Method for regulating and controlling stale fragrance and stale taste in white spirit

Abstract

The invention discloses a method for regulating and controlling stale fragrance and stale flavor in baijiu, and belongs to the technical field of baijiu aging. A catalytic promoter and argil are uniformly mixed, water is added for forming, the catalytic promoter is obtained, the catalytic promoter is composed of two components, the first component is two or three of Fe2O3 (at) SiO2-Al2O3, CuO (at) SiO2-Al2O3 and Pt-Pb (at) SiO2-Al2O3, and the second component is one or more of Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, Al2O3, the second component is one or more of Fe2O3 (ferric oxide), SiO2 (silicon dioxide), Al2O3 (aluminum oxide) and CuO (copper oxide); the mass ratio of the first component to the second component is 2: (0.1-6); and then adding a catalytic promoter in the process of storing and aging the white spirit, and storing and aging the white spirit. The method provided by the invention can regulate and control the stale aroma and stale flavor in the white spirit, is simple to operate, and does not introduce impurities.

Description

Technical Field

[0001] The invention relates to a method for regulating and controlling the aged aroma and flavor in liquor, and belongs to the technical field of liquor aging. Background Art

[0002] The aged aroma and taste of liquor are the unique flavor and aroma that gradually develops during the long storage process. These changes are mainly due to physical and chemical changes, including oxidation, reduction, acetalization, esterification, etc., which lead to changes in the content and proportion of substances such as acids, aldehydes, alcohols, and esters in the liquor, thereby improving the sensory flavor of the liquor and promoting the improvement of the liquor quality.

[0003] Conventional methods for regulating the aroma and flavor of liquor include natural aging, physical aging, chemical aging and biological aging. Among them, natural aging (Yang Guohua, Qiu Shuyi, Huang Yongguang. Research on aroma-producing microorganisms in the production of Maotai-flavor liquor [J]. China Brewing, 2011(4): 24-27.) is to allow liquor to mature naturally in pottery jars or wine seas under suitable environmental conditions, such as temperature, humidity, light, etc., but the aging cycle is long, occupies a lot of money and space, and is greatly affected by environmental factors; physical aging (Tang Liyun, Zhu Mengjiang, Wang Yubin. Modernization and new technology research of traditional liquor production [J]. China Food Industry, 2022(5): 124-127.) is to use physical means such as microwaves, ultrasound, high-voltage electric fields to accelerate chemical reactions in liquor to shorten the aging time, but it may affect the flavor of liquor. The chemical aging method (Zhen Pan. Study on the variation of trace components in the process of storage in Fenjiu ceramic jars [J]. Winemaking, 2015, 42(3): 51-53.) is to promote esterification and oxidation reactions in liquor by adding chemical substances such as catalysts and oxidants to improve the aroma and flavor of liquor, but it may introduce impurities and affect the safety and taste of liquor. The biological aging method (Wu Huachang, You Yaohui, Lu Zhongming, et al. Preliminary study on the application of lipase in liquor aging [J]. China Brewing, 2011(3): 75-77.) is to use microbial fermentation or enzyme catalysis to simulate the biochemical reactions in the natural aging process to improve the aroma and flavor of liquor, but it is technically difficult and has high requirements on the selection of microbial strains and enzymes. In addition, the aging effect may be limited by the activity of microorganisms.

[0004] Therefore, there is an urgent need for an efficient, simple and convenient method for regulating the aged aroma and flavor of liquor.

[0005] Based on this demand, the applicant adopted the mode of industry-university-research cooperation and commissioned relevant universities and research institutes to carry out research and development, making full use of the scientific research resources and innovation capabilities of universities and research institutes, and fully combining the actual needs of the market to achieve rapid transformation from theoretical research to product development. Summary of the invention

[0006] [Technical issues]

[0007] Conventional methods of regulating the aged aroma and flavor of liquor are time-consuming, costly, and will affect the flavor of the liquor.

[0008] [Technical solution]

[0009] In order to solve the above problems, the present invention mixes the catalyst promoter and clay evenly, adds water to form, and obtains the catalyst promoter, wherein the catalyst promoter is composed of two components, the first component is Fe 2 O 3 @SiO 2 -Al 2 O 3 、CuO@SiO 2 -Al 2 O 3 、Pt-Pb@SiO 2 -Al 2 O 3 Two or three of the following: 2 O 3 、SiO 2 、Al 2 O 3 , CuO; the mass ratio of the first component to the second component is 2:0.1-6; then, during the storage of aged liquor, a catalytic aid is added, and the liquor is stored for aging. The method of the invention can regulate the aged aroma and flavor of liquor, and is simple to operate without introducing impurities.

[0010] The first object of the present invention is to provide a method for regulating the aged aroma and flavor of liquor, comprising the following steps:

[0011] (1) mixing the catalyst promoter and clay evenly, adding water to mix and forming, and firing to obtain the catalyst promoter;

[0012] The catalyst is composed of two components. The first component is Fe 2 O 3 @SiO 2 -Al 2 O 3 、CuO@SiO 2 -Al 2 O 3 、Pt-Pb@SiO 2 -Al 2 O 3 Two or three of the following: 2 O 3 、SiO 2 、Al 2 O 3, CuO; the mass ratio of the first component to the second component is 2:0.1-6;

[0013] (2) A catalytic aid is added during the storage of aged liquor, and the amount of the catalytic aid added is 0.1-15% of the liquor mass, but not 0.

[0014] In one embodiment of the present invention, the particle size of the catalyst promoter and clay in step (1) is 0.01-1 mm.

[0015] In one embodiment of the present invention, in step (1), the mass ratio of the catalyst promoter, clay and water is 1-30:100:10-30.

[0016] In one embodiment of the present invention, the first component of the catalyst promoter in step (1) contains Fe 2 O 3 @SiO 2 -Al 2 O 3 、CuO@SiO 2 -Al 2 O 3 、Pt-Pb@SiO 2 -Al 2 O 3 The mass ratio of Fe in the second component is 1-3:1-3:1-3; 2 O 3 、SiO 2 、Al 2 O 3 , CuO is in a mass ratio of 0.5-1.5:1-6:1-6:0.5-1.5.

[0017] In one embodiment of the present invention, the first component of the catalyst promoter in step (1) contains Fe 2 O 3 @SiO 2 -Al 2 O 3 、CuO@SiO 2 -Al 2 O 3 The mass ratio of Fe in the second component is 1-3:1-3; 2 O 3 、Al 2 O 3 The mass ratio is 0.5-1.5:1-6.

[0018] In one embodiment of the present invention, the first component of the catalyst promoter in step (1) is CuO@SiO 2 -Al 2 O 3、Pt-Pb@SiO 2 -Al 2 O 3 The mass ratio of Fe in the second component is 1-3:1-3; 2 O 3 、SiO 2 The mass ratio is 0.5-1.5:1-6.

[0019] In one embodiment of the present invention, the first component of the catalyst promoter in step (1) contains Fe 2 O 3 @SiO 2 -Al 2 O 3 、Pt-Pb@SiO 2 -Al 2 O 3 The mass ratio of SiO in the second component is 1-3:1-3; 2 、Al 2 O 3 , and CuO are in a mass ratio of 1-6:1-6:0.5-1.5.

[0020] In one embodiment of the present invention, the first component of the catalyst promoter in step (1) contains Fe 2 O 3 @SiO 2 -Al 2 O 3 、CuO@SiO 2 -Al 2 O 3 The mass ratio of SiO in the second component is 1-3:1-3; 2 、Al 2 O 3 , and CuO are in a mass ratio of 1-6:1-6:0.5-1.5.

[0021] In one embodiment of the present invention, the first component of the catalyst promoter in step (1) is Pt-Pb@SiO 2 -Al 2 O 3 、CuO@SiO 2 -Al 2 O 3 The mass ratio of SiO in the second component is 1-3:1-3; 2 、Al 2 O 3 , and CuO are in a mass ratio of 1-6:1-6:0.5-1.5.

[0022] In one embodiment of the present invention, the first component of the catalyst promoter in step (1) is Pt-Pb@SiO 2-Al 2 O 3 、CuO@SiO 2 -Al 2 O 3 The mass ratio of Fe in the second component is 1-3:1-3; 2 O 3 、SiO 2 、Al 2 O 3 , CuO is in a mass ratio of 0.5-1.5:1-6:1-6:0.5-1.5.

[0023] In one embodiment of the present invention, the first component of the catalyst promoter in step (1) contains Fe 2 O 3 @SiO 2 -Al 2 O 3 、CuO@SiO 2 -Al 2 O 3 The mass ratio of Fe in the second component is 1-3:1-3; 2 O 3 、SiO 2 、Al 2 O 3 , CuO is in a mass ratio of 0.5-1.5:1-6:1-6:0.5-1.5.

[0024] In one embodiment of the present invention, the forming in step (1) is performed by using a mold, and the shape can be a sheet, a sphere, a regular hexahedron, a cylinder, a cone, a honeycomb, etc.

[0025] In one embodiment of the present invention, the firing in step (1) is performed at 800-1400° C. for 5-36 hours.

[0026] In one embodiment of the present invention, the container used for storing the aged liquor in step (2) is a ceramic jar, a stainless steel tank, or a glass jar.

[0027] In one embodiment of the present invention, step (2) specifically comprises:

[0028] The newly distilled liquor is put into a container, a catalytic aid is added, and the liquor is stored for aging to obtain a liquor with a mature aroma and flavor.

[0029] In one embodiment of the present invention, the liquor in step (2) is one or more of Maotai-flavor liquor, Qing-flavor liquor, and Luzhou-flavor liquor.

[0030] In one embodiment of the present invention, the storage and aging in step (2) is storage and aging at 10-40° C. for more than one month.

[0031] In one embodiment of the present invention, step (2) may be assisted by one or more of dissolved oxygen, irradiation, ultrasound, and electromagnetic radiation; wherein, dissolved oxygen is ventilated 1-5 times per month; irradiation is irradiated by one or more of electron beam, ray, and ultraviolet light; the intensity of electron beam irradiation is 0.5-2.5 kGy, and the time is 10-60 days; the intensity of Co-γ ray is 0.5-4 kGy, and the time is 10-60 days; the ultraviolet light wavelength of ultraviolet light irradiation is 340-400 nm, the duration is 5-300 h, and the power is 0.6-5 KW.

[0032] In one embodiment of the present invention, the characteristic substance of aged aroma and flavor is one or more of 2,3-butanedione, dimethyl trisulfide, methyl-2-methyl-3-furanyl disulfide, 4-methylguaiacol, vanillyl ethyl ketone, HDMF, HEMF, vanillin, γ-nonalactone, 2-ethylpyrazine, 2,5-dimethylpyrazine, fenugreek lactone, 2-methylpyrazine, 4-methylphenol, γ-butyrolactone, 2-acetyl-5-methylfuran, 2,3-dimethylpyrazine, 5-methylfurfural, 2,6-dimethylpyrazine, 2-acetylfuran, 2,3,5-trimethylpyrazine, 2,3-dimethyl-5-ethylpyrazine, 2,3,5,6-tetramethylpyrazine, 2-methylpropionic acid, 3-hydroxy-2-butanone, furfural, and 3-methyl-2,4-nonanedione.

[0033] In one embodiment of the present invention, in step (1), Fe 2 O 3 @SiO 2 -Al 2 O 3 The preparation method is as follows:

[0034] S1: 166 mg of 1,4-phthalic acid and 675 mg of ferric chloride hexahydrate were reacted in 15 mL of N,N-dimethylformamide at 160 °C for 22 h to obtain MIL-101-Fe;

[0035] S2: Disperse 0.01 g of aluminum sec-butoxide in 150 μL of sec-butanol to obtain an aluminum sec-butoxide solution; mix 300 μL of tetramethyl orthosilicate, 150 μL of the aluminum sec-butoxide solution, 20 μL of acetic acid and 10 μL of ethyl acetoacetate to obtain a mixed solution;

[0036] S3: MIL-101-Fe is vacuum activated; then, it is immersed in the mixed solution at room temperature for 3 hours, taken out, filtered, and the obtained solid is dried at 80°C for 12 hours to form SiAl@MIL;

[0037] S4: SiAl@MIL was heat treated at 950℃ for 2h to obtain Fe 2 O 3@SiO 2 -Al 2 O 3 .

[0038] In one embodiment of the present invention, in step (1), CuO@SiO 2 -Al 2 O 3 The preparation method is as follows:

[0039] A: 1-methyl-2-pyrrolidone, polyethersulfone and polyvinylpyrrolidone were mixed in a mass ratio of 1:1.5:1.5, and stirred at 60 rpm for 2.5 h in a sealed constant temperature water bath at 75°C to obtain a light yellow viscous liquid;

[0040] B: Add 1500 mg SiO2 to 15 mL of light yellow viscous liquid. 2 , 3500 mg of alumina monohydrate, 2000 mg of CuO, fully dispersed at 25° C. and 180 rpm for 24 h to obtain a dispersion;

[0041] C: The dispersion is squeezed into spherical particles of equal size, and then soaked in water at room temperature (25°C) for 3 days, during which the water is constantly changed to allow phase transformation to occur to form small solid particles;

[0042] D: Sinter the solid small particles as follows:

[0043] The first stage (removal of free water): heating to 100 °C at a heating rate of 1.5 °C / min and maintaining for 2.5 h;

[0044] The second stage (removal of bound water and some organic matter): heating from 100°C to 200°C at a heating rate of 1.5°C / min and maintaining for 2.5h;

[0045] The third stage (removal of organic matter): the temperature was increased from 200°C to 400°C at a heating rate of 1.5°C / min and maintained for 2.5h;

[0046] The fourth stage (conversion of alumina monohydrate to activated alumina): finally, the temperature was increased from 400°C to 600°C at a heating rate of 1.5°C / min and maintained for 2.5h;

[0047] CuO@SiO 2 -Al 2 O 3 ;

[0048] All the raw materials used were dried in an oven at 65°C overnight.

[0049] In one embodiment of the present invention, in step (1), Pt-Pb@SiO 2 -Al2 O 3 The preparation method is as follows:

[0050] a: 150 μL of a mixed solution of aluminum sec-butoxide and sec-butanol (0.01 g of aluminum sec-butoxide dispersed in 150 μL of sec-butanol), 300 μL of tetramethyl orthosilicate, 20 μL of acetic acid and 10 μL of ethyl acetoacetate were mixed to obtain a mixed solution A;

[0051] b: 5g chloroplatinic acid (H 2 PtCl 6 6H 2 O) and 5gPdCl 2 Dissolve in 15 mL of 0.2 mol / L dilute hydrochloric acid aqueous solution to obtain mixed solution B, then mix mixed solution B with mixed solution A at a volume ratio of 1:1, and stir at 25°C (normal temperature) and 500 rpm for 3 h to obtain mixed solution C;

[0052] c: The mixed solution C was dried under microwave for 30 min and then calcined in a muffle furnace (heated to 550 °C at 2 °C / min and maintained for 5 h) to obtain Pt-Pb@SiO 2 -Al 2 O 3 .

[0053] The second object of the present invention is the aged fragrant and flavored liquor prepared by the method of the present invention.

[0054] The third object of the present invention is to use the aged fragrant and flavored liquor of the present invention in the field of liquor processing.

[0055] The fourth object of the present invention is a finished liquor, which is obtained by blending the aged liquor with aged aroma and flavor described in the present invention.

[0056] [Beneficial Effects]

[0057] The invention adds a catalytic aid during the storage and aging process, which is beneficial to improving the flavor components in the liquor, greatly improving the characteristic substances of aged aroma and flavor, especially improving the contents of 3-hydroxy-2-butanone, 4-methylguaiacol, vanillyl ethyl ketone, HDMF, HEMF, vanillin, fenugreek lactone and 2,3,5-trimethylpyrazine. BRIEF DESCRIPTION OF THE DRAWINGS

[0058] Figure 1 This is the full two-dimensional chromatogram of the liquor obtained in Example 1.

[0059] Figure 2 This is the three-dimensional chromatogram of the liquor obtained in Example 1.

[0060] Figure 3This is the GC-MS chromatogram obtained in Example 1. DETAILED DESCRIPTION

[0061] The preferred embodiments of the present invention are described below. It should be understood that the embodiments are for better explaining the present invention and are not used to limit the present invention.

[0062] Test method:

[0063] 1. Determination of compound content:

[0064] (1) Detection of furanones:

[0065] ① Liquid-liquid extraction sample pretreatment:

[0066] 20 mL of liquor sample was diluted with saturated saline to an alcohol content of 10% vol, and then the isotope internal standard of fenugreek lactone was added, followed by extraction with 20 mL of dichloromethane as the extractant, a total of 3 extractions, each for 5 min; a total of 60 mL of the extraction components were collected, 30 g of anhydrous sodium sulfate was added thereto, and stored at -20°C overnight; the 60 mL of the extraction components were then concentrated to 200 μL by nitrogen blowing and waited for injection.

[0067] ②Use gas chromatography-mass spectrometry (GC-MS) to analyze samples in selected ion monitoring mode (SIM);

[0068] The GC conditions are as follows:

[0069] Agilent 7890 gas chromatograph tandem with 5975 mass spectrometer was used;

[0070] The chromatographic column was DB-FFAP (60 m × 0.25 mm × 0.25 μm, Agilent, America); the temperature program of the chromatographic column (DB-FFAP) was as follows: the initial temperature was 45 °C for 2 min, then increased to 230 °C at 6 °C / min and maintained for 10 min;

[0071] He (>99.999%) was used as carrier gas, with a flow rate of 2 mL / min and an injection port temperature of 230 °C;

[0072] The MS conditions are as follows:

[0073] The sample solvent delay time was 8 min;

[0074] EI ionization source, ionization energy of 70 eV, ion source temperature of 230 ° C, mass spectrometry ion scanning range of 35-350 amu;

[0075] The quantification of fenugreek lactone, furanone HDMF and ethyl furanone HEMF was carried out in the selected ion monitoring (SIM) mode, and the characteristic ions were 128 m / z, 128 m / z and 142 m / z, respectively.

[0076] ③ Standard curve drawing:

[0077] Use chromatographic grade ethanol and ultrapure water to prepare a simulated liquor matrix solution (pH = 3.5, alcohol content 53% vol) for later use;

[0078] Accurately weigh a certain mass of furanone compound standards (trigonelline lactone, HDMF and ethyl furanone HEMF) and dissolve them in a simulated liquor solution to prepare a series of standard solutions with different concentration gradients; treat the standard solutions according to the sample pretreatment method in step ①, perform instrumental analysis according to step ②, and prepare a standard curve based on the peak area ratio and concentration ratio of the target substance to the internal standard as the horizontal and vertical coordinates, respectively.

[0079] ④Detection:

[0080] The liquor to be tested is tested according to steps ① and ② to obtain the peak area, which is then substituted into the standard curve of step ③ to obtain the concentration of the substance to be tested.

[0081] (2) Detection of other substances:

[0082] ①Pretreatment of liquor samples:

[0083] The liquor sample was diluted with ultrapure water to an alcohol content of 10% vol, and then 5 mL was added to a 20 mL headspace bottle, followed by 1.5 g NaCl and 2-methylpyrazine-d6, guaiacol-d3, and diisopropyl disulfide as internal standards.

[0084] After the samples were mixed, HS-SPME was performed using a MPS2 (Gerstel, Germany) multifunctional autosampler. The conditions were as follows: the samples were equilibrated at 40°C for 5 minutes, stirred and extracted at 250 rpm for 40 minutes, and the extraction head model was DVB / CAR / PDMS (2 cm, 50 / 30 μm, Supelco, America). After the extraction, desorption was performed at 250°C for 5 minutes.

[0085] ② Determination of compound content in liquor samples by comprehensive two-dimensional gas chromatography:

[0086] Chromatographic conditions: The gas chromatograph was Agilent 7890B (Agilent, America), the first-dimensional chromatographic column was a DB-FFAP capillary column (60m×0.25mm×0.25μm, Agilent, America), and the second-dimensional chromatographic column was an Rx-17 Si capillary column (0.8m×0.25mm×0.36μm, Restek, America); the first-dimensional chromatographic column and the second-dimensional chromatographic column were connected in series through a four-nozzle two-stage thermal modulator, and the transmission temperature was 240°C; He (>99.999%) was used as the carrier gas, the flow rate was 1mL / min, and the injection port temperature was 250°C.

[0087] The temperature heating program of the one-dimensional chromatographic column mainly consists of four stages. The starting temperature of the first stage is set to 45°C and maintained for 3 minutes; the second stage is heated to 150°C at a heating rate of 4°C / min and then maintained for 2 minutes; the third stage is heated to 200°C at a heating rate of 6°C / min; the last stage is heated to 230°C at a heating rate of 10°C / min and then maintained for 10 minutes.

[0088] The total time of the entire analysis process was 53 minutes, and the temperature of the second-dimensional column oven was 5°C higher than that of the first-dimensional column oven throughout the process; the compensation temperature of the modulator was set to 20°C, the modulation cycle of the modulator was 4 seconds, and the heat pulse time was 0.8 seconds.

[0089] Mass spectrometry conditions: ion source voltage 70 eV, temperature 230 °C, transfer line temperature 240 °C, ion scan range 35-400 amu, scan frequency 100 spestra / s.

[0090] ③ Standard curve drawing:

[0091] Use chromatographic grade ethanol and ultrapure water to prepare a simulated liquor matrix solution (pH = 3.5, alcohol content 53% vol) for later use;

[0092] Accurately weigh a certain mass of the compound standard and dissolve it in the simulated liquor solution to prepare a series of standard solutions with different concentration gradients. The standard solution is treated according to the above sample pretreatment method and then analyzed by the instrument. The peak area ratio and concentration ratio of the target substance to the internal standard substance are used as the horizontal and vertical coordinates to prepare the standard curve.

[0093] ④Detection:

[0094] The liquor to be tested is tested according to steps ① and ② to obtain the peak area, which is then substituted into the standard curve of step ③ to obtain the concentration of the substance to be tested.

[0095] 2. Sensory test:

[0096] Standard substances with aged aroma characteristics (trigonelline lactone, HDMF, vanillin, etc.) were prepared into a certain concentration and diluted to a certain concentration range. An intensity scale was established. A unified scale was reached through discussion by the tasting panel, and a scale test was conducted after two weeks of training.

[0097] The evaluators scored the intensity of the aged aroma characteristics on a scale of 0 (none) to 100 (very strong). The evaluation team consisted of 40 people (22 women and 18 men, aged 25 to 40) with extensive sensory evaluation experience. All evaluators had previously received more than one year of training in the description of odor attributes. The evaluators scored the sensory characteristics of the liquor samples on three levels: color, aroma, and taste, on a scale of 0 (none) to 100 (very strong). The score was calculated by removing the highest value, removing the lowest value, and then taking the average value as the final sensory score.

[0098] The raw materials used in the embodiment:

[0099] 1.Fe 2 O 3 @SiO 2 -Al 2 O 3 Preparation:

[0100] (1) 166 mg of 1,4-phthalic acid and 675 mg of ferric chloride hexahydrate were subjected to solvothermal reaction in 15 mL of N,N-dimethylformamide at 160° C. for 22 h to obtain MIL-101-Fe;

[0101] (2) dispersing 0.01 g of aluminum sec-butoxide in 150 μL of sec-butanol to obtain an aluminum sec-butoxide solution; mixing 300 μL of tetramethyl orthosilicate, 150 μL of the aluminum sec-butoxide solution, 20 μL of acetic acid and 10 μL of ethyl acetoacetate to obtain a mixed solution;

[0102] MIL-101-Fe was vacuum activated, then immersed in the mixed solution at room temperature (25°C) for 3 h, taken out, filtered, and the obtained solid was dried at 80°C for 12 h to form SiAl@MIL;

[0103] (3) SiAl@MIL was heat treated at 950℃ for 2h to obtain Fe 2 O 3 @SiO 2 -Al 2 O 3 .

[0104] 2.CuO@SiO 2 -Al 2 O 3 Preparation:

[0105] (1) 1-methyl-2-pyrrolidone, polyethersulfone and polyvinylpyrrolidone were mixed in a mass ratio of 1:1.5:1.5, and the mixture was sealed in a constant temperature water bath at 75° C. and stirred at 60 rpm for 2.5 h to obtain a light yellow viscous liquid;

[0106] (2) Add 1500 mg SiO 2 , 3500 mg of alumina monohydrate, 2000 mg of CuO, fully dispersed at 25° C. and 180 rpm for 24 h to obtain a dispersion;

[0107] (3) The dispersion is squeezed into spherical particles of equal size, and then immersed in water at 25°C for 3 days, during which the water is constantly changed to allow phase transformation to occur to form solid small particles;

[0108] (4) Sintering the solid small particles as follows:

[0109] The first stage (removal of free water): heating to 100 °C at a heating rate of 1.5 °C / min and maintaining for 2.5 h;

[0110] The second stage (removal of bound water and some organic matter): heating from 100°C to 200°C at a heating rate of 1.5°C / min and maintaining for 2.5h;

[0111] The third stage (removal of organic matter): heating from 200°C to 400°C at a heating rate of 1.5°C / min and maintaining for 2.5h;

[0112] The fourth stage (conversion of alumina monohydrate to activated alumina): finally, the temperature was increased from 400°C to 600°C at a heating rate of 1.5°C / min and maintained for 2.5h;

[0113] CuO@SiO 2 -Al 2 O 3 ;

[0114] All the raw materials used were dried in an oven at 65°C overnight.

[0115] 3. Pt-Pb@SiO 2 -Al 2 O 3 The preparation method is as follows:

[0116] (1) 150 μL of a mixed solution of aluminum sec-butoxide and sec-butanol (0.01 g of aluminum sec-butoxide dispersed in 150 μL of sec-butanol), 300 μL of tetramethyl orthosilicate, 20 μL of acetic acid, and 10 μL of ethyl acetoacetate were mixed to obtain a mixed solution A;

[0117] (2) Add 5 g of chloroplatinic acid (H 2PtCl 6 6H 2 O) and 5g PdCl 2 Dissolve in 15 mL of 0.2 mol / L dilute hydrochloric acid aqueous solution to obtain mixed solution B, then mix mixed solution B with mixed solution A at a volume ratio of 1:1, and stir at 25°C (normal temperature) and 500 rpm for 3 h to obtain mixed solution C;

[0118] (3) The mixed solution C was dried under microwave for 30 min and then calcined in a muffle furnace (heated to 550 °C at 2 °C / min and maintained for 5 h) to obtain Pt-Pb@SiO 2 -Al 2 O 3 .

[0119] 4.Fe 2 O 3 @SiO 2 -Al 2 O 3 、CuO@SiO 2 -Al 2 O 3 、Pt-Pb@SiO 2 -Al 2 O 3 , Fe 2 O 3 、SiO 2 、Al 2 O 3 , the particle size of CuO is 0.1mm.

[0120] 5. Clay: Clay used for making pottery jars, without modification or treatment, with a particle size of 0.1 mm.

[0121] 6. Pottery powder and pottery fragments: Pottery powder is the powder obtained by grinding the pottery jar, with a particle size of 0.1mm; pottery fragments are fragments of the pottery jar.

[0122] 7. The sauce-flavor liquor is new liquor that has not been stored and is purchased from Guizhou.

[0123] 8. Ceramic jars and stainless steel tanks: Ceramic jars and stainless steel tanks are commonly used to store liquor.

[0124] Example 1

[0125] A method for regulating the aged aroma and flavor of liquor comprises the following steps:

[0126] (1) 3g Fe 2 O 3 @SiO 2 -Al 2 O 3 、3g CuO@SiO2 -Al 2 O 3 、3g Pt-Pb@SiO 2 -Al 2 O 3 4gFe 2 O 3 、4gSiO 2 、4gAl 2 O 3 , 4g CuO and 100g clay were mixed evenly, 30g water was added to mix, and a spherical mold (with a radius of 1cm) was put into shape, and sintered at 1000°C for 36h to obtain a catalyst promoter;

[0127] (2) The newly distilled liquor (sauce-flavor liquor) is placed in a ceramic jar, and 10% (relative to the mass percentage of the liquor) of a catalytic aid is added. The jar is stored and aged at 30° C. for 2 months, and oxygen is aerated once a month until the liquor is saturated with oxygen to obtain a liquor with a mature aroma and flavor.

[0128] The obtained aged liquor with aged aroma and flavor was subjected to performance test, and the test results are shown in Table 1:

[0129] Table 1 Characteristic substances test of aged aroma and flavor

[0130] Characteristic substances Concentration (μg / L) 2,3-Butanedione 1132±33.96 Dimethyl trisulfide 183±3.66 Methyl-2-methyl-3-furyl disulfide 2.92±0.02 4-Methylguaiacol 39.1±0.57 Vanillyl acetone 50.5±0.92 HDMF 61.5±1.66 HEMF 85.4±1.11 Vanillin 771±5.42 γ-Nonalactone 364±10.56 2-Ethylpyrazine 171±3.42 2,5-Dimethylpyrazine 290±5.81 Trigonella Lactone 645±9.80 2-Methylpyrazine 342±6.84 4-Methylphenol 403±12.09 γ-Butyrolactone 871±17.42 2-Acetyl-5-methylfuran 969±29.07 2,3-Dimethylpyrazine 915±8.17 5-Methylfurfural 2723±17.23 2,6-Dimethylpyrazine 2454±43.62 2-Acetylfuran 2864±61.92 2,3,5-Trimethylpyrazine 4464±69.28 2,3-Dimethyl-5-ethylpyrazine 2701±27.01 2,3,5,6-Tetramethylpyrazine 61310±239.31 2-Methylpropionic acid 8689±347.56 3-Hydroxy-2-butanone 9355±784.85 Furfural 226207±4524.14 3-Methyl-2,4-nonanedione 9.48±0.07

[0131] Example 2

[0132] Adjust the "3g Fe 2 O 3 @SiO 2 -Al 2 O 3 、3g CuO@SiO 2 -Al 2 O 3 、3g Pt-Pb@SiO 2 -Al 2 O 3 4gFe 2 O 3 , 4g SiO 2 , 4g Al 2 O 3 , 4g CuO" is "4.5g Fe 2 O 3 @SiO 2 -Al 2 O 3 、4.5g CuO@SiO 2 -Al 2 O 3 、10gFe 2 O3 , 6g SiO 2 ", the rest is consistent with Example 1, and a liquor with aged fragrance and flavor is obtained.

[0133] Example 3

[0134] The "ceramic jar" in step (1) of Example 1 is adjusted to a "stainless steel tank", and the rest remains the same as Example 1 to obtain a liquor with an aged aroma and flavor.

[0135] Example 4

[0136] The amount of the catalyst aid added in step (2) of Example 1 was adjusted to 5%, and the other conditions were kept consistent with Example 1 to obtain a liquor with an aged aroma and flavor.

[0137] Example 5

[0138] The dissolved oxygen in the storage aging process of step (2) of Example 1 was adjusted to irradiation (electron beam, intensity 0.5 kGy, time 40 days), and the other conditions were kept consistent with Example 1 to obtain a liquor with an aged aroma and flavor.

[0139] Example 6

[0140] Adjust the "3g Fe 2 O 3 @SiO 2 -Al 2 O 3 、3g CuO@SiO 2 -Al 2 O 3 、3g Pt-Pb@SiO 2 -Al 2 O 3 4gFe 2 O 3 , 4g SiO 2 , 4g Al 2 O 3 , 4g CuO" is "4.5g Fe 2 O 3 @SiO 2 -Al 2 O 3 、4.5g Pt-Pb@SiO 2 -Al 2 O 3 , 5g SiO 2 、5gAl 2 O 3 , 6g CuO", and the rest is consistent with Example 1 to obtain a liquor with an aged aroma and flavor.

[0141] Example 7

[0142] The dissolved oxygen in the storage aging process of step (2) of Example 1 is omitted, and the other steps are the same as those of Example 1 to obtain a liquor with an aged aroma and flavor.

[0143] The obtained liquor was subjected to performance test, and the test results are as follows:

[0144] Table 2 Characteristic substances test of aged aroma and taste

[0145]

[0146] Table 3 Sensory test results

[0147]

[0148] Comparative Example 1

[0149] The amount of the catalyst aid added in step (2) of Example 1 was adjusted to 0, and the other factors were kept consistent with Example 1 to obtain liquor.

[0150] Comparative Example 2

[0151] Adjust the CuO@SiO in step (1) of Example 1 2 -Al 2 O 3 The mass ratio of CuO and SiO is 1:10:10. 2 、Al 2 O 3 A mixture of nanomaterials (0.1 mm) and other conditions are consistent with those in Example 1 to obtain white wine.

[0152] Comparative Example 3

[0153] Adjust the "3g Fe 2 O 3 @SiO 2 -Al 2 O 3 、3g CuO@SiO 2 -Al 2 O 3 、3g Pt-Pb@SiO 2 -Al 2 O 3 4gFe 2 O 3 , 4g SiO 2 、4gAl 2 O 3 , 4g CuO" is "25g Fe with a mass ratio of 1.5:1.5:10:10 2 O 3 ,CuO,SiO 2 、Al 2 O3 A mixture of nanomaterials (0.1 mm) was prepared, and the rest was consistent with Example 1 to obtain white wine.

[0154] Comparative Example 4

[0155] Step (1) of Example 1 is omitted, and the catalyst in step (2) is adjusted to a ceramic piece (50×50 mm). The rest is kept consistent with Example 1 to obtain white wine.

[0156] Comparative Example 5

[0157] Adjust the "3g Fe 2 O 3 @SiO 2 -Al 2 O 3 、3g CuO@SiO 2 -Al 2 O 3 、3g Pt-Pb@SiO 2 -Al 2 O 3 4gFe 2 O 3 , 4g SiO 2 、4gAl 2 O 3 , 4g CuO” is “25g pottery powder”, and the rest is consistent with Example 1 to obtain white wine.

[0158] The obtained liquor was subjected to performance test, and the test results are as follows:

[0159] Table 4 Characteristic substances test of aged aroma and taste

[0160]

[0161] Table 5 Sensory test results

[0162]

[0163] Although the present invention has been disclosed as above in the form of a preferred embodiment, it is not intended to limit the present invention. Anyone familiar with this technology can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be based on the definition of the claims.

Claims

1. A method for regulating the aged aroma and flavor of liquor, characterized in that: The steps include: (1) mixing the catalyst promoter and clay evenly, adding water to mix and forming, and firing to obtain the catalyst promoter; The catalyst promoter is composed of two components, the first component is two or three of Fe2O3@SiO2-Al2O3, CuO@SiO2-Al2O3, and Pt-Pb@SiO2-Al2O3; the second component is one or more of Fe2O3, SiO2, Al2O3, and CuO; the mass ratio of the first component to the second component is 2:0.1-6; (2) A catalytic aid is added during the storage of aged liquor, and the amount of the catalytic aid added is 0.1-15% of the liquor mass, but not 0.

2. The method according to claim 1, characterized in that In step (1), the mass ratio of the catalyst aid, clay and water is 1-30:100:10-30.

3. The method according to claim 1, characterized in that The mass ratio of Fe2O3@SiO2-Al2O3, CuO@SiO2-Al2O3 and Pt-Pb@SiO2-Al2O3 in the first component of the catalyst in step (1) is 1-3:1-3:1-3; the mass ratio of Fe2O3, SiO2, Al2O3 and CuO in the second component is 0.5-1.5:1-6:1-6:0.5-1.

5.

4. The method according to claim 1, characterized in that: Step (2) is specifically: The newly distilled liquor is put into a container, a catalytic aid is added, and the liquor is stored for aging to obtain a liquor with a mature aroma and flavor.

5. The method according to claim 1, characterized in that In step (2), the liquor is one or more of sauce-flavor liquor, light-flavor liquor, and strong-flavor liquor.

6. The method according to claim 1, characterized in that The storage and aging in step (2) is performed at 10-40° C. for more than one month.

7. The method according to claim 1, characterized in that Step (2) may be assisted by one or more of dissolved oxygen, irradiation, ultrasound, and electromagnetic.

8. The liquor with aged aroma and flavor prepared by the method according to any one of claims 1 to 7.

9. Use of the aged fragrant and flavored liquor according to claim 8 in the field of liquor processing.

10. A finished liquor, characterized in that: The liquor is obtained by blending the aged fragrant and flavored liquor described in claim 8.

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