A method for preparing low-deuterium liquor with precise and controllable deuterium content

Abstract

The present application relates to the technical field of liquor processing, and particularly relates to a low-deuterium liquor preparation method with precisely controllable deuterium content. The method detects the alcohol content of high-grade liquor base liquor, the deuterium concentration of the water phase of the base liquor, and the deuterium concentrations of low-deuterium blending water and ordinary blending drinking water, and sets the target alcohol content of the product and the target deuterium concentration of the water phase of the product. Based on the deuterium conservation relationship of the whole liquor body taking into account the deuterium contribution of the water phase of the base liquor, the volume of the low-deuterium blending water and the ordinary blending drinking water to be added is calculated. The two kinds of blending water are mixed uniformly in advance and then blended with the base liquor. The volume shrinkage effect of the mixture of ethanol and water is compensated through a small-scale experiment. The deuterium concentration of the water phase and the alcohol content of the blended liquor are detected and closed-loop fine-tuned. Finally, the low-deuterium liquor is obtained through filtration and filling. The method does not need to modify the traditional brewing process, can prepare low-deuterium liquor with a deuterium content of 10-130 ppm and an alcohol content of 30%-65%vol, and reduces the use amount of high-purity low-deuterium water.

Description

Technical Field

[0001] This invention relates to the field of liquor processing technology, specifically to a method for blending and preparing low-deuterium liquor with precisely controllable deuterium content. Background Technology

[0002] Deuterium is a stable isotope of hydrogen. The background deuterium content in ordinary freshwater in nature is consistently between 145 and 155 ppm. Low-deuterium water refers to special water bodies with a deuterium content significantly lower than the background level of natural water bodies. Using low-deuterium water in the blending of baijiu (Chinese white liquor) can optimize the association structure of water molecules in the liquor, improving its taste and storage stability. Low-deuterium baijiu has become an important development direction for the upgrading and segmentation of the baijiu category.

[0003] Existing low-deuterium baijiu production processes mainly fall into two categories. One category involves replacing deuterium water throughout the entire brewing process, using deuterium water in the entire process of koji making, grain moistening, water addition, fermentation, and distillation. This approach reduces the base deuterium content of the liquor from the source, but requires modifications to the entire brewing production line's water supply system. The overall consumption of deuterium water is extremely high, resulting in high production costs. Traditional mature production lines are difficult to integrate with this approach, making it only suitable for newly built specialized workshops and challenging for industrialization. The other category involves direct blending in the later stages, where deuterium water is directly added to high-proof baijiu to reduce its alcohol content. This is currently the mainstream, simplified process in the industry, but it suffers from the following technical drawbacks: First, the contribution of deuterium in the water phase of the base liquor is ignored. The original liquor of high-proof baijiu naturally contains a certain proportion of native water, with a deuterium content of about 150 ppm. Existing technology only calculates the deuterium value of the added low-deuterium water and does not establish a deuterium conservation model for the water phase of the whole liquor, resulting in the deuterium content of the finished product deviating significantly from the design value. Secondly, there is no precise quantitative proportioning system. Existing technologies are mostly qualitative feeding, lacking a general mathematical calculation model, and cannot achieve standardized and reproducible production with specified deuterium content. Third, the physical error was not compensated. There was a significant volume shrinkage effect when ethanol was mixed with water. The theoretical feed volume and the actual production volume were different, resulting in a double loss of control over alcohol content and deuterium content. Fourth, the feeding method is unreasonable. Directly adding low-deuterium water and ordinary water separately can easily cause local deuterium concentration stratification in the tank, resulting in poor homogeneity of the liquor. Fifth, there is a lack of a closed-loop quality control system and a lack of quality control processes for finished product testing and reverse fine-tuning. Product indicators vary greatly between different production batches, making it difficult to achieve industrialized and standardized mass production.

[0004] In addition, some processes use distillation of the original liquor to remove water and then blend it with low-deuterium water. Although this can avoid interference from the water in the base liquor, the distillation process will cause a large loss of flavor substances such as esters and alcohols in the liquor, destroying the inherent style of the original liquor and reducing the sensory quality of the product.

[0005] The existing technology lacks an industrial-scale preparation technology for low-deuterium baijiu that does not alter the traditional brewing process, does not damage the flavor of the original liquor, can precisely and quantitatively control the deuterium content, has strong batch consistency, and has controllable production costs. Summary of the Invention

[0006] The technical problem to be solved by the present invention is to overcome the problems of inaccurate deuterium content and large batch differences caused by neglecting the contribution of deuterium in the water phase of the base liquor, lack of quantitative proportioning model, failure to compensate for volume shrinkage, uneven feeding, and lack of closed-loop quality control in the blending process of low deuterium liquor in the existing technology, and to provide a method for blending and preparing low deuterium liquor with precise and controllable deuterium content.

[0007] The technical solution adopted by the present invention to solve its technical problem is: a method for preparing low-deuterium baijiu, which first measures the alcohol content of high-proof baijiu base liquor, the deuterium concentration of the base liquor's own aqueous phase, the deuterium concentration of low-deuterium blending water and ordinary blended drinking water, and sets the target alcohol content and the target deuterium concentration of the finished product's aqueous phase. Then, the volume of feed is calculated based on the deuterium conservation relationship of the whole liquor. This conservation relationship relates the total deuterium of the aqueous phase of the base liquor, the total deuterium of the added low-deuterium blending water, and the total deuterium of the added ordinary blending drinking water to the total deuterium of the entire aqueous phase of the finished liquor. Thus, the deuterium contribution of the aqueous phase of the base liquor is included in the calculation. The volumes of the added low-deuterium blending water and the added ordinary blending drinking water are obtained by solving the system of equations. The calculated volume of deuterium-rich blended water was then pre-mixed evenly with ordinary blended drinking water to prepare compound blended water. Then, the compounded water is added to the high-proof liquor base and stirred and mixed. Before blending, the alcohol content is measured by a small-scale test and the amount of water added is corrected to compensate for the volume shrinkage effect of ethanol and water mixing. Afterwards, the deuterium concentration and alcohol content of the blended liquor were tested. When the measured values ​​deviated from the target values, the amount of water to be added was calculated in reverse according to the aforementioned deuterium conservation relationship of the whole liquor. A small amount of low-deuterium blended water or ordinary blended drinking water was added for fine adjustment. Finally, the finely adjusted liquor was filtered and bottled to obtain the low-deuterium baijiu finished product.

[0008] Furthermore, the volume V of low-deuterium conditioning water is added. L The calculation formula is as follows;

[0009] Add the volume of regular prepared drinking water V N The calculation formula is as follows;

[0010] in, C 0 The deuterium concentration in the aqueous phase of the base liquor. CL To reduce the deuterium concentration in the prepared water, C N The deuterium concentration for ordinary prepared drinking water, C T The target deuterium concentration in the aqueous phase of the finished product. V win The volume of the aqueous phase inherent in the base spirit. This refers to the total volume of the aqueous phase in the finished wine. To replenish the total volume of the water to be prepared, and , To replenish the volume of deuterium-treated water, To supplement the volume of ordinary prepared drinking water.

[0011] Furthermore, when the calculation yields If the concentration is ≤0, it indicates that the target deuterium concentration is too high, and there is no need to add low-deuterium blended water. All additional blended water should be ordinary drinking water. When the calculated concentration is... ≥ If this occurs, it indicates that the existing deuterium concentration in the blended water is too high and cannot meet the target low deuterium index, so it is necessary to replace it with low deuterium blended water with an even lower deuterium concentration.

[0012] Furthermore, the base liquor for high-proof baijiu is grain distilled using solid-state or liquid-state methods, with an alcohol content of 70%~85% vol; the deuterium concentration of the low-deuterium blending water is 1~130 ppm; the ordinary blended drinking water is drinking water that meets the GB5749 standard, with a deuterium concentration of 145~155 ppm; the target alcohol content of the finished product is 30%~65% vol, and the target deuterium concentration of the aqueous phase of the finished product is 10~130 ppm.

[0013] Furthermore, the deuterium-rich blended water and ordinary blended drinking water are stirred and mixed in a premixing tank for 15-30 minutes to obtain homogeneous compound blended water; When mixing, the stirring speed should be 30~80 r / min and the stirring time should be 15~45 min; the scale of the small-scale experiment should be 5~10.

[0014] Furthermore, the blended liquor is sealed and kept in the dark for 7 to 30 days to mature, with the storage environment temperature being 10 to 25°C, so that the liquor structure can be stabilized through natural molecular association.

[0015] Furthermore, when the measured deuterium concentration in the finished product's aqueous phase deviates from the target deuterium concentration by more than ±2 ppm, or when the measured alcohol content exceeds the national standard tolerance range, the volume of low-deuterium blended water or ordinary blended drinking water to be added is calculated in reverse based on the deuterium conservation relationship of the whole liquor. After adding a small amount, the mixture is stirred and homogenized until the measured indicators are met.

[0016] Furthermore, the concentration of deuterium in the aqueous phase was detected by liquid water isotope mass spectrometry or aqueous phase nuclear magnetic resonance (NMR). Before detection, the wine was pretreated by separating the ethanol and aqueous phases, and the contribution of deuterium isotopes in the ethanol phase was negligible.

[0017] The beneficial effects of this invention are as follows: First, by incorporating the deuterium contribution from the base liquor's aqueous phase into the overall deuterium conservation relationship and quantitatively calculating the amount of water to be added, the deuterium content of the finished product can avoid deviations from the design value due to neglecting the background deuterium in the base liquor, thus achieving quantitative and reproducible production of the specified target deuterium content; Second, by pre-mixing low-deuterium blending water and ordinary blending drinking water evenly before adding the raw materials, local deuterium concentration stratification within the tank can be avoided, improving the homogeneity and batch consistency of the liquor; Third, by compensating for the volume shrinkage effect of mixing ethanol and water through small-scale experiments, it is possible to... The system corrects the volume deviation between theoretical calculations and actual production, ensuring that both alcohol content and deuterium content meet standards simultaneously. Fourth, the closed-loop quality control system, which includes finished product testing and reverse fine-tuning, corrects batch-to-batch index drift and ensures product index stability. Fifth, since the system is implemented only in the blending stage without altering core processes such as koji making, fermentation, and distillation, and reduces the amount of high-purity low-deuterium water by blending ordinary water with low-deuterium water, it helps reduce production costs and is compatible with existing baijiu production lines. Sixth, since there is no need to remove the water from the original liquor through distillation, the system can retain the flavor substances such as esters and alcohols inherent in the original liquor, maintaining its original style. Attached Figure Description

[0018] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0019] Figure 1 This is a flowchart illustrating the overall process flow of a method for preparing low-deuterium baijiu with precisely controllable deuterium content according to the present invention. Detailed Implementation

[0020] The present invention will now be described in further detail with reference to the accompanying drawings. These drawings are simplified schematic diagrams, illustrating only the basic structure of the invention, and therefore only show the components relevant to the invention.

[0021] like Figure 1 As shown, the low-deuterium baijiu blending and preparation method of the present invention includes the following process modules: raw material parameter detection, accurate calculation using a deuterium conservation model, dual-source premixing, small-scale volume shrinkage compensation, base liquor blending and stirring, closed-loop constant-temperature aging, closed-loop fine-tuning of the deuterium content and alcohol content of the finished product, filtration and bottling, etc. Step S1: Confirm the raw material parameters by testing: Measure the alcohol content of the high-proof baijiu base liquor, the deuterium concentration of the base liquor's aqueous phase, the deuterium concentration of the low-deuterium blending water, and the deuterium concentration of the ordinary blended drinking water. Set the target alcohol content and target deuterium concentration of the finished product's aqueous phase. The high-proof baijiu base liquor is a grain distilled raw liquor prepared by solid-state or liquid-state methods, with an alcohol content of 70%~85% vol. The deuterium content of the low-deuterium blending water is 1~130 ppm. The ordinary blended drinking water is production water that meets the GB5749 drinking water standard, with a deuterium content of 145~155 ppm. The target alcohol content of the finished product is limited to 30%~65% vol, and the target deuterium content of the finished product's aqueous phase is limited to 10~130 ppm. The deuterium content of the aqueous phase is detected using liquid water isotope mass spectrometry or aqueous phase nuclear magnetic resonance (NMR). Before detection, ethanol and aqueous phases are separated and pretreated. The contribution of deuterium isotopes in the ethanol phase is negligible. Step S2: Calculate the volume of each component based on the deuterium conservation model: Using 100L of high-proof baijiu base liquor as a unified calculation benchmark, first calculate the volume of ethanol in the base liquor and the volume of the original water in the base liquor according to the alcohol content of the base liquor, and then calculate the ideal total volume of the finished product and the total volume of all water phases of the finished liquor according to the target alcohol content. This yields the total volume of blending water that needs to be added during the blending and dilution stage. Based on the conservation relationship that the sum of the total deuterium in the water phase of the base liquor, the total deuterium in the added low-deuterium water, and the total deuterium in the added ordinary water equals the total deuterium in the water phase of the finished product, solve the equations simultaneously to obtain the volume of low-deuterium blending water and the volume of ordinary blending drinking water. Step S3, Premixing treatment of blended water: Mix the calculated volume of low-deuterium blended water with ordinary blended drinking water in a special premixing tank for 15-30 minutes to obtain homogeneous blended water. The base liquor is added after the two water sources are premixed evenly to avoid the deuterium concentration stratification in the tank caused by direct addition of materials. Step S4, blending and volume shrinkage compensation: Slowly pump the compounding water into the base liquor blending tank, stirring at 30~80 r / min for 15~45 min. Since there is physical volume shrinkage when ethanol and water are mixed, the theoretical calculation is an ideal model. Before the formal mass production, conduct a 5~10L small-scale experiment to measure the alcohol content of the small-scale product, make a slight correction to the total amount of water added, compensate for the volume shrinkage error, and ensure that the alcohol content of the mass production meets the standard. Step S5, Sealed Aging: The blended liquor is stored in a sealed, light-proof container and allowed to mature for 7 to 30 days. The storage temperature is controlled at 10 to 25°C. This process stabilizes the liquor structure through natural molecular association, eliminates the flavor fragmentation caused by blending disturbances, and preserves the original aroma and taste. Step S6, Finished Product Closed-Loop Testing and Reverse Fine-Tuning: After aging, take a sample, separate the aqueous phase to test the actual deuterium content and test the finished product alcohol content. When the measured deuterium content deviates from the target value by more than ±2ppm, or the alcohol content exceeds the national standard tolerance range, reuse the deuterium conservation relationship from step S2 for reverse calculation, add a small amount of low-deuterium blended water or ordinary blended drinking water for fine-tuning, stir and homogenize again until the indicators meet the standards; Step S7, Filtration and Bottling: The finely adjusted and qualified liquor is precisely filtered to remove trace suspended matter and impurities, and then filled and sealed in accordance with the national standard liquor bottling process to obtain standardized low-deuterium liquor finished product.

[0022] Example 1: A 53% vol, 50 ppm deuterium-containing baijiu was blended using a 75% vol strong-aroma base liquor. Based on 100L of base liquor, the deuterium concentration in the aqueous phase of the base liquor was 150 ppm, the deuterium concentration in the low-deuterium blending water was 25 ppm, and the deuterium concentration in the ordinary blending drinking water was 150 ppm. The target alcohol content was 53% vol, and the target deuterium concentration was 50 ppm. Model calculations showed that the ethanol volume in the base liquor was 75.00L, the aqueous phase volume of the base liquor was 25.00L, the ideal total volume of the finished product was approximately 141.51L, and the total volume of all aqueous phases in the finished product was 66.51L. Therefore, a total of 41.51L of blending water needed to be added, including the low-deuterium blending water. 33.21L of low-deuterium blended water and 8.30L of ordinary blended drinking water were added. The 33.21L of low-deuterium blended water and 8.30L of ordinary blended drinking water were stirred for 20 minutes to homogenize. After small-scale calibration, the mixture was stirred at 50r / min for 30 minutes to complete the blending. It was then sealed and left to stand for 14 days at a storage temperature of 18~22℃. The actual measured values ​​showed that the deuterium content of the aqueous phase of the finished product was 49.6ppm and the alcohol content was 53.1%vol. The indicators were qualified and no fine-tuning was required. After filtration and bottling, the finished product had a mellow body and pure aroma, retaining the original strong-aroma base liquor style. The above measured data were obtained based on the raw material parameters and process conditions recorded in this embodiment and are not extrapolated to other raw materials and operating conditions not recorded.

[0023] Example 2: A low-deuterium baijiu (Chinese white liquor) with a concentration of 53% vol and 50 ppm was blended using 83% vol base liquor. Based on 100L of base liquor, the base liquor aqueous phase deuterium concentration was 150 ppm, the low-deuterium blending water concentration was 25 ppm, and the ordinary blending drinking water concentration was 150 ppm. The target concentration was 53% vol and 50 ppm. Calculations showed that 45.28L of low-deuterium blending water and 11.32L of ordinary blending drinking water were added. After premixing and homogenizing the two waters, the mixture was stirred and blended. A small-scale shrinkage compensation test was conducted, and the mixture was sealed and allowed to stand for 20 days. Actual measurements showed that the finished product had a deuterium content of 50.2 ppm and an alcohol content of 52.8% vol, meeting the required standards. The above measured data are based on the raw material parameters and process conditions described in this example and are not extrapolated to other raw materials and operating conditions not described.

[0024] Example 3: A 45% vol, 60 ppm low-deuterium baijiu was blended using a 72% vol light-aroma base liquor. The base liquor aqueous phase deuterium concentration was 148 ppm, the low-deuterium blending water deuterium concentration was 40 ppm, and the ordinary blending drinking water deuterium concentration was 150 ppm. The target was 45% vol and 60 ppm. The process was carried out according to the above instructions. The actual measured deuterium content of the finished product was 58.9~61.1 ppm, and the alcohol content was 44.4~45.6% vol. The batch stability was good. The above measured data were obtained based on the raw material parameters and process conditions recorded in this example and are not extrapolated to other raw materials and operating conditions not recorded.

[0025] Comparative Example 1: Using the traditional single low-deuterium water direct blending process: Using the same raw materials as in Example 1, but without using the calculation model of this invention, 41.51L of pure 25ppm low-deuterium water was directly added to blend to 53%vol. According to the actual measurement, the deuterium content of the finished aqueous phase was only 34.2ppm, which is seriously deviated from the design target of 50ppm, indicating that the traditional process is difficult to accurately control the deuterium index.

[0026] Comparative Example 2, using a direct separate feeding process without premixing: The raw materials are the same as in Example 1. Low-deuterium water and ordinary water are directly added to the base wine tank. Multiple sampling points in the tank show that the deuterium content is distributed between 30ppm and 58ppm. The wine is severely uneven and the product consistency is poor, indicating that separate feeding will cause the deuterium concentration in the tank to stratify.

[0027] Based on the above-described preferred embodiments of the present invention, and through the foregoing description, those skilled in the art can make various changes and modifications without departing from the inventive concept. The technical scope of this invention is not limited to the contents of the specification, but must be determined according to the scope of the claims.

Claims

1. A method for preparing low-deuterium baijiu (Chinese liquor), characterized in that, include: The alcohol content of high-proof baijiu base liquor, the deuterium concentration of the aqueous phase of the base liquor, the deuterium concentration of low-deuterium blending water, and the deuterium concentration of ordinary blended drinking water are tested, and the target alcohol content and target deuterium concentration of the finished product's aqueous phase are set. The volume of raw materials is calculated based on the deuterium conservation relationship of the whole liquor. The deuterium conservation relationship of the whole liquor is that the sum of the total deuterium in the aqueous phase of the base liquor, the total deuterium in the added low-deuterium blending water, and the total deuterium in the added ordinary blending drinking water equals the total deuterium in the entire aqueous phase of the finished liquor.

2. Based on the aforementioned deuterium conservation relationship of the whole liquor and taking into account the deuterium contribution of the water phase inherent in the base liquor, the volume of low-deuterium blending water and the volume of ordinary blending drinking water to be added are calculated. The calculated volume of deuterium-rich blended water is premixed evenly with ordinary blended drinking water to obtain compound blended water; The compounded water was added to the high-proof liquor base and stirred and mixed. The amount of water added was corrected through small-scale experiments to compensate for the volume shrinkage effect of mixing ethanol and water. The deuterium concentration and alcohol content of the blended liquor were tested in the aqueous phase. When the measured value deviates from the target value, the amount of water to be added is calculated in reverse according to the deuterium conservation relationship of the whole wine, and a small amount of low-deuterium blended water or ordinary blended drinking water is added for fine adjustment; The finely adjusted liquor is filtered and bottled to obtain the low-deuterium baijiu product.

3. The method for preparing low-deuterium baijiu as described in claim 1, characterized in that, The high-proof liquor base is a grain distilled raw liquor prepared by solid-state or liquid-state methods, with an alcohol content of 70%~85% vol. The deuterium concentration of the low-deuterium blended water is 1~130ppm; The ordinary blended drinking water is drinking water that meets the GB5749 standard, with a deuterium concentration of 145~155 ppm; The target alcohol content of the finished product is 30%~65% vol; The target deuterium concentration in the aqueous phase of the finished product is 10~130ppm.

4. The method for preparing low-deuterium baijiu as described in claim 1, characterized in that, The deuterium-rich blended water and ordinary blended drinking water are stirred and mixed in a premixing tank for 15-30 minutes to obtain homogeneous compound blended water.

5. The method for preparing low-deuterium baijiu as described in claim 1, characterized in that, The stirring speed during the mixing process is 30~80 r / min, and the stirring time is 15~45 min; The scale of the small-scale experiment is 5~10L, and the total amount of water added is corrected according to the measured alcohol content of the finished product in the small-scale experiment.

6. The method for preparing low-deuterium baijiu as described in claim 1, characterized in that, After blending, the liquor should be sealed and kept away from light for 7 to 30 days to mature, with the storage environment temperature being 10 to 25℃.

7. The method for preparing low-deuterium baijiu as described in claim 1, characterized in that, When the measured deuterium concentration in the finished product's aqueous phase deviates from the target deuterium concentration by more than ±2 ppm, or when the measured alcohol content exceeds the national standard tolerance range, the volume of low-deuterium blended water or ordinary blended drinking water should be added in reverse calculation based on the aforementioned deuterium conservation relationship of the whole liquor. After adding a small amount, the mixture should be stirred and homogenized until the measured indicators meet the standards.

8. The method for preparing low-deuterium baijiu as described in claim 1, characterized in that, The concentration of deuterium in the aqueous phase was detected by liquid water isotope mass spectrometry or aqueous phase nuclear magnetic resonance (NMR). Before detection, the wine was pretreated by separating the ethanol and aqueous phases.

9. A low-deuterium baijiu (Chinese liquor), characterized in that, The low-deuterium baijiu is prepared by the blending method according to any one of claims 1 to 7, wherein the alcohol content of the low-deuterium baijiu is 30% to 65% vol and the deuterium content in the aqueous phase of the liquor is 10 to 130 ppm.

Images