquid in the feed tank is pumped to the chromatography column for further adsorption. After adsorption is complete, it is collected in the second product tank. Column chromatography can remove off-flavors and higher fatty acid esters.

[0048] (4) Product mixing: Mix the liquor in the first product tank with the liquor in the first product tank to obtain a liquor product with impurities and high fatty acid esters removed.

[0049] Sensory evaluation of the baijiu product after removing off-flavors and higher fatty acid esters: The alcohol content showed no significant change, the aroma components were basically collected and preserved, the aroma was pure, there were no obvious off-flavors, and the body was clean. Physicochemical indicators: alcohol content 50° (under standard conditions at 20℃, the same below), total acid 1.69g / L, hexanoic acid 31.3mg / 100mL, acetic acid 117.4mg / 100mL, ethyl hexanoate 121.6mg / 100mL, ethyl lactate 217.9mg / 100mL, ethyl acetate 46.3mg / 100mL, ethyl butyrate 13.2mg / 100mL, ethyl palmitate 12.5mg / 100mL, ethyl oleate 8.4mg / 100mL, ethyl linoleate 5.9mg / 100mL, furfural 4.8mg / 100mL.

Claims

1. An apparatus for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor), characterized in that, The outlet of the raw material tank (1) is connected to the membrane separator (4) and the chromatography column (3) respectively through valves. The permeate side outlet of the membrane separator (4) is connected to the first product tank (6) through the condenser (5). The osmotic side outlet of the membrane separator (4) is connected to the raw material tank (1). The outlet of the chromatography column (3) is connected to the second product tank (7).

2. The apparatus for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor) according to claim 1, characterized in that, A heat exchanger (2) is also provided between the outlet of the raw material tank (1) and the membrane separator (4).

3. The apparatus for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor) according to claim 2, characterized in that, A pump is also provided between the outlet of the raw material tank (1) and the heat exchanger (2).

4. The apparatus for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor) according to claim 1, characterized in that, A pump is also provided between the outlet of the raw material tank (1) and the chromatography column (3).

5. The apparatus for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor) according to claim 1, characterized in that, The condenser (5) is connected to the vacuum pump (8).

6. The apparatus for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor) according to claim 1, characterized in that, The first product tank (6) is connected to the second product tank (7).

7. The apparatus for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor) according to claim 1, characterized in that, The membrane of the membrane separator (4) 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, polyvinylidene fluoride or inorganic ceramics; the active layer is composed of one or more of polydimethylsiloxane, hydrophobic nano titanium dioxide or polyvinyl alcohol.

8. The apparatus for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor) according to claim 1, characterized in that, The membrane separator (4) is either spiral wound or tubular.

9. The apparatus for removing off-flavors and higher fatty acid esters from baijiu (Chinese liquor) according to claim 1, characterized in that, A pump is also provided between the chromatography column (3) and the second product tank (7).

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