KR20170036958A - Method for manufacturing distilled alcoholic beverage using pot-continuous complex still - Google Patents

Abstract

The present invention relates to a method for producing distilled alcoholic beverage by using pot-continuous complex still type. The method comprises: an initial stream fraction step of fractionating cooled collected liquid from a start of distillation until a time when content of the cooled collected liquid is 0.5 to 2.0 vol% with respect to volume of total fermented alcoholic beverage; a main stream fraction step of fractionating the cooled collected liquid from right after the initial stream fraction until a time when alcohol concentration of the cooled collected liquid is 45 to 60%; and a final stream fraction step of fractionizing the cooled collected liquid from after the main stream fraction step until a time when the alcohol concentration is 5%. The present invention can produce the distilled alcoholic beverage having excellent taste and flavor while reducing amount of distilled alcoholic beverage wasted as the first stream or the final stream. In addition, the present invention can further reduce toxic substance content of the distilled alcoholic beverage within a standard value.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a distillation column for a distillation column,

The present invention relates to a process for producing a distillation column using a simple-continuous continuous distillation process, and more particularly to a process for producing a distillation column capable of reducing waste of a distillation column to be removed into a stream or a wake, ≪ / RTI >

Distilled liquor refers to a process in which alcohol is fermented by fermenting a raw material and distilling the fermented brew. Since the moisture and alcohol contained in the brewing are different in vaporization temperature depending on the boiling point thereof, a distillation column having desired frequency and flavor can be produced by cooling and recovering the vapor containing alcohol by adjusting the heating temperature and time.

In this method of producing distilled liquor, the recovered liquid containing the alcohol recovered by cooling can be divided into a fresh stream, a mainstream stream and a wake stream. The wastewater is the cooling of the steam recovered in the early stage of distillation. The wake is the cooling of the steam recovered in the latter stage of distillation. The mainstream is the part used as the distillation column and the steam recovered between the wastewater and the wake is cooled.

Generally, the fresh stream has a relatively high methanol content, so it is used to prevent toxicity.

Generally, in the production of distilled liquor, it is important to improve the taste and flavor of distilled liquor by decreasing the harmful substances and improving the productivity by setting the standards of the fresh stream, mainstream and wake differently. However, It is not easy to reduce harmful substances while securing preference for flavor.

In the conventional industrial distilled liquor production method, from the start point of distillation to the point at which 5 wt% of the cooling liquor is produced relative to the weight of the whole distilled liquor, The cooling recovery liquid generated from the time when the concentration becomes less than or equal to the concentration is collectively recognized as a wake and discarded. However, this method not only has a large loss of distillation wastes which are discarded as a fresh stream or a wake, Acetaldehyde, ethyl carbamate and the like can be contained in an amount exceeding an allowable level.

Another conventional method for producing a distilled liquor is Korean Patent Registration No. 10-1272285 (hereinafter referred to as Patent Document 1). In the above Patent Document 1, 30% or more of acetaldehyde is removed by removing the first 1/5 fraction and the wake of the first flow, or removing the first 2/5 fraction and the wake of the first flow to collect the remaining fraction, A manufacturing method of soju has been proposed.

On the other hand, the main hazardous substances that can be included in the distillation column include methanol, acetaldehyde, ethyl carbamate and the like.

Methanol, called methyl alcohol, is a colorless, volatile, flammable, toxic liquid that can cause blindness and death if it is absorbed in large quantities in the body. The boiling point of methanol is 64 ° C, which is lower than the boiling point (78 ° C) of ethanol, which is the main component of alcohol, and is contained in a large amount in the flow.

Acetaldehyde is a kind of aldehyde compound that exists as a colorless liquid, formed during the metabolism of ethanol, and is a substance that causes hangover such as vomiting and headache. The boiling point of acetaldehyde is 22 ° C, which is lower than the boiling point of ethanol (78 ° C) and contained in large amounts in the flow.

Ethyl carbamate is a naturally occurring toxic substance during food storage and aging processes and has recently been classified as a human carcinogen (IARC carcinogen grade 2A). In addition, ethyl carbamate is produced by reacting precursor materials such as hydrocyanic acid, urea, citrulline, cyanoglycoside and N-carbamyl compound with ethanol, and it is difficult to reduce the generation amount or to predict the generation behavior during distillation, It is important to lower its content.

One object of the present invention is to provide a distillation column which can reduce the amount of distillation liquor to be discarded as a fresh stream or a wake but at the same time has excellent taste and flavor and can further reduce the content of harmful substances within a standard value. And a method for producing the same.

One embodiment of the present invention is a method for producing a distilled liquor in which a fermentation liquor is distilled using a simplex-continuous multiple distillation method, wherein a time point at which the content of the cooling liquor after the start of the distillation reaches 0.5 to 2.0 vol% A fresh-flow fractionation step of fractionating the cooling-recovered liquid from A main fractionation step of fractionating the cooling recovery solution from the point immediately after the ultrafiltration step to the point when the alcohol concentration in the cooling recovery solution reaches 45% to 60%; And a wake fractionation step of fractionating the cooling recovery liquid from the main fractionation step to the point at which the alcohol concentration reaches 5%. The present invention also relates to a method for producing a distillation column using the single-continuous multiple distillation method.

In the method for producing a distilled liquor using the single-continuous multiple distillation method, the cooling recovery liquid fractionated in the ultrafiltration step may be discarded, and the cooling recovery liquid fractionated in the downstream fractionation step may be refluxed by distillation .

The mainstream fractionation step may include filtering the fractionated cooling liquor with at least one of a ceramic filter, a porous filter, and a food filtration charcoal.

The single-stage continuous distillation system may be a distillation apparatus including a single distillation apparatus and a continuous distillation apparatus.

The distillation apparatus may further comprise a copper catalytic converter.

The copper catalytic converter may comprise at least one of a filter coated with copper on its surface, a copper fiber or a copper woven.

The fermented beverage may be cereal or fruit juice.

The present invention relates to a method for producing a distillation stock using a single-continuous multiple distillation method which can reduce the amount of distilled liquor to be discarded as a fresh stream or a wake, while at the same time having an excellent taste and flavor and further reducing the content of the derived material within a standard value .

1 is a manufacturing process diagram of a manufacturing method of the present invention.
2 is a photograph of a single-continuous composite still used in Example 1 of the present invention.
3 is a photograph of the copper catalyst conversion apparatus used in Example 2 of the present invention.
4 is a graph showing the results of alcohol concentration analysis for Example 1. FIG.
5 is a graph showing the results of ethyl carbamate analysis for Example 1. Fig.
6 is a graph showing the analysis result of the low-boiling point hazardous substance in Example 1. FIG.
7 is a graph showing the results of alcohol concentration analysis for Example 2. Fig.
8 is a graph showing the results of ethyl carbamate analysis for Example 2. Fig.
FIG. 9 is a graph showing the analysis result of the low-boiling point hazardous substance according to Example 2. FIG.
10 is a graph showing the results of alcohol concentration analysis for Example 3. Fig.
11 is a graph showing the results of ethyl carbamate analysis for Example 3. Fig.

The method for producing a distilled liquor of the present invention uses a single-continuous complex distillation method. A flow chart of such a distillate production method is illustrated in FIG.

As used herein, the term " alcohol " used in expressing the "alcohol concentration" For example, "alcohol" includes ethanol as the main component, and may be an alcohol mixture that does not contain methanol. In this specification, methanol is a toxic substance requiring reduction of its content, and its content is separately measured and indicated.

In the present specification, the single-continuous complex distillation system means that the fermentation distillate is distilled using a single-stage continuous distillation apparatus including a single distiller and a continuous distiller at the time of distillation. A photograph of a single-continuous continuous distillation apparatus comprising an exemplary single distillation apparatus and a continuous distillation apparatus used in the present invention is shown in FIG.

The single distiller is a distiller designed to distill the fermentation broth and acquire the cooling recovery solution. The distillation column is firstly distilled and then the recovered distillation column is second distilled to obtain a distillation column having a desired alcohol content. These single distillers enhance the original flavor of the raw material.

The continuous distiller is a still that is designed to continuously feed the fermentation broth to distiller at the time of distillation and to obtain a cooling recovery solution by fractional distillation through a multi-stage layer formed therein. Such a continuous distiller has an excellent effect of increasing the alcohol content of the distillation column.

The single-continuous continuous distillation system of the present invention using the single distiller and the continuous distiller in combination, not only improves the taste and flavor of the distilled liquor through the single distillation but also provides a high concentration of alcohol It is possible to obtain a cooling recovery liquid having a low temperature. In this case, it is possible to omit the process of repeating the redistillation in order to realize the alcohol concentration of the distilled liquor at a high concentration, and the effect of preserving the taste and flavor lost in re-distillation is excellent.

The distiller may be a stainless steel still, a copper distiller, a shochu ring made of earthenware, or the like depending on the material. In the case of using the middle distillation still, the distillation temperature can be controlled more advantageously, and the distillation accuracy can be further improved, and the effect of adsorbing harmful substances and adsorbing offensive substances can be excellent.

The single-stage continuous distillation apparatus may further include a copper catalytic converter. In this case, the effect of improving the taste and flavor of the distillation column by the single-continuous continuous distillation method of the present invention is more excellent, and the effect of reducing harmful substances can be further excellently applied.

The copper catalytic converter may include, for example, a filter coated with copper on its surface, a woven fabric made of copper fiber or copper wire, and the like. Such a copper catalytic converter can bind to or adsorb a sulfur compound or an ethyl carbamate precursor that generates odor, and can inhibit the production of ethyl carbamate which is a harmful substance.

The above-mentioned single-continuous complex distillation process can be performed by an atmospheric distillation process, and can be performed by a direct heating process or an indirect heating process. In this case, the effect of preventing loss of flavor caused by distillation can be further improved.

The fermented beverage may be cereal or fruit juice. In this case, the effect of improving the taste and flavor during the production of the distilled liquor by the single-continuous multiple distillation method of the present invention is excellent and the effect of reducing harmful substances can be further excellently applied.

The method for producing the fermented beverage is not particularly limited. For example, the fermented bean curd can be prepared by washing cereal grains and immersing them in water, removing water from the grains, fermenting them with yeast, enzymes and water. As another example, fruit juices can be prepared by washing fruit, removing the wash water and non-edible parts, crushing and fermenting with potassium sulfite and yeast.

Hereinafter, each step of the method for producing a distillate of the present invention will be described in more detail.

One embodiment of the present invention is a method for producing a distilled liquor in which a fermentation liquor is distilled using a simplex-continuous multiple distillation method, wherein a time point at which the content of the cooling liquor after the start of the distillation reaches 0.5 to 2.0 vol% A fresh-flow fractionation step of fractionating the cooling-recovered liquid from A main fractionation step of fractionating the cooling recovery solution from the point immediately after the ultrafiltration step to the point when the alcohol concentration in the cooling recovery solution reaches 45% to 60%; And a wax fractionation step of fractionating the cooling recovery liquid from the main fractionation stage to the point when the alcohol concentration reaches 5%; To a process for producing a distillation column using a simple-continuous multiple distillation process.

First, in this specification, the point in time when the fermentation broth is put into the distillation apparatus and the heating is started is regarded as the starting point of the distillation. In addition, the vapor produced after the start of distillation is separately separated and then cooled down to be liquefied is regarded as a fraction of the cooling recovery liquid.

The supernatant fraction is fractionated by distillation until the content of the cooling recovered fraction from the beginning of distillation reaches 0.5 to 2.0 vol% of the volume of the whole fermentation stock. Hereinafter, the cooling recovery liquid fractionated through this step will be referred to as " super concentrate ".

When the content of the edible meats is less than 0.5% by volume relative to the weight of the fermented beverage, the distilled beverage has a very high content of toxic methanol, and the content of low boiling point harmful substances such as methanol and acetaldehyde exceeds the standard of commercial distilled beverage, . On the other hand, when the content of the edible meats is more than 2.0% by volume of the fermentation broth, the productivity of the distilled liquor is deteriorated, and the taste and flavor are lowered.

The fractionation time of the edible stream may be, for example, from 0.5% by volume to 2.0% by volume or from 1.0% by volume to 2.0% by volume. Within the above-mentioned range, the productivity of the final product and the quality of the distillate can both be improved, and the effect of reducing methanol and low-boiling point harmful substances can be further improved.

In the mainstream fractionation step, the cooling recovery liquid is fractionated from immediately after the supernatant fractionation to the point where the alcohol concentration of the cooling recovery liquid reaches 45% to 60%. Hereinafter, the cooling recovery liquid fractionated through this step will be referred to as mainstream.

When the main alcohol is fractionated at an alcohol concentration of less than 45%, the content of ethyl carbide contained in the distillation column may be increased. On the other hand, when the main alcohol is fractionated at an alcohol concentration of more than 60%, the productivity of the distilled liquor is deteriorated, and the taste and flavor are lowered.

The time point of fractionation of the main stream may be, for example, 45% to 60%, 45% to 55% or 45% to 50%. Within the above-mentioned range, the productivity of the final product and the quality of the distillate can both be improved, and the effect of reducing methanol and low-boiling point harmful substances can be further improved.

In addition, the mainstream fractionation step may further include filtering the mainstream during the fractionation. At this time, the mainstream filtration can be performed by a ceramic filter, a porous filter, and a food filtration charcoal. In this case, the copper recovering solution, which is partially contained in the copper distillation unit or the copper catalytic converter, can be filtered through adsorption. In this case, the effect of reducing harmful low-boiling point substances is further improved, and the flavor of the mainstream can be improved.

In the wake fractionation step, the cooling recovery liquid from the main fractionation stage to the point where the alcohol concentration reaches 5% is fractionated. The cooling recovery liquid fractionated through this step is hereinafter referred to as a wake.

When the alcohol concentration in the downstream is less than 5%, the number of the distillation columns is low, which is not only economical for producing the desired number of distillation columns, but also can lead to odors such as tanks.

In the method for producing a distilled liquor using the single-continuous multiple distillation method, the cooling recovery liquid fractionated in the ultrafiltration step may be discarded, and the cooling recovery liquid fractionated in the downstream fractionation step may be refluxed by distillation . In this case, the productivity of distilled water can be further improved while effectively removing toxic methanol and low-boiling point harmful substances contained in the distillate.

For example, when the distillation column manufactured by the above-described method of producing a distillation column using the single-continuous multiple distillation method of the present invention is processed into a final product having an alcohol content of 40%, for example, the methanol content is 10 ppm or less, the acetaldehyde content May be implemented at 2.5 ppm or less. At the same time, the final product can be produced in an excellent range of 5.5 L or more. In this case, high-quality spirits with high taste and flavor as well as preventing hangover particularly induced in cereal or fruit wine can be produced with excellent productivity.

< Example >

Hereinafter, the configuration and operation of the present invention will be described in more detail with reference to preferred embodiments of the present invention. It is to be understood, however, that the same is by way of illustration and example only and is not to be construed in a limiting sense. The contents not described here are sufficiently technically inferior to those skilled in the art, and a description thereof will be omitted.

Example  One

The fermentation broth made from rice was distilled with a single-continuous complex distillation apparatus including a copper catalytic converter. At this time, the cooling recovered from the start of the distillation to the time when the volume ratio of the cooling solution to the total fermentation solution became 1 volume% was fractionated into the supernatant. The cooling recovery liquid generated until the alcohol concentration of the cooling recovery liquid became 50% immediately after the fractionation of the supernatant was fractionated into mainstream. From the fractionation of the mainstream, the cooling recovery liquid generated until the alcohol concentration of the cooling recovery liquid became 5% was fractionated into a wake.

For the analysis, the cooling and recovering liquids of the fresh, mainstream and downstream wafers fractionated in Example 1 were classified by 1 volume% based on the total volume of the fermented liquor added at the time of distillation, and the sample number was given according to the order of the obtained Respectively. Alcohol concentration, acetalate content, methanol content and ethyl carbamate content were measured for each sample by the following analytical method. The results are shown in Table 1 below.

<Analysis method>

1) Analysis of methanol and acetaldehyde

Each sample was filtered with 0.45 μm membrane filter and 0.22 μm membrane filter and quantified with gas chromatography (Agilent, 7890A). 1 μl of sample was injected into a DB-WAX column (30m × 0.25mm Id, 0.25μm), and the detector was maintained at FID, injector temperature of 200 ° C, detector temperature of 200 ° C, column oven temperature of 45 ° C for 1 minute, And the mixture was allowed to stand at 130 ° C for 1 minute, and nitrogen was used as a carrier gas. Quantitation was calculated by comparing the area of the chromatogram of the standard material.

2) Analysis of ethyl carbamate

Each sample was filtered with 0.45 μm membrane filter and 0.22 μm membrane filter and analyzed by gas chromatography mass spectrometry (Agilent, 5975C). 1 μl of sample was injected into a DB-WAX column (30 m × 0.25 mm Id, 0.25 μm). The detector was kept at FID, MS transfer line temperature of 250 ° C., inlet temperature of 210 ° C., column oven temperature of 50 ° C. for 1 minute, The temperature was raised by 7 ℃ and the temperature was kept at 180 ℃ for 1 minute. Helium was used as a carrier gas. Quantitation was calculated by comparing the area of the chromatogram of the standard material.

3) Measurement of alcohol cumulative distillation ratio (%)

The cumulative distillation rate of alcohol is calculated by dividing the cumulative alcohol content of the sample by the total alcohol content. At this time, the alcohol content of the sample is calculated by multiplying the alcohol concentration by the weight of the sample.

sample
number Alcohol Acetaldehyde Methanol Ethyl carbamate Measures
(v / v%) accumulate
distillation
ratio
(%) Measures
(ppm) importance
(%) Measures
(ppm) importance
(%) Measures
(ppb) importance
(%) Fresh stream One 68.70 4.35 86.46 61.06 168.03 52.02 126.57 39.92 Mainstream 2 78.20 9.30 23.35 17.90 69.05 21.38 190.47 60.08 3 78.40 14.26 8.05 5.69 34.74 10.76 0.00 0.00 4 79.60 19.30 4.34 3.06 5.54 1.71 0.00 0.00 5 81.00 24.42 2.46 1.74 3.31 1.03 0.00 0.00 6 82.10 29.62 1.79 1.27 2.92 0.90 0.00 0.00 7 82.80 34.86 1.16 0.82 2.67 0.83 0.00 0.00 8 83.00 40.11 0.88 0.62 2.53 0.78 0.00 0.00 9 83.10 45.37 0.63 0.45 2.35 0.73 0.00 0.00 10 83.20 50.63 0.63 0.45 2.38 0.74 0.00 0.00 11 83.00 55.89 0.50 0.36 4.27 1.32 0.00 0.00 12 82.60 61.11 0.29 0.20 2.65 0.82 0.00 0.00 13 82.00 66.30 0.41 0.29 2.72 0.84 0.00 0.00 14 80.70 71.41 0.56 0.39 3.04 0.94 0.00 0.00 15 78.50 76.38 0.62 0.44 3.59 1.11 0.00 0.00 16 74.40 81.08 0.60 0.42 3.60 1.12 0.00 0.00 17 66.50 85.29 0.67 0.47 3.06 0.95 0.00 0.00 18 55.50 88.81 0.58 0.41 2.32 0.72 0.00 0.00 Wake 19 43.80 91.58 1.07 0.75 2.46 0.76 0.00 0.00 20 33.30 93.68 0.57 0.40 1.76 0.54 0.00 0.00 21 26.90 95.39 0.39 0.27 0.00 0.00 0.00 0.00 22 25.80 97.02 0.39 0.27 0.00 0.00 0.00 0.00 23 23.80 98.53 0.94 0.67 0.00 0.00 0.00 0.00 24 10.80 99.21 0.67 0.47 0.00 0.00 0.00 0.00 25 7.40 99.68 0.97 0.68 0.00 0.00 0.00 0.00 26 5.10 100.00 0.63 0.45 0.00 0.00 0.00 0.00

(The results of the above Table 1 are shown graphically in FIG. 4 to FIG. 6. Specifically, the alcohol concentration analysis result is shown in FIG. 4, the ethyl carbamate and urea analysis results are shown in FIG. 5, the low boiling point harmful substances including methanol and acetaldehyde The results of the analysis are shown in Fig.

As can be seen from Table 1, the distillate production method of Example 1 has the effect of removing 52.02% by weight of methanol, 61.06% by weight of acetaldehyde and 39.92% by weight of ethyl carbamate through the fractions of the fresh stream, % Alcohol distillation ratio. In addition, the distillate production method of Example 1 achieves an 84.46% alcohol cumulative distillation rate through the fraction of the main stream to obtain a high yield of distillate with a high alcohol content while a wake having a cumulative distillation rate of 11.19% It was possible to further improve the taste and flavor of the product.

Example  2

The fermented wine made from red grapes was distilled by a single-continuous complex distillation apparatus including a copper catalytic converter. At this time, the cooling recovery liquid generated until the volume ratio of the cooling solution to the total fermentation solution after the start of the distillation reached 1 vol% was fractionated into the supernatant. The cooling recovery liquid generated from immediately after fractionation of the supernatant to the point when the alcohol concentration of the cooling recovery liquid became 60% was fractionated into mainstream. From the fractionation of the mainstream, the cooling recovery liquid generated until the alcohol concentration of the cooling recovery liquid became 5% was fractionated into a wake.

For the analysis, the cooling and recovering solutions of the fresh, mainstream and downstream wafers fractionated in Example 2 were classified according to the volume of 1 volume% of the total volume of the fermented beans fed at the time of distillation, and the samples were numbered according to the obtained order Respectively. Alcohol concentration, acetaldehyde content, methanol content and ethyl carbamate content were measured for each sample using the above-described analytical method. The results are shown in Table 2 below.

sample
number Alcohol content Acetaldehyde Methanol Ethyl carbamate Measures
(v / v%) accumulate
distillation
ratio
(%) Measures
(ppm) importance
(%) Measures
(ppm) importance
(%) Measures
(ppb) importance
(%) Fresh stream One 80.11 5.48 21.39 18.52 128.34 26.84 0.00 0.00 Mainstream 2 83.24 11.18 15.06 13.04 80.38 16.81 0.00 0.00 3 84.72 16.97 11.07 9.58 63.21 13.22 0.00 0.00 4 85.81 22.84 8.56 7.41 25.37 5.31 0.00 0.00 5 86.52 28.76 6.78 5.87 21.08 4.41 0.00 0.00 6 86.88 34.71 5.06 4.38 17.69 3.70 0.00 0.00 7 87.02 40.66 4.18 3.62 15.10 3.16 0.00 0.00 8 87.04 46.61 3.39 2.93 13.62 2.85 0.00 0.00 9 86.98 52.57 2.97 2.57 13.78 2.88 0.00 0.00 10 86.84 58.51 3.04 2.63 12.33 2.58 0.00 0.00 11 86.51 64.43 1.55 1.35 10.76 2.25 0.00 0.00 12 85.91 70.30 1.48 1.29 9.86 2.06 0.00 0.00 13 85.05 76.12 3.57 3.09 9.75 2.04 24.32 31.59 14 83.60 81.84 4.48 3.88 9.95 2.08 27.34 35.52 15 80.38 87.34 5.52 4.78 10.84 2.27 9.09 11.81 16 62.23 91.60 6.80 5.89 10.18 2.13 0.00 0.00 Wake 17 38.75 94.25 4.43 3.84 7.69 1.61 0.00 0.00 18 27.52 96.13 2.46 2.13 5.09 1.06 0.00 0.00 19 19.29 97.45 1.72 1.49 4.05 0.85 0.00 0.00 20 14.56 98.45 0.46 0.40 3.26 0.68 0.00 0.00 21 11.00 99.20 0.39 0.34 2.70 0.56 14.17 18.40 22 6.72 99.66 0.67 0.58 1.77 0.37 2.06 2.67 23 4.96 100.00 0.46 0.40 1.38 0.29 0.00 0.00

(The results of the above Table 2 are shown graphically in Figs. 7 to 9. Specifically, the alcohol concentration analysis results are shown in Fig. 7, the ethyl carbamate and urea analysis results are shown in Fig. 8, the low boiling point harmful substances including methanol and acetaldehyde The results of the analysis are shown in Fig.

As can be seen from Table 2, the distillate production method of Example 2 has the effect of removing the specific gravity of 26.84% of methanol and the specific gravity of 18.52% of acetaldehyde through the fraction of the supernatant, while at the same time the alcohol loss is 5.48% . In addition, the distillate production method of Example 2 achieves a high yield of distillate with a high alcohol content by achieving a cumulative distillation rate of 86.12% alcohol through the fraction of the main stream, while the wake having a distillation ratio of 8.04% And the flavor could be further improved.

Example  3

The same procedure as in Example 2 was carried out except that the fermentation broth was distilled with a single-continuous complex distillation apparatus not containing a copper catalytic converter.

For the analysis, the cooling and recovering solutions of the fresh, mainstream and downstream wafers fractionated in Example 3 were classified by 1 volume% based on the total volume of the fermented stocks fed at the time of distillation, and the sample numbers were assigned according to the order of the obtained Respectively. Alcohol concentration and ethyl carbamate content were measured for each sample using the above-described analytical method. The results are shown in Table 3 below.

Fraction
No. Example 3 Alcohol cumulative distillation rate
(v / v%) Ethyl carbamate
(ppb) Fresh stream One 82.28 71.50 Mainstream 2 84.53 68.65 3 86.62 10.97 4 87.53 14.16 5 87.97 33.85 6 88.07 44.44 7 87.99 42.48 8 87.80 87.27 9 87.63 129.66 10 87.27 178.26 11 86.63 195.12 12 85.68 231.27 13 83.90 248.27 14 80.47 262.22 15 71.46 262.26 16 54.05 268.27 Wake 17 38.99 280.24 18 28.81 290.27 19 21.50 50.24 20 15.76 48.00 21 11.38 26.17 22 8.80 16.90 23 6.88 17.10

(The results of Table 3 are shown graphically in FIG. 10 to FIG. 11. Specifically, the alcohol concentration analysis results are shown in FIG. 10, and the ethyl carbamate and urea analysis results are shown in FIG.

Example  4

A fermentation broth containing rice as a raw material was fractionated in the same manner as in Example 1, and a final product having an alcohol content of 40%, such as general whiskey or brandy, was prepared using the mainstream. The alcohol concentration, the methanol content and the ethyl carbamate content of the final product of Example 4 were measured and shown in Table 4.

Example  5

The same procedure was followed as in Example 1, except that the rice bran was fractionated in the same manner as in Example 1, except that the breaking point (fractionation time) of the fresh-cut was changed to 2 vol%. The alcohol content was 40% &Lt; / RTI &gt; The alcohol concentration, methanol content and ethyl carbamate content of the final product of Example 5 were measured and are shown in Table 4.

Comparative Example  One

The same procedure was followed as in Example 1, except that the rice bran was fractionated in the same manner as in Example 1, except that the breaking point (fractioning point) was changed to 0 vol%. The alcohol content was 40% &Lt; / RTI &gt; The alcohol concentration, the methanol content and the ethyl carbamate content of the final product of Comparative Example 6 were measured and shown in Table 4.

Comparative Example  2

The same procedure was followed as in Example 1, except that the fresh-broke fermentation broth was fractionated using the same method except that the fresh-broke point (fractionation time) of Example 1 was changed to 3 vol%, and the alcohol content was 40% &Lt; / RTI &gt; The alcohol concentration, the methanol content and the ethyl carbamate content of the final product of Comparative Example 2 were measured and shown in Table 4.

Breaking Point Acetaldehyde
(ppm) Methanol
(ppm) Ethyl Carbamate
(ppb) Final product output Example 4 1 volume% 1.73 5.23 6.50 5.86L Example 5 2 volume% 0.91 3.05 0.00 5.53L Comparative Example 1 0 volume% 4.46 10.45 10.31 6.15L Comparative Example 2 3 volume% 0.66 1.90 0.00 5.19L

As can be seen from Table 4, the final product having an alcohol content of 40% produced by the distillate production method of Examples 4 to 5 had methanol content of less than 6 ppm and acetaldehyde content of less than 2 ppm, But the final product yield was superior to 5.5L. On the other hand, the final product having an alcohol content of 40% produced through the distillate production process of Comparative Example 1 had a methanol content exceeding 10 ppm and an acetaldehyde content exceeding 4 ppm, And inhibited alcohol metabolism, indicating that the quality as a mainstream was not excellent. In addition, it was found that the productivity of Comparative Example 2 was not excellent because the final product yield was less than 5.5 L.

Example  6

A final product having an alcohol content of 40%, such as general whiskey or brandy, was prepared by fractionating the red wine using the red wine as a raw material in the same manner as in Example 2. The alcohol concentration, methanol content, acetaldehyde content and ethyl carbamate content of the final product of Example 6 were measured and shown in Table 5.

Example  7

A fermentation broth having red grapes as a raw material was fractionated by the same method as that of Example 3 (using a copper composite still), and then a final product having an alcohol content of 40%, such as general whiskey or brandy, was prepared using the mainstream. The alcohol concentration, the methanol content, the acetaldehyde content and the ethyl carbamate content of the final product of Example 7 were measured and shown in Table 5.

Comparative Example  3

A final product having an alcohol content of 40% was prepared in the same manner as in Example 6, except that a single distillation method in which a fermentation product was indirectly heated using a copper distiller was used. The alcohol concentration, the methanol content and the ethyl carbamate content of the final product of Comparative Example 3 were measured and shown in Table 5.

Comparative Example  4

A final product having an alcohol content of 40% was prepared in the same manner as in Example 6, except that the single distillation method in which the distillation was directly heated by using a distiller was used in the production process of the fermented beverage. The alcohol concentration, the methanol content and the ethyl carbamate content of the final product of Comparative Example 3 were measured and shown in Table 5.

Alcohol (V / V%)  Content of alcohol (%) Acetaldehyde (ppm) Methanol
(ppm) urea
(ppb) Ethyl carbamate
(ppb) Example 6 80.95 83.07 2.40 8.27 0.59 2.00 Example 7 73.56 40.09 2.39 9.92 11.62 130.91 Comparative Example 3 59.66 49.72 2.53 9.76 1.98 0.32 Comparative Example 4 58.66 47.43 2.96 9.50 1.72 31.81

(% Of the alcohol in Table 5 = the coefficient of the mainstream / the coefficient of the total sample)

<Notation>

This research was conducted by the Ministry of Agriculture, Forestry and Livestock Food and Beverage, and the Ministry of Agriculture, Food and Rural Affairs.

Claims (7)

A method for producing a distilled liquor in which a fermentation liquor is distilled using a simplex-continuous multiple distillation system,
A fresh stream fractionation step of fractionating a cooling recovery liquid from the start of distillation to a point of time when the content of the cooling recovery liquid becomes 0.5 volume% to 2.0 volume% of the volume of the entire fermentation stock;
A main fractionation step of fractionating the cooling recovery solution from the point immediately after the ultrafiltration step to the point when the alcohol concentration in the cooling recovery solution reaches 45% to 60%; And
And a wake fractionation step of fractionating the cooling recovery liquid from the main fractionation step to the point when the alcohol concentration reaches 5%.
The method according to claim 1, wherein the cooling recovery liquid fractionated in the ultrafiltration step is discarded, and the cooling recovery liquid fractionated in the downstream fractionation step is refluxed by a distiller and re-distilled. Gt;
The method according to claim 1, wherein the main fractionation step comprises filtering the fractionated cooling solution with at least one of a ceramic filter, a porous filter, and a charcoal for food filtration.
The method according to claim 1, wherein the single-continuous multiple distillation system uses a distillation apparatus including a single distillation apparatus and a continuous distillation apparatus.
5. The method of claim 4, wherein the distillation apparatus further comprises a copper catalytic converter.
6. The method of claim 5, wherein the copper catalyst conversion apparatus comprises at least one of a copper coated surface, a copper fiber or a copper woven fabric.
[Claim 3] The method according to claim 1, wherein the fermentation liquor is cereal or fruit wine.

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