Method for catalyzing liquor aging

Abstract

The application provides a method for catalyzing liquor aging. The method comprises the following steps: S1: pressurizedly conveying newly-brewed liquor from a storage device to a self-made container, and laying 2-4 layers of sepiolite-chitosan composite membranes on the upper part of the self-made container; S2: continuously pressurizing the bottom of the self-made container, and allowing the newly-brewed liquor to pass through the sepiolite-chitosan composite membranes from bottom to top for catalytic aging for 30 min; and S3: collecting the liquor passing through the sepiolite-chitosan composite membranes from the upper part of the container, and obtaining the aged liquor. The method of pressurization combined with sepiolite-chitosan composite membranes is used to treat the newly-brewed liquor, the pressurization can promote the collision between liquor molecules and accelerate the occurrence of aging reaction; the sepiolite-chitosan composite membranes can filter the liquor, meanwhile, the sepiolite-chitosan composite membranes have the selective passing effect on esters, and the composite enzyme loaded thereon can accelerate the aging speed of the liquor.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of liquor processing, in particular to a method for catalyzing liquor aging. BACKGROUND

[0002] Liquor is a traditional liquor in China and is also a distillate liquor known worldwide, and is one of the seven major distillate liquors in the world. It has won the favor of the public with its long history, exquisite technology and unique style. The newly distilled liquor is generally pungent, not mellow, and not soft, and contains volatile substances such as hydrogen sulfide, mercaptans, sulfides, and a small amount of propylene aldehyde, butylene aldehyde, free ammonia and other impurity substances. These substances and other substances with similar boiling points constitute the main body of the new wine flavor. If these substances are reduced, the new wine flavor and impurity flavor will be less. Generally, through storage, a large amount of low-boiling-point odor substances are volatilized, reducing the impurities in the wine. Therefore, the newly distilled liquor is pungent, violent, and has strong irritating alcohol flavor, sediment flavor, mud flavor, bitter flavor and other strange flavors. It needs to be stored for a certain period of time to make the impurities disappear, the wine body soft and the flavor increase, and the wine body mellow and soft, and the taste more coordinated. This change is generally called aging, also known as aging.

[0003] In the aging process of liquor, the storage time is often long, which occupies a large amount of factory building and equipment, and accumulates a large amount of funds. The leakage loss of the liquor is also large, which seriously affects the turnover of production funds, increases the cost, and is not suitable for the requirements of modern economic development. Therefore, liquor factories have been looking forward to a new type of high-efficiency practical artificial aging technology, which can greatly increase the yield and improve the production efficiency on the basis of ensuring the same taste quality and style of liquor. Therefore, research on accelerating the aging of liquor and improving the efficiency has become an important research topic in the liquor industry. SUMMARY

[0004] The technical problem to be solved: In view of the above technical problems, the purpose of the present application is to provide a method for catalyzing liquor aging, which uses a method of pressurization combined with sepiolite-chitosan composite membrane to treat newly brewed liquor. The pressurization can promote the collision between liquor molecules and accelerate the occurrence of aging reaction. The sepiolite-chitosan composite membrane can filter the liquor, and at the same time, it has the function of selectively passing esters. The composite enzyme loaded thereon can accelerate the aging speed of the liquor.

[0005] Technical scheme: A method for catalyzing liquor aging, which uses a method of pressurization combined with sepiolite-chitosan composite membrane treatment. Further, the sepiolite-chitosan composite membrane is loaded with a composite enzyme; the pore size of the sepiolite-chitosan composite membrane is 0.01-0.1 μm, and the porosity is 75-80%.

[0006] Further, the complex enzyme is ethanol dehydrogenase, esterifying enzyme and inositol oxidase, and the mass ratio of the three is 1:10:4.

[0007] Further, the preparation method of the sepiolite-chitosan composite film is as follows:

[0008] (1) The sepiolite powder is soaked with 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 h, filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder;

[0009] (2) Take chitosan powder, add 2% acetic acid solution and stir to dissolve, add modified sepiolite powder, and continue to stir for 1 h as an electrospinning solution;

[0010] (3) Using an electrospinning device, the electrospinning solution is placed in a needle cylinder, and electrospinning is carried out to obtain an electrospinning film;

[0011] (4) The electrospinning film is taken off from the receiving plate and placed in a vacuum drying oven at 60°C for drying;

[0012] (5) Soak in a 5% hexanediamine solution for 1 h, and then wash with distilled water;

[0013] (6) Continue to soak in a 3% glutaraldehyde solution for 75 min, and then wash with distilled water to obtain a modified composite film;

[0014] (7) The complex enzyme is fully dissolved in a solution with a pH of 6.5-7.0 to obtain a complex enzyme solution, and the modified composite film is soaked in it for 8-10 h to obtain a sepiolite-chitosan composite film.

[0015] Further, the sepiolite particle size is 500-1000 nm.

[0016] Further, the chitosan Mw=200000, and the degree of deacetylation is 90%.

[0017] Further, the mass-volume ratio of chitosan, acetic acid solution and modified sepiolite powder is (2-4) g:100 mL:(10-18) g.

[0018] Further, the electrospinning conditions are as follows: electrospinning temperature is 25-28°C, electrospinning solution flow rate is 0.1-0.5 mL / h, electrospinning voltage is 18V, and distance from receiving plate is 15 cm.

[0019] Further, the above-mentioned method for catalyzing the aging of baijiu specifically includes the following steps:

[0020] S1: Pressurizedly conveying new baijiu from a storage to a self-made container, and laying 2-4 layers of sepiolite-chitosan composite film in the upper part of the self-made container;

[0021] S2: continuously pressurizing from the bottom of the container, and the newly brewed liquor is reverse osmosis through the sepiolite-chitosan composite membrane from bottom to top for aging for 30 minutes;

[0022] S3: collecting the liquor through the sepiolite-chitosan composite membrane from the upper part of the container, and obtaining the aged liquor.

[0023] Further, the pressurizing pressure in S2 is 15-66 MPa.

[0024] Beneficial effects:

[0025] 1. The method of the present application uses pressurization combined with a sepiolite-chitosan composite membrane to treat the newly brewed liquor. The pressurization can promote the collision between the liquor molecules and the extrusion collision between the liquor and the composite membrane, and accelerate the aging reaction. The porous structure of the sepiolite-chitosan composite membrane can filter the liquor. Meanwhile, the sepiolite-chitosan composite membrane has a selective passing effect on esters, and the composite enzyme loaded thereon can accelerate the aging speed of the liquor.

[0026] 2. The present application uses a bottom pressurization mode, and the newly brewed liquor is reverse osmosis through the sepiolite-chitosan composite membrane from bottom to top. On the one hand, the flow rate of the liquor can be controlled by the pressure, so as to control the contact time of the liquor with the sepiolite-chitosan composite membrane. On the other hand, the pressure strength is considered. According to the data, when the pressurization strength is greater than 66 MPa, the aging effect of the liquor does not increase obviously, and when the pressurization strength is greater than 80 MPa, the composite membrane will be damaged. Therefore, the pressurization strength of the present application is less than 66 MPa.

[0027] 3. The sepiolite-chitosan composite membrane in the present application has an adsorption effect on the four esters in the liquor. Since the affinity of ethyl lactate is stronger than that of ethyl hexanoate, the ethyl lactate can quickly displace the adsorbed ethyl hexanoate, so that the content of ethyl lactate is reduced, and finally a better ratio of ethyl lactate to ethyl hexanoate is obtained, so that the liquor has a better aroma and taste.

[0028] 4. In the present application, sepiolite is added to chitosan, which not only increases the adsorption effect, but also improves the acid resistance of the composite membrane. On the other hand, the -OH in sepiolite can form hydrogen bonds with the -OH and -NH2 in chitosan, thereby improving the mechanical properties.

[0029] 5. The composite enzyme is loaded and fixed on the composite membrane in the present application, so that it can be reused, which not only saves resources, but also saves the step of enzyme inactivation. BRIEF DESCRIPTION OF DRAWINGS

[0030] Figure 1The self-made container of the embodiment 12 of the present application is shown in the figure, wherein 1 is the self-made container; 2 is the sepiolite-chitosan composite membrane; 3 is the liquor collecting pipe; 4 is the newly-brewed liquor conveying pipe; 5 is the pressurizing pump; and 6 is the pressurizing pump pipe. DETAILED DESCRIPTION

[0031] The present application proposes a method for catalyzing liquor aging. In order to make the purpose, technical scheme and effects of the present application more clear and definite, the present application will be further described in detail in combination with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and not used to limit the present application.

[0032] The composite enzyme used in the following embodiments is ethanol dehydrogenase, esterifying enzyme and inositol oxidase, and the mass ratio of the three is 1:10:4.

[0033] Embodiment 1

[0034] The preparation method of the sepiolite-chitosan composite membrane is as follows:

[0035] (1) Sepiolite powder with a particle size of 500-1000 nm is soaked in 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 h, filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder;

[0036] (2) Chitosan powder with a chitosan Mw of 200000 and a degree of deacetylation of 90% is added with 2% acetic acid solution and stirred to dissolve, and the modified sepiolite powder is added and stirred for 1 h as an electrospinning solution; the mass-volume ratio of chitosan, acetic acid solution and modified sepiolite powder is 4 g:100 mL:10 g;

[0037] (3) An electrospinning device is used to place the electrospinning solution in a needle cylinder to perform electrospinning, and the electrospinning conditions are as follows: the electrospinning temperature is 25°C, the electrospinning solution flow rate is 0.3 mL / h, the electrospinning voltage is 18 V, and the distance from the receiving plate is 15 cm, to obtain an electrospinning membrane;

[0038] (4) The electrospinning membrane is taken off from the receiving plate and placed in a vacuum drying oven at 60°C for drying;

[0039] (5) It is immersed in a 5% hexanediamine solution for 1 h, and then taken out and washed with distilled water;

[0040] (6) It is further immersed in a 3% glutaraldehyde solution for 75 min, taken out and washed with distilled water to obtain a modified composite membrane;

[0041] (7) The composite enzyme is fully dissolved in a solution with a pH of 6.8 to obtain a composite enzyme solution with a concentration of 5 mg / mL, and the modified composite membrane is immersed therein for 9 h to obtain a sepiolite-chitosan composite membrane.

[0042] The pore size of the sepiolite-chitosan composite membrane is 0.01-0.1 μm.

[0043] Example 2

[0044] The preparation method of the sepiolite-chitosan composite membrane is as follows:

[0045] (1) Sepiolite powder with a particle size of 500-1000 nm is soaked in 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 h, suction filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder;

[0046] (2) Chitosan powder with a molecular weight of 200000 and a degree of deacetylation of 90% is added with 2% acetic acid solution and stirred to dissolve, and the modified sepiolite powder is added and continuously stirred for 1 h to obtain an electrospinning solution; the mass-volume ratio of chitosan, acetic acid solution, and modified sepiolite powder is 3 g:100 mL:10 g;

[0047] (3) The electrospinning solution is placed in a needle cylinder by using an electrospinning device, and electrospinning is performed under the following conditions: electrospinning temperature is 25°C, electrospinning solution flow rate is 0.3 mL / h, electrospinning voltage is 18 V, and the distance from the receiving plate is 15 cm, to obtain an electrospinning membrane;

[0048] (4) The electrospinning membrane is taken off from the receiving plate and placed in a vacuum drying oven at 60°C for drying;

[0049] (5) It is immersed in a hexanediamine solution with a concentration of 5% for 1 h, and then taken out and washed with distilled water;

[0050] (6) It is continuously immersed in a glutaraldehyde solution with a concentration of 3% for 75 min, taken out, and washed with distilled water to obtain a modified composite membrane;

[0051] (7) The composite enzyme is fully dissolved in a solution with a pH of 6.8 to obtain a composite enzyme solution with a concentration of 5 mg / mL, and the modified composite membrane is immersed therein for 9 h to obtain a sepiolite-chitosan composite membrane.

[0052] The pore size of the sepiolite-chitosan composite membrane is 0.01-0.1 μm.

[0053] Example 3

[0054] The preparation method of the sepiolite-chitosan composite membrane is as follows:

[0055] (1) Sepiolite powder with a particle size of 500-1000 nm is soaked in 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 h, suction filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder;

[0056] (2) Take chitosan powder, chitosan Mw = 200000, degree of deacetylation is 90%, add 2% acetic acid solution stirring to dissolve, add modified sepiolite powder, continue to stir 1h, as electrospinning liquid; The mass volume ratio of chitosan, acetic acid solution and modified sepiolite powder is 4g:100mL:15g;

[0057] (3) Using electrospinning device, the electrospinning liquid is placed in the needle cylinder, electrospinning is carried out, the electrospinning conditions are: electrospinning temperature is 25℃, electrospinning liquid flow rate is 0.3mL / h, electrospinning voltage is 18V, the distance from the receiving plate is 15cm, electrospinning membrane is obtained;

[0058] (4) The electrospinning membrane is taken off from the receiving plate and placed in a vacuum drying oven at 60℃ for drying;

[0059] (5) Immersed in 5% hexanediamine solution for 1h, take out and wash with distilled water;

[0060] (6) Continue to immerse in 3% glutaraldehyde solution for 75min, take out and wash with distilled water, obtain modified composite membrane;

[0061] (7) The composite enzyme is fully dissolved in a solution with pH 6.8 to obtain a composite enzyme solution with a concentration of 5mg / mL, and the modified composite membrane is immersed therein for 9h to obtain a sepiolite-chitosan composite membrane.

[0062] It is determined that the pore size of the sepiolite-chitosan composite membrane is 0.01-0.1μm.

[0063] Example 4

[0064] The preparation method of the sepiolite-chitosan composite membrane is as follows:

[0065] (1) The sepiolite powder with particle size of 500-1000nm is soaked with 1mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16h, filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder;

[0066] (2) Take chitosan powder, chitosan Mw = 200000, degree of deacetylation is 90%, add 2% acetic acid solution stirring to dissolve, add modified sepiolite powder, continue to stir 1h, as electrospinning liquid; The mass volume ratio of chitosan, acetic acid solution and modified sepiolite powder is 4g:100mL:18g;

[0067] (3) Using electrospinning device, the electrospinning liquid is placed in the needle cylinder, electrospinning is carried out, the electrospinning conditions are: electrospinning temperature is 25℃, electrospinning liquid flow rate is 0.3mL / h, electrospinning voltage is 18V, the distance from the receiving plate is 15cm, electrospinning membrane is obtained;

[0068] (4) The electrospun membrane was taken off from the receiving plate and put into a vacuum drying oven at 60°C for drying;

[0069] (5) The membrane was immersed in a 5% hexanediamine solution for 1 h and then washed with distilled water;

[0070] (6) The membrane was further immersed in a 3% glutaraldehyde solution for 75 min and then washed with distilled water to obtain a modified composite membrane;

[0071] (7) The composite enzyme was dissolved in a solution with a pH of 6.8 to obtain a composite enzyme solution with a concentration of 5 mg / mL, and the modified composite membrane was immersed in the solution for 9 h to obtain a sepiolite-chitosan composite membrane.

[0072] It was determined that the sepiolite-chitosan composite membrane had a pore size of 0.01-0.1 μm.

[0073] Example 5

[0074] The sepiolite-chitosan composite membrane was prepared as follows:

[0075] (1) Sepiolite powder with a particle size of 500-1000 nm was soaked in 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 h, filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder;

[0076] (2) Chitosan powder with a Mw of 200000 and a degree of deacetylation of 90% was added to a 2% acetic acid solution and stirred to dissolve, and the modified sepiolite powder was added and stirred for 1 h to obtain an electrospinning solution; the mass-volume ratio of chitosan, acetic acid solution, and modified sepiolite powder was 2 g:100 mL:10 g;

[0077] (3) An electrospinning device was used, and the electrospinning solution was placed in a needle cylinder to perform electrospinning; the electrospinning temperature was 25°C, the electrospinning solution flow rate was 0.3 mL / h, the electrospinning voltage was 18 V, the distance from the receiving plate was 15 cm, and an electrospun membrane was obtained;

[0078] (4) The electrospun membrane was taken off from the receiving plate and put into a vacuum drying oven at 60°C for drying;

[0079] (5) The membrane was immersed in a 5% hexanediamine solution for 1 h and then washed with distilled water;

[0080] (6) The membrane was further immersed in a 3% glutaraldehyde solution for 75 min and then washed with distilled water to obtain a modified composite membrane;

[0081] (7) The complex enzyme is dissolved in a solution with pH of 6.8 to obtain a complex enzyme solution with a concentration of 5 mg / mL, and the modified composite membrane is immersed in the solution for 9 h to obtain the sepiolite-chitosan composite membrane.

[0082] The pore size of the sepiolite-chitosan composite membrane is 0.01-0.1 μm.

[0083] Example 6

[0084] The preparation method of the sepiolite-chitosan composite membrane is as follows:

[0085] (1) Sepiolite powder with a particle size of 500-1000 nm is soaked in 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 h, filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder;

[0086] (2) Chitosan powder with a molecular weight of 200000 and a degree of deacetylation of 90% is added with 2% acetic acid solution and stirred to dissolve, and the modified sepiolite powder is added and stirred for 1 h as an electrospinning solution; the mass-volume ratio of chitosan, acetic acid solution and modified sepiolite powder is 3 g:100 mL:18 g;

[0087] (3) An electrospinning device is used to place the electrospinning solution in a needle cylinder to perform electrospinning, and the electrospinning conditions are as follows: the electrospinning temperature is 25°C, the electrospinning solution flow rate is 0.3 mL / h, the electrospinning voltage is 18 V, and the distance from the receiving plate is 15 cm to obtain an electrospinning membrane;

[0088] (4) The electrospinning membrane is taken off from the receiving plate and placed in a vacuum drying oven at 60°C for drying;

[0089] (5) The membrane is immersed in a hexanediamine solution with a concentration of 5% for 1 h, and then taken out and washed with distilled water;

[0090] (6) The membrane is continuously immersed in a glutaraldehyde solution with a concentration of 3% for 75 min, and then taken out and washed with distilled water to obtain a modified composite membrane;

[0091] (7) The complex enzyme is dissolved in a solution with pH of 6.8 to obtain a complex enzyme solution with a concentration of 5 mg / mL, and the modified composite membrane is immersed in the solution for 9 h to obtain the sepiolite-chitosan composite membrane.

[0092] The pore size of the sepiolite-chitosan composite membrane is 0.01-0.1 μm.

[0093] Example 7

[0094] The preparation method of the sepiolite-chitosan composite membrane is as follows:

[0095] (1) Sepiolite powder with particle size of 500-1000 nm was soaked with 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 h, filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder;

[0096] (2) Chitosan powder with Mw of 200000 and deacetylation degree of 90% was added into 2% acetic acid solution and stirred to dissolve, and the modified sepiolite powder was added and stirred for 1 h to obtain an electrospinning solution; the mass-volume ratio of chitosan, acetic acid solution and modified sepiolite powder was 2 g:100 mL:15 g;

[0097] (3) The electrospinning solution was placed in a needle cylinder by using an electrospinning device, and electrospinning was performed at a temperature of 25°C, a flow rate of 0.3 mL / h, a voltage of 18 V, and a distance of 15 cm from the receiving plate to obtain an electrospinning membrane;

[0098] (4) The electrospinning membrane was taken off from the receiving plate and placed in a vacuum drying oven at 60°C for drying;

[0099] (5) The membrane was immersed in a 5% hexanediamine solution for 1 h, and then washed with distilled water;

[0100] (6) The membrane was further immersed in a 3% glutaraldehyde solution for 75 min, and then washed with distilled water to obtain a modified composite membrane;

[0101] (7) The composite enzyme was fully dissolved in a solution with pH of 6.8 to obtain a composite enzyme solution with a concentration of 5 mg / mL, and the modified composite membrane was immersed in the solution for 9 h to obtain a sepiolite-chitosan composite membrane.

[0102] It was determined that the pore size of the sepiolite-chitosan composite membrane was 0.01-0.1 μm.

[0103] Example 8

[0104] The preparation method of the sepiolite-chitosan composite membrane is as follows:

[0105] (1) Sepiolite powder with particle size of 500-1000 nm was soaked with 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 h, filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder;

[0106] (2) Chitosan powder with Mw of 200000 and deacetylation degree of 90% was added into 2% acetic acid solution and stirred to dissolve, and the modified sepiolite powder was added and stirred for 1 h to obtain an electrospinning solution; the mass-volume ratio of chitosan, acetic acid solution and modified sepiolite powder was 2 g:100 mL:18 g;

[0107] (3) The electrospinning solution is placed in a needle cylinder by using an electrospinning device to perform electrospinning, and the electrospinning conditions are as follows: the electrospinning temperature is 25°C, the electrospinning solution flow rate is 0.3 mL / h, the electrospinning voltage is 18 V, the distance from the receiving plate is 15 cm, and an electrospinning film is obtained;

[0108] (4) The electrospinning film is taken off from the receiving plate and placed in a vacuum drying box at 60°C for drying;

[0109] (5) The electrospinning film is immersed in a 5% hexanediamine solution for 1 h, taken out and washed with distilled water;

[0110] (6) The electrospinning film is continuously immersed in a 3% glutaraldehyde solution for 75 min, taken out and washed with distilled water, and a modified composite film is obtained;

[0111] (7) The composite enzyme is fully dissolved in a solution with a pH of 6.8 to obtain a composite enzyme solution with a concentration of 5 mg / mL, and the modified composite film is immersed therein for 9 h to obtain a sepiolite-chitosan composite film.

[0112] It is determined that the pore size of the sepiolite-chitosan composite film is 0.01-0.1 μm.

[0113] Example 9

[0114] The preparation method of the sepiolite-chitosan composite film is as follows:

[0115] (1) Sepiolite powder with a particle size of 500-1000 nm is soaked in 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 h, filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder;

[0116] (2) Chitosan powder with a chitosan Mw of 200000 and a degree of deacetylation of 90% is added with 2% acetic acid solution to be stirred and dissolved, and the modified sepiolite powder is added to continue stirring for 1 h to serve as an electrospinning solution; the mass-volume ratio of chitosan, acetic acid solution and modified sepiolite powder is 3 g:100 mL:18 g;

[0117] (3) The electrospinning solution is placed in a needle cylinder by using an electrospinning device to perform electrospinning, and the electrospinning conditions are as follows: the electrospinning temperature is 25°C, the electrospinning solution flow rate is 0.1 mL / h, the electrospinning voltage is 18 V, the distance from the receiving plate is 15 cm, and an electrospinning film is obtained;

[0118] (4) The electrospinning film is taken off from the receiving plate and placed in a vacuum drying box at 60°C for drying;

[0119] (5) The electrospinning film is immersed in a 5% hexanediamine solution for 1 h, taken out and washed with distilled water;

[0120] (6) continue to immerse in 3% glutaraldehyde solution for 75 min, take out and wash with distilled water to obtain the modified composite membrane;

[0121] (7) dissolve the composite enzyme in a solution with pH of 6.8 to obtain a composite enzyme solution with a concentration of 5 mg / mL, immerse the modified composite membrane therein for 9 h to obtain the sepiolite-chitosan composite membrane.

[0122] It is determined that the pore size of the sepiolite-chitosan composite membrane is 0.01-0.1 μm.

[0123] Example 10

[0124] The preparation method of the sepiolite-chitosan composite membrane is as follows:

[0125] (1) immerse sepiolite powder with a particle size of 500-1000 nm in 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 h, filter, wash with distilled water until neutral, and dry to obtain modified sepiolite powder;

[0126] (2) take chitosan powder with a chitosan Mw of 200000 and a degree of deacetylation of 90%, add 2% acetic acid solution to stir and dissolve, and add the modified sepiolite powder to continue stirring for 1 h as an electrospinning solution; the mass-volume ratio of chitosan, acetic acid solution and modified sepiolite powder is 3 g:100 mL:18 g;

[0127] (3) use an electrospinning device to place the electrospinning solution in a needle cylinder to perform electrospinning, and the electrospinning conditions are as follows: the electrospinning temperature is 25°C, the electrospinning solution flow rate is 0.5 mL / h, the electrospinning voltage is 18 V, and the distance from the receiving plate is 15 cm to obtain an electrospinning membrane;

[0128] (4) take the electrospinning membrane from the receiving plate and place it in a vacuum drying oven at 60°C for drying;

[0129] (5) immerse in a 5% hexanediamine solution for 1 h, take out and wash with distilled water;

[0130] (6) continue to immerse in a 3% glutaraldehyde solution for 75 min, take out and wash with distilled water to obtain the modified composite membrane;

[0131] (7) dissolve the composite enzyme in a solution with pH of 6.8 to obtain a composite enzyme solution with a concentration of 5 mg / mL, immerse the modified composite membrane therein for 9 h to obtain the sepiolite-chitosan composite membrane.

[0132] It is determined that the pore size of the sepiolite-chitosan composite membrane is 0.01-0.1 μm.

[0133] Comparative Example 1

[0134] The difference between this embodiment and embodiment 6 is that sepiolite is not contained, and the preparation method is as follows:

[0135] The preparation method of the chitosan membrane is as follows:

[0136] (1) chitosan powder with Mw=200000 and deacetylation degree of 90% is taken, 2% acetic acid solution is added for stirring and dissolving, and the chitosan and acetic acid solution are used as the electrospinning solution; the mass-volume ratio of the chitosan and acetic acid solution is 3g:100mL;

[0137] (2) the electrospinning solution is placed in a needle cylinder by using an electrospinning device, electrospinning is performed, the electrospinning temperature is 25°C, the electrospinning solution flow rate is 0.3mL / h, the electrospinning voltage is 18V, the distance from the receiving plate is 15cm, and an electrospinning membrane is obtained;

[0138] (3) the electrospinning membrane is taken off from the receiving plate and placed in a vacuum drying box at 60°C for drying;

[0139] (4) the membrane is immersed in a 5% hexanediamine solution for 1h, taken out and washed with distilled water;

[0140] (5) the membrane is continuously immersed in a 3% glutaraldehyde solution for 75min, taken out and washed with distilled water, and a modified composite membrane is obtained;

[0141] (6) the composite enzyme is fully dissolved in a solution with pH of 6.8 to obtain a composite enzyme solution with concentration of 5mg / mL, and the modified composite membrane is immersed in the solution for 9h, and a sepiolite-chitosan composite membrane is obtained.

[0142] It is determined that the pore size of the chitosan membrane is 0.01-0.1μm.

[0143] Some physical and chemical properties of the sepiolite-chitosan composite membrane are determined, including porosity, acid resistance and compressive strength, and the results are shown in the following table:

[0144] Table 1 Partial properties of sepiolite-chitosan composite membrane

[0145] Porosity (%) Acid resistance (pH) Compressive strength (MPa) Example 1 80.0 2.6 83.6 Example 2 79.4 2.6 84.7 Example 3 78.8 2.5 85.4 Example 4 78.1 2.5 86.9 Example 5 77.3 2.5 88.3 Example 6 76.5 2.5 89.1 Example 7 75.6 2.4 89.4 Example 8 75.1 2.4 89.2 Example 9 77.1 2.5 88.9 Example 10 76.0 2.5 88.6 Comparative Example 1 88.2 2.8 67.5

[0146] Some technical indexes of the composite enzyme after loading the composite enzyme are determined:

[0147] Determination of enzyme loading: the enzyme loading is determined by determining the difference in protein concentration of the composite enzyme solution before and after immobilization;

[0148] The results are shown in Table 2 as follows:

[0149] Table 2

[0150]

[0151]

[0152] After comprehensive comparison of the physicochemical properties and enzyme loading performance of the sepiolite-chitosan composite membrane, the sepiolite-chitosan composite membrane prepared in Example 6 was used in the subsequent test.

[0153] The storage time of the new-brewed liquor used in the following examples was January 10, 2024, and the liquor degree was 65 degrees.

[0154] Example 11

[0155] A method for catalyzing liquor aging, characterized in that it specifically comprises the following steps:

[0156] S1: The new-brewed liquor is pressurized and transported from the storage device to the self-made container, and 3 layers of sepiolite-chitosan composite membranes are laid in the upper part of the self-made container;

[0157] S2: The bottom of the self-made container is continuously pressurized, the pressurization pressure is 15 MPa, and the new-brewed liquor is reverse osmosis through the sepiolite-chitosan composite membrane from bottom to top for catalytic aging for 30 min;

[0158] S3: The liquor passing through the sepiolite-chitosan composite membrane is collected from the upper part of the container, and the aged liquor is obtained.

[0159] Example 12

[0160] A method for catalyzing liquor aging, characterized in that it specifically comprises the following steps:

[0161] S1: The new-brewed liquor is pressurized and transported from the storage device to the self-made container, and 3 layers of sepiolite-chitosan composite membranes are laid in the upper part of the self-made container;

[0162] S2: The bottom of the self-made container is continuously pressurized, the pressurization pressure is 40 MPa, and the new-brewed liquor is reverse osmosis through the sepiolite-chitosan composite membrane from bottom to top for catalytic aging for 30 min;

[0163] S3: The liquor passing through the sepiolite-chitosan composite membrane is collected from the upper part of the container, and the aged liquor is obtained.

[0164] Example 13

[0165] A method for catalyzing liquor aging, characterized in that it specifically comprises the following steps:

[0166] S1: The new-brewed liquor is pressurized and transported from the storage device to the self-made container, and 3 layers of sepiolite-chitosan composite membranes are laid in the upper part of the self-made container;

[0167] S2: continuously pressurize the bottom of the self-made container, the pressurization pressure is 66 MPa, and the newly brewed liquor is subjected to reverse osmosis through the sepiolite-chitosan composite membrane from bottom to top for liquor aging for 30 min;

[0168] S3: the liquor subjected to the sepiolite-chitosan composite membrane is collected from the upper part of the container, and the aged liquor is obtained.

[0169] Example 14

[0170] A method for catalyzing liquor aging, specifically comprising the following steps:

[0171] S1: the newly brewed liquor is pressurized and transported from the storage to the self-made container, and 2 layers of sepiolite-chitosan composite membranes are laid in the upper part of the self-made container;

[0172] S2: continuously pressurize the bottom of the self-made container, the pressurization pressure is 66 MPa, and the newly brewed liquor is subjected to reverse osmosis through the sepiolite-chitosan composite membrane from bottom to top for liquor aging for 30 min;

[0173] S3: the liquor subjected to the sepiolite-chitosan composite membrane is collected from the upper part of the container, and the aged liquor is obtained.

[0174] Example 15

[0175] A method for catalyzing liquor aging, specifically comprising the following steps:

[0176] S1: the newly brewed liquor is pressurized and transported from the storage to the self-made container, and 4 layers of sepiolite-chitosan composite membranes are laid in the upper part of the self-made container;

[0177] S2: continuously pressurize the bottom of the self-made container, the pressurization pressure is 66 MPa, and the newly brewed liquor is subjected to reverse osmosis through the sepiolite-chitosan composite membrane from bottom to top for liquor aging for 30 min;

[0178] S3: the liquor subjected to the sepiolite-chitosan composite membrane is collected from the upper part of the container, and the aged liquor is obtained.

[0179] Comparative Example 2

[0180] The difference between this comparative example and Example 13 is that the pressurization pressure is 80 MPa, and the specific process is as follows:

[0181] A method for catalyzing liquor aging, specifically comprising the following steps:

[0182] S1: the newly brewed liquor is pressurized and transported from the storage to the self-made container, and 3 layers of sepiolite-chitosan composite membranes are laid in the upper part of the self-made container;

[0183] S2: continuously pressurize from the bottom of the self-made container, the pressurizing pressure is 80 MPa, the newly brewed liquor is reverse osmosis through the sepiolite-chitosan composite membrane from bottom to top for 30 min of liquor aging;

[0184] S3: collect the liquor through the sepiolite-chitosan composite membrane from the upper part of the container, and obtain the aged liquor.

[0185] Comparative Example 3

[0186] The difference between the present comparative example and Example 13 is that no sepiolite-chitosan composite membrane is laid, and the holding time in the self-made container is consistent with that of Example 13, which is as follows:

[0187] A method for catalyzing liquor aging, which is characterized by comprising the following steps:

[0188] S1: pressurize the newly brewed liquor from the storage to the self-made container;

[0189] S2: continuously pressurize from the bottom of the self-made container, the pressurizing pressure is 66 MPa, and the pressurizing is maintained for 30 min;

[0190] S3: collect the liquor from the upper part of the container, and obtain the aged liquor.

[0191] Comparative Example 4

[0192] The difference between the present comparative example and Example 13 is that no additional pressure is applied, and only the sepiolite-chitosan composite membrane is penetrated by the delivery pressure, which is as follows:

[0193] A method for catalyzing liquor aging, which is characterized by comprising the following steps:

[0194] S1: pressurize the newly brewed liquor from the storage to the self-made container, and lay 3 layers of sepiolite-chitosan composite membrane on the upper part of the self-made container;

[0195] S2: continuously deliver the newly brewed liquor, and the newly brewed liquor is reverse osmosis through the sepiolite-chitosan composite membrane from bottom to top for 30 min of liquor aging; S3: collect the liquor through the sepiolite-chitosan composite membrane from the upper part of the container, and obtain the aged liquor.

[0196] Determination of total acid: organic acid is both a flavoring substance and a taste substance in liquor, and is a precursor of synthetic ester. The acid in the liquor body is related to the aftertaste of the liquor, and insufficient acid results in short liquor taste;

[0197] Determination of total ester: ester compounds are the main body of liquor flavor, and exhibit a certain bitter taste at a certain concentration.

[0198] Determination of fusel oil: n-propanol, isobutyl alcohol and isoamyl alcohol in Baijiu constitute fusel oil, n-propanol and isobutyl alcohol have bitter taste and affect the taste of Baijiu; too much fusel oil in Baijiu will make the Baijiu have strong irritation and cause headache after drinking.

[0199] Determination of clarity: after Baijiu is frozen for more than 12 hours, it is naturally restored to 0℃, and the turbidity of the Baijiu sample is observed by visual method.

[0200] Table 3: determination of physicochemical indexes of Baijiu

[0201] Total acid (g / L) Total ester (g / L) Fusel oil (g / L) Clarity Initial 0.58 3.06 0.84 Hazy, loss of brilliance Example 11 0.71 2.73 0.38 Clear and transparent Example 12 0.72 2.75 0.36 Clear and transparent Example 13 0.72 2.78 0.33 Clear and transparent Example 14 0.70 2.70 0.40 Clear and transparent Example 15 0.73 2.81 0.31 Clear and transparent Comparative Example 2 0.74 2.79 0.50 Clear and transparent Comparative Example 3 0.56 2.98 0.81 With flocculent suspension Comparative Example 4 0.67 2.84 0.53 Clear and transparent Aged naturally for 3 years 0.75 2.78 0.30 Clear and transparent

[0202] As can be seen from Table 3, the total acid content of Baijiu aged by the application increases, the total ester content decreases, which is consistent with the traditional aging trend of Baijiu, mainly because the complex enzyme and the pressurization accelerate the conversion of alcohol substances in Baijiu into acid substances, and promote the hydrolysis of ester substances in Baijiu, so the total acid content of Baijiu increases, the total ester content decreases, and the alcohol content decreases. From the data, after the pressurization intensity is 66 MPa, the aging effect of Baijiu does not increase significantly, and when the pressurization intensity reaches 80 MPa, the composite membrane will be damaged, so the application selects 66 MPa or less. n-propanol, isobutyl alcohol and isoamyl alcohol in Baijiu constitute fusel oil, n-propanol and isobutyl alcohol have bitter taste and affect the taste of Baijiu; too much fusel oil in Baijiu will make the Baijiu have strong irritation, and after the treatment of the application, the content of fusel oil decreases significantly.

[0203] The content of main taste-producing ester, acid and alcohol substances in Baijiu was determined, and the results are shown in Table 4 below:

[0204] Table 4: content of main taste-producing ester, acid and alcohol substances

[0205]

[0206] As shown in Table 4, the contents of ethyl hexanoate, ethyl acetate, and ethyl butyrate in the baijiu aged by the catalytic aging process of this invention increased, while the content of ethyl lactate decreased. This is mainly because the sepiolite-chitosan composite membrane used has an adsorption effect on these four esters. Since ethyl lactate has a stronger affinity than ethyl hexanoate, it quickly displaces the adsorbed ethyl hexanoate, thus reducing the ethyl lactate content. Ultimately, the ratio of ethyl lactate to ethyl hexanoate in Example 13 was 0.73, and in Example 15 it was 0.70, both falling within the optimal ratio range of 0.4-0.8. The initial ratio of 0.83 resulted in a poorer taste and aroma. The significant increase in butyric acid and hexanoic acid content is mainly related to the hydrolysis of ethyl butyrate and ethyl hexanoate; while the lactic acid content changed less, mainly due to the adsorption of ethyl lactate, reducing its content and decreasing the amount of hydrolysate raw materials. Among them, valeric acid, heptanoic acid and β-phenylethanol are also the main aroma substances in baijiu. Although their content is relatively low in the overall content of baijiu, their aroma effect is more obvious. After being processed by the method of this invention, their content has also increased significantly.

[0207] Sensory evaluation was conducted on the processed liquor. The evaluation team randomly selected 10 participants from the research institute to conduct sensory evaluations, and the average value was taken. The results are shown in Table 5.

[0208] Table 5 Sensory Evaluation of Baijiu

[0209] Colour (10) Aroma (25) Taste (50) Style (15) Total score (100) Initial 8 18 29 14 69 Example 13 10 24 45 15 94 Comparative Example 2 10 23 45 15 93 Comparative Example 3 9 20 33 14 76 Comparative Example 4 10 21 44 15 90 Aged naturally for 3 years 10 23 47 15 95

[0210] As can be seen from Table 5 above, the color, aroma and taste of the baijiu aged by the catalytic aging of this invention are basically the same as those of baijiu aged naturally for 3 years.

Claims

1. A method for catalyzing aging of Baijiu, characterized in that, A method combining pressure treatment with sepiolite-chitosan composite membrane treatment is adopted; the sepiolite-chitosan composite membrane is loaded with a composite enzyme; the pore size of the sepiolite-chitosan composite membrane is 0.01-0.1μm, and the porosity is 75-80%. The complex enzyme consists of alcohol dehydrogenase, esterase and inositol oxidase, with a mass ratio of 1:10:

4. The method for preparing the sepiolite-chitosan composite membrane is as follows: (1) The sepiolite powder was soaked in 1 mol / L hydrochloric acid at a solid-liquid ratio of 1:10 for 16 hours, filtered, washed with distilled water until neutral, and dried to obtain modified sepiolite powder. (2) Take chitosan powder, add 2% acetic acid solution and stir to dissolve, add modified sepiolite powder, and continue stirring for 1 hour to make electrospinning solution; (3) Using an electrospinning device, the electrospinning solution is placed in a syringe for electrospinning to obtain an electrospinning membrane; (4) Remove the electrospun film from the receiving plate and place it in a vacuum drying oven at 60°C to dry; (5) Immerse in a 5% hexamethylenediamine solution for 1 hour, then remove and wash with distilled water; (6) Continue to immerse in a 3% glutaraldehyde solution for 75 minutes, remove and wash with distilled water to obtain a modified composite membrane; (7) Dissolve the composite enzyme fully in a solution with a pH of 6.5-7.0 to obtain a composite enzyme solution. Immerse the modified composite membrane in the solution for 8-10 hours to obtain a sepiolite-chitosan composite membrane. The mass-to-volume ratio of chitosan, acetic acid solution and modified sepiolite powder is (2-4)g:100mL:(10-18)g.

2. The method for catalyzing the aging of Baijiu according to claim 1, characterized in that, The sepiolite powder has a particle size of 500-1000 nm.

3. The method for catalyzing the aging of Baijiu according to claim 1, characterized in that, The chitosan has an Mw of 200,000 and a degree of deacetylation of 90%.

4. The method for catalyzing the aging of Baijiu according to claim 1, characterized in that, The electrospinning conditions are as follows: electrospinning temperature is 25-28℃, electrospinning solution flow rate is 0.1-0.5mL / h, electrospinning voltage is 18V, and the distance between the electrospinning solution and the receiving plate is 15cm.

5. The method for catalyzing the aging of Baijiu according to claim 1, characterized in that, Specifically, the following steps are included: S1: Pressurize and transport the newly brewed liquor from the storage container to the self-made container, the upper part of which is lined with 2-4 layers of sepiolite-chitosan composite film; S2: The bottom of the homemade container is continuously pressurized, and the newly brewed baijiu is aged for 30 minutes by reverse osmosis from bottom to top through the sepiolite-chitosan composite membrane; S3: Collect the baijiu that has passed through the sepiolite-chitosan composite membrane from the top of the container to obtain the aged baijiu.

6. The method for catalyzing the aging of Baijiu according to claim 5, characterized in that, The pressurization pressure in S2 is 15-66 MPa.

Images