KR101272285B1 - Method for preparing distilled soju with improved flavor characteristics - Google Patents

Abstract

PURPOSE: A method for manufacturing soju with excellent taste and flavor is provided to maintain main flavor and taste by reducing acetaldehyde by 30% or more. CONSTITUTION: A method for manufacturing soju by fermenting ingredients and multi-stage distillation comprises: a step of distilling a fermented liquid at normal pressure; a step of refluxing and re-distilling the distilled soju liquid and separating the liquid into head, medium and tail; and a step of removing 1/5 fraction of the head and the tail, initial 2/5 fraction of the head and the tail, and collecting residual liquid. The soju contains acetaldehyde which is reduced by 30% or more and improved flavor and taste. The ingredient of soju is rice or barley. The multi-stage distillation is performed using 15 stage-type-distiller. [Reference numerals] (AA) Coolant outlet; (BB) Coolant inlet

Description

Method for preparing distilled soju with excellent flavor characteristics {METHOD FOR PREPARING DISTILLED SOJU WITH IMPROVED FLAVOR CHARACTERISTICS}

The present invention relates to a method for preparing distilled shochu, and more particularly, to a method for preparing distilled shochu having excellent flavor characteristics prepared by combining fractions obtained through atmospheric reflux.

Distilled liquor with relatively high alcohol content can be divided into distilled liquor, whiskey, liqueur and general distilled liquor. Representative shochu is divided into two kinds of distilled shochu and distilled shochu. The most popular distilled shochu is prepared by diluting alcohol with over 95% by weight of alcohol with water, and then adding sweetener and acidulant. It is prepared by distillation. Distilled shochu is rich in flavors such as acetaldehyde, fusel oil, furfural and other unique ingredients. Can be.

Most distilled shochus on the market are focused on eliminating flavors and giving them a refreshing taste.However, consumers' demand for flavors derived from the raw materials themselves continues, so manufacturers are trying to develop shochus with excellent flavors. Continues. However, since there are many acetaldehydes that are the main causes of hangover in the flavor components, it is very difficult to simultaneously achieve two tasks of increasing the flavor component and decreasing the hangover component.

Accordingly, the present invention provides a method for preparing distilled shochu with a significant reduction in acetaldehyde, which is a major cause of hangover, and an increased flavor component.

In order to achieve the above object, the present invention is a method of producing a distilled shochu by fermenting the raw material of soju in a multi-stage re-distillation method, (1) by distillation of the distillate distilled at atmospheric pressure distillation of the fermentation broth at atmospheric pressure reflux (head) ), Separating into medium and tail; And (2) removing the first 1/5 fraction and wake of the herb in the aliquot, or removing the first 2/5 fraction and wake of the herb to collect the remaining fractions, wherein at least 30% of acetaldehyde is removed and flavored. Provides an improved method of preparing distilled shochu.

Through the production method of the present invention, while main acetaldehyde, which is a major cause of hangover, is reduced by 30% or more, the main flavor component is maintained, so that distilled soju having excellent flavor characteristics can be prepared, which is very useful in the liquor industry.

1 is a schematic diagram of a multi-stage still used in the present invention.
Figure 2 is a graph showing the alcohol concentration by fraction according to various re-distillation methods.
3 is a graph showing the change of acetaldehyde concentration according to various re-distillation method.
Figure 4 is a graph showing the change in the concentration of ethyl acetate according to the various distillation method.
5 is a graph showing a change in concentration of n-propanol according to various re-distillation methods.
6 is a graph showing the change in concentration of i-butanol according to various re-distillation methods.
7 is a graph showing a change in concentration of i-amyl alcohol according to various re-distillation methods.
8 is a graph showing a change in concentration of i-amyl acetate according to various re-distillation methods.
9 is a graph showing the concentration change of ethyl lactate according to various re-distillation methods.
10 is a graph showing the change in concentration of ethyl caproate according to various re-distillation methods.
11 is a graph showing the concentration change of ethyl caprylate according to various re-distillation methods.
12 is a graph showing the change in concentration of ethyl caprate according to various re-distillation method.
13 is a graph showing the change in concentration of 2-phenylethanol according to various re-distillation methods.
14 is a graph showing a change in concentration of 2-phenylethyl acetate according to various redistillation methods.

The present invention is a method of producing a distilled shochu by fermenting the raw material of soju by a multi-stage re-distillation method, (1) at a reflux distillation of the distillate distilled at atmospheric pressure distillation of the fermentation broth at atmospheric pressure reflux (head), medium (medium) And separating into a tail; And (2) removing the first 1/5 fraction and wake of the herb in the aliquot, or removing the first 2/5 fraction and wake of the herb to collect the remaining fractions, wherein at least 30% of acetaldehyde is removed and flavored. Provides an improved method of preparing distilled shochu.

In the method of the present invention, as a raw material that can be used as a raw material of shochu is not particularly limited as a raw material commonly used in the art, rice or barley is preferred. The method of the present invention is characterized in that the fermentation broth obtained by fermenting the raw material of soju is first distilled and then the fraction obtained by re-distillation is combined. Fermentation of the raw material may be carried out by a method commonly used in the art. One feature of the present invention is the primary distillation of the fermentation broth under atmospheric pressure. Typically distillation can be carried out under atmospheric pressure or reduced pressure, the atmospheric pressure means a normal atmospheric pressure and the reduced pressure means a pressure section represented by 0 ~ -760 mmHg, preferably a pressure of -760 to -500 mmHg. Currently commercial distilled soju is produced under reduced pressure in order to produce a product with low productivity and less blemish components, but the method of the present invention has an advantage of obtaining many flavor components by primary distillation under normal pressure. Another feature of the present invention is that the primary distilled distillate is distilled under atmospheric pressure reflux and separated into a head, a medium, and a tail. Whereas conventional distilled liquor re-distillates under reduced pressure, the present invention is characterized by re-distilling under normal pressure and introducing reflux upon re-distillation. In order to concentrate acetaldehyde and huesel oil (such as n-propanol, i-butanol or i-isoamyl alcohol) to the downstream, the distillation is carried out using a 15-stage multi-stage distillator with three 5-stage columns. It is preferably carried out by, but any type of distillation machine can be used as long as it is a multi-stage distillation machine capable of achieving the above object.

The reflux reflux distillation used in the production method of the present invention may be carried out under normal pressure, thereby obtaining many times more flavor components than the reduced pressure. However, in the case of atmospheric distillation, there is a high possibility that raw material odor or coal is generated in addition to the flavor component compared to the reduced pressure, which may be caused to flow out to the first or the downstream through reflux distillation through a multi-stage distillation unit. Distilled shochu with excellent flavor can be produced by eliminating raw odor, coal and the like. The atmospheric reflux distillation may be performed under reflux ratio 4: 1 (eg, Reflux 40 seconds: Receiver 10 seconds, etc.), but is not limited thereto.

As used herein, the term "head" refers to a fraction from the beginning of distillation to a distillation ratio of 7 ± 0.5%, and the term "medium" refers to a distillation ratio of 7 ± 0.5% to 94 ± 0.5%. Fractions, and the term "tail" means fractions that flow out after 94 ± 0.5%.

In step 1 of the method of the present invention, the distilled liquor obtained by atmospheric distillation of the fermentation broth is separated into an initial stream, a middle stream and a downstream stream through atmospheric reflux distillation.

Step 2 of the method of the present invention is the step of combining the above-mentioned first, middle and downstream to reduce acetaldehyde, and to prepare a soju excellent in flavor characteristics. Each fraction obtained in step 1 has a higher content of flavor components than the conventional distilled soju, and particularly shows the tendency of acetaldehyde, which is the main cause of hangover, to concentrate in the first and second streams. When the fraction of the obtained supernatant is finely divided, the first 20 mL fraction of the herbaceous acid (50 mL total), that is, 2/5, contains at least 34% of the total acetaldehyde, and the first 10 mL fraction, that is, 1/5 fraction 22% is included. In the downstream, about 9% of the total acetaldehyde is concentrated. Thus, by removing the first 2/5 fractions and wakes in the stream, at least 40% of the total acetaldehyde can be removed, and by removing the first 1/5 fractions and wakes in the stream, at least 30% of the total acetaldehyde can be removed. have.

Distilled shochu prepared according to the method of the present invention can obtain a number of flavor components through atmospheric reflux distillation, excellent flavor characteristics, remove the first 1/5 fractions and the wake of the first or second of the first By eliminating fractions and wakes, problems with hangovers can be significantly reduced.

Hereinafter, the present invention will be described in detail by way of examples.

However, the following examples are illustrative of the present invention, and the present invention is not limited to the following examples.

Example  1: of rice Atmospheric pressure  Distillate Atmospheric Reflux Distillation

In 2011, the Hite Jinro Co., Ltd. Icheon plant fermented rice as a raw material and distilled at atmospheric pressure using a pilot atmospheric distillation unit to obtain a distilled stock solution. At this time, the alcohol concentration was cut at 20%. The distillate stock was redistilled at atmospheric pressure using a multistage distillator (FIG. 1) with three 5-stage columns having a vacuum jacket coated with silver. The initial setting of the capacitor was 2 ° C. (temperature rose to 10 ° C. as the distillation proceeded) and cooling water was used. In order to find out the effect of reflux during the re-distillation, reflux was introduced by setting a device capable of automatically adjusting the reflux and reflux ratio. At this time, the reflux ratio was set to 4: 1 (Reflux 40 seconds: Receiver 10 seconds). 50 mL of the re-distilled fractions were recovered.

Example  2: barley Atmospheric distillation Atmospheric Reflux  Re-distillation

In Example 1, barley was used instead of rice as a raw material, except that the alcohol concentration of the distillate was cut at 45%, the procedure of Example 1 was repeated to recover an aliquot by 50 mL.

Comparative example  1: of rice Atmospheric distillation  Atmospheric Red Distillation Unreflected )

In Example 1, 50 mL aliquots were recovered by re-distillation without using reflux.

Comparative example  2: reduced pressure distillation of rice Reduced pressure reflux distillation

After distilling at atmospheric pressure in Example 1, instead of reflux distillation at atmospheric pressure, distilled at reduced pressure (-700mmHg), and then distilling at reflux under reduced pressure, repeating the procedure of Example 1 to recover the aliquots by 50 mL. It was.

Comparative example  3: barley Atmospheric distillation  Atmospheric distillation Unreflected )

In Example 2, 50 mL portions were recovered by re-distillation without using reflux.

Comparative example  4: decompression distillation of barley Reduced pressure reflux distillation

After distilling at atmospheric pressure in Example 2, instead of refluxing at reflux at atmospheric pressure, the distillation at reduced pressure and distillation at reflux at reduced pressure were repeated to recover the aliquots by 50 mL.

Experimental Example  One: By fraction  Check the alcohol frequency change

For each fraction obtained in Example 1, Comparative Examples 1 and 2, Example 2 and Comparative Example 3, the alcohol concentration was measured using GC. GC analysis conditions were as follows: Instrument: Perkin-Elmer Autosystem, Column: AT-wax (internal diameter 0.53 μm, film thickness 0.25 μm, length 30 m), oven temperature: 45 ° C. (3 min)-> 20 ° C./min- > 180 ° C. (10 min), injector: 250 ° C. (split mode), detector: FID (300 ° C.), carrier gas: He (45 KPa). The experimental results are shown in Table 1 and FIG. 2.

Distillate
Stroke (ml) Example 1 Comparative Example 1 Comparative Example 2 Example 2 Comparative Example 3 Distillate
Stroke (ml) Example 1 Comparative Example 1 Comparative Example 2 Example 2 Comparative Example 3 0-50 80.5 77.8 84.5 81.3 74.1 550-600 91.4 59.9 93.7 91.4 60.3 50-100 93.0 85.5 94.9 91.9 83.8 600-650 49.5 53.2 57.8 53.5 55.6 100-150 94.7 86.9 95.1 91.8 86.7 650-700 10.7 49.3 9.9 9.4 51.2 150-200 95.0 86.6 95.5 93.4 86.8 700-750 2.8 43.8 - 3.6 45.3 200-250 95.2 84.2 95.4 94.8 85.1 750-800 - 35.8 - - 38.8 250-300 95.2 79.9 95.4 95.3 81.0 800-850 - 28.5 - - 30.3 300-350 95.3 72.9 95.4 95.4 74.1 850-900 - 20.1 - - 22.5 350-400 95.2 71.6 95.3 95.3 70.8 900-950 - 14.5 - - 16.1 400-450 95.1 69.7 95.2 95.3 70.0 950-1000 - 7.9 - - 11.7 450-500 94.7 66.9 95.3 95.1 67.6 Alcohol
yield(%) 98.9 96.6 98.4 98.5 98.0

As shown in Table 1 and Figure 2, it was confirmed that the total alcohol recovery was 98% or more by re-distillation. There was no significant difference in the total alcohol recovery of Examples 1 and 2 and Comparative Examples 1 to 3 according to the present invention.

In addition, looking at the differences between the fractions, alcohol recovery according to atmospheric distillation and reduced pressure distillation did not have a significant difference, but showed a significant difference depending on whether reflux during distillation. That is, in the case of Comparative Example 1 and Comparative Example 3 that does not reflux, the alcohol is continuously reduced toward the downstream, while in Example 1, Comparative Example 2 and Example 2 refluxed to a high alcohol of about 95% up to 600mL It was confirmed that the leak continued.

The main priority in the liquor industry is alcohol recovery, which has the advantage of removing a large amount of acetaldehyde while minimizing the discarded alcohol by moving acetaldehyde, which is spread throughout the entire region, to the first and second streams.

Experimental Example  2: main fragrance By fraction  Concentration change

For the fractions obtained in Examples 1 and 2 and Comparative Examples 1 to 3, the concentration change of the main fragrance components was analyzed using GC as in Experimental Example 1.

The concentration changes of acetaldehyde and ethyl acetate are shown in FIGS. 3 and 4, respectively.

As shown in FIGS. 3 and 4, acetaldehyde leaks from 0-50 mL and 50-100 mL in both rice and barley during unreflux, whereas acetaldehyde flows out in 70% at reflux. Showed a pattern. On the other hand, in the case of ethyl acetate, both the rice and barley showed a 20% increase in the initial outflow during reflux.

The concentration changes of the three main hull oils (n-propanol, i-butanol, i-amyl alcohol) and i-amyl acetate are shown in FIGS. 5 to 8, respectively. As shown in FIGS. 5 to 8, the three kinds of hull oil showed a similar pattern, while unrefluxed outflow relatively evenly by fraction, while refluxed afterwards, especially around 600-650ml, in which alcohol outflow drastically decreased. The concentration tended to be concentrated in the fraction section. In the case of amyl acetate, it was concentrated in the superfluid at the time of unreflux, but it was shown to flow out into the superfluid and the downstream at the reflux, which was different from the movement of other components to only the first or the downstream.

The fractional concentration changes of the main high boiling point components (ethyl lactate, ethyl caproate, ethyl caprylate, ethyl caprate, 2-phenylethanol and 2-phenylethyl acetate) are shown in FIGS. 9 to 14, respectively. As shown in FIGS. 9 to 14, in the case of ethyl lactate, it flowed out over the entire period at about 5 ppm at the time of unreflux, but only at the downstream side at the time of reflux. In case of ethyl caproate, only unflowed spilled into the superstream, while reflux flowed in a small amount from the stream and the remainder flowed from the downstream. In addition, in the case of ethyl caprylate, similar to the trend of the outflow of ethyl caproate, the component that flowed out in the first stream showed a characteristic of flowing out in the downstream by reflux. In the case of ethyl caprate, the components which flowed out to the distillation stream and the middle part at the time of unreflux were discharged only in the downstream by reflux. Furthermore, 2-phenolethanol tended to increase from the middle of the distillation to the second half of the distillation after the distillation when the reflux was not distilled out, but concentrated in the downstream after the reflux. In the case of 2-phenylethyl acetate, the outflow evenly over the middle of distillation during unrefluxing tended to concentrate on the downstream side at reflux.

Experimental Example  3: main fragrance By fraction  Concentration change

In order to examine the difference in the fragrance components according to atmospheric reflux distillation and reduced pressure reflux distillation, each fraction was obtained as in Example 1 and Comparative Example 2 and analyzed using GC in the same manner as in Experiment 1. The analysis results are shown in Table 2 below.

As shown in Table 2, it was found that the amount of the fragrance component is several times more at normal pressure than the reduced pressure for each fraction. In the case of atmospheric distillation, many flavor components were concentrated and concentrated in the herbaceous material, so that more excellent flavor components were obtained than the reduced pressure. At atmospheric distillation, the fermentation urine is heated to a high temperature, and the fragrance component is higher than that of the reduced pressure, but a lot of raw odor and coal are generated, so that the main quality is not good. At this time, by removing the components of the raw odor or in the coal through the multi-stage reflux to the first or particularly downstream, it is possible to develop a product utilizing the good scent components of atmospheric distillation far more than the reduced pressure.

Experimental Example  4: of rice Atmospheric Reflux Distillation Super current  Analysis of fractions

The first fraction (0-50 mL) of Example 1 (atmospheric reflux distillation) was finely divided into 10 mL units, and then divided into 50 mL units to examine the content of acetaldehyde, which is a major cause of alcohol and hangover. The experimental results are shown in Table 3 below.

Fraction (mL) Alcohol(%) Acetaldehyde importance (%) 0-10 70.1 1821 21.85 10-20 75.2 1022 12.26 20-30 80.4 727 8.72 30-40 84.9 659 7.91 40-50 91.4 451 5.41 50-100 93.0 1250 15.00 100 to 150 94.7 501 6.01 150 ~ 200 95.0 315 3.78 200 to 250 95.2 163 1.96 250 to 300 95.2 143 1.72 300 to 350 95.3 120 1.44 350-400 95.2 96 1.15 400 to 450 95.1 90 1.08 450 to 500 94.7 85 1.02 500-550 94.7 91 1.09 550 to 600 91.4 92 1.10 600-650 49.5 710 8.52 system 8336 ppm 100%

As shown in Table 3, the first 10 mL fraction of the herbicidal fraction (0-50 mL) contained 22% acetaldehyde, while other components were present in trace amounts. Acetaldehyde is known to be the main cause of hangover among fragrances, and if only the first 10ml fraction is removed, the prototype can be used to remove more than 20% of the total amount of acetaldehyde without changing the overall flavor. In addition, it was determined that removing the downstream fraction could remove about 30% of acetaldehyde. On the other hand, the first or afterstream fraction not used in the manufacture of the product can be included in the next re-distillation, it is possible to maintain the alcohol recovery rate of 95% or more.

Experimental Example  5: Distillation formula by fractionation of redistillation stock  Soju( Alc .20%) Manufacturing and Sensory Evaluation

Sensory evaluation was carried out according to the formulation of each fraction of re-distilled stock solution using rice as a raw material. For control, 0-850 mL fractions were recovered without atmospheric reflux, and reflux prototype A was distilled from 0 to 650 mL fractions at reflux reflux. , Reflux prototype C recovers 10 ~ 600 mL fraction of atmospheric reflux distillation, reflux prototype D recovers 50 ~ 600 mL fraction of atmospheric reflux distillation. Sensory evaluation was performed. Specific characteristics of the prepared prototypes are shown in Table 4 below, and the results of aroma sensory test and taste sensory test are shown in Tables 5 and 6.

division Fraction (ml) Alcohol recovery rate (%) Characteristic rice Unreduced (control) 0-850 93.1 Without super cut
Wake cut from alcohol 20% Reflow Prototype A 0-650 97.5 Reflow Prototype B 50-650 90.7 Chop one fraction cut Reflow Prototype C 10 to 600 93.3 10 mL cut of vinegar, one fraction cut of the wake Reflow Prototype D 50-600 86.6 Cut 1 part each for the first and second streams barley Unreduced (control) 0-700 84.2 Without super cut
Wake cut from alcohol 50% Reflow Prototype A 0-650 97.4 Reflow Prototype B 50-650 90.6 Chop one fraction cut Reflow Prototype C 10 to 600 93.0 Cut 10 mL of vinegar, cut one fraction of the wake Reflow Prototype D 50-600 86.2 Cut 1 part each for the first and second streams

Incense sensory test result division Unreflected
Re-distillation Rice reflux
Prototype A Rice reflux
Prototype B Rice reflux
Prototype C Rice reflux
Prototype D 5 points total
(10 people) 33 points 27 points 22 points 39 points 29 points 1st frequency 3 people 1 person 1 person 3 people 2 people Sensuality Strong scent
Ester flavor steel
Strong wake smell
Flavor variety
Slightly coarse incense Choru, odor
Rough incense
Out of harmony No single directional
Wake smell
negative Fruity abundance
Moderate Distilled Scent
Cool incense
No off-flavor
Super-river Lack of incense
No vinegar, no smell.
No rejection
Clean incense

Taste sensory test result division Unreflected
Re-distillation Rice reflux
Prototype C Rice reflux
Prototype D 3 point sum
(10 people) 20 points 24 points 16 points 1st frequency 4 people 4 people 2 people Sensuality Familiar flavor
It's a bit rough,
Conventional rice shochu
Better than Sweetness feels strong
First taste is sweet and fruity
Abundant, but after the middle
Taste slightly irritating Sweet but moderate
The taste is monotonous
Incense too low
Prefer clean

As shown in Table 6, the tasting evaluation of the three products showing a high preference in the fragrance evaluation resulted in a high score of prototype C without addition of the part of the initial part and the after fraction, and the non-reflux distillation as a control. It was shown that the preference was higher in the order of prototype D which did not add the sample and the first / after fraction. Similar to the previous fragrance evaluation, unreflux re-distillation alone reduced the raw material odor and burntness of the existing atmospheric distillate liquor, and the coarse taste was noted as a disadvantage. If the cuts of vinegar and vinegar were cut like the prototype D, they had a clean taste, but had a weak taste because of the low flavor.

On the other hand, the results of evaluating the aroma and flavor in the same manner as described above with barley as shown in Tables 7 and 8.

Incense rating division Unreflected
Re-distillation Barley reflux
Prototype A Barley reflux
Prototype B Barley reflux
Prototype C Barley reflux
Prototype D 5 points total
(10 people) 32 points 30 points 24 points 35 points 29 points 1st frequency 2 people 3 people 0 people 3 people 2 people Sensuality Boring frankincense
High raw odor
Cool incense
Off-flavor Directional, Fragrance
A mild flavor
A little raw odor
heaviness A little raw odor
Lack of unidirectional
Lack of refreshment
clean Sweet and fruity
Aldehydes
A little barley
Memit Low scent
Clean

Although the difference in preference score was not large, it was preferred in order of prototype C, unreflux distillation, and prototype A, and similar to the results of aroma evaluation of rice, the preference of prototype C and unreflux distillation prototype was high, and there was no herb, but only afterstream. Prototype B was evaluated with the lowest preference.

Flavor evaluation division Unreflected
Re-distillation Barley reflux
Prototype A Barley reflux
Prototype C Three points of sum total (ten) 22 points 14 points 24 points 1st frequency 4 people 2 people 4 people Sensuality A mild flavor
There is raw material smell, odor
Common taste Slightly oily
Less fragrant and bitter
Lack of sweetness Sweet and strong
Scented but bitter
Some irritation

As shown in Table 8, in the flavor evaluation, the preference of prototype C was high, and the score of the non-reflux distillation sample as a control was high.

Prototype C is good because it has a super flavor and sweet taste in the first taste, but the bitterness in the back is pointed out as a disadvantage, and the unrefluxed distillation sample has a mild and familiar flavor, but a slight raw and smell.

From the results of sensory evaluation of distilled soju based on rice and barley, it was judged that Prototype C with the first 1/5 fraction of the herb and the afterstream removed was the best.

Claims (7)

In the method of producing a distilled shochu by fermenting the raw material of shochu and multi-stage re-distillation method,
(1) distilling the distillate distilled from the fermentation broth at atmospheric pressure to distillate at atmospheric pressure reflux to separate the head, medium and tail; And
(2) removing at least 30% acetaldehyde and flavoring by removing the first 1/5 fraction and wake of the herb in said fraction, or collecting the remaining fraction by removing the first 2/5 fraction and wake of the herb; Improved method of preparing distilled soju.
The method according to claim 1, wherein the raw material of shochu is rice or barley.
The method according to claim 1, wherein the multistage re-distillation is performed by using a 15-stage multistage distillator in which three 5-stage columns are connected.
The process according to claim 1, wherein atmospheric distillation of the fermentation broth is carried out under normal atmospheric pressure.
The method according to claim 1, wherein the atmospheric reflux distillation is performed at a reflux ratio of 1: 1 to 5: 1.
The method according to claim 1, wherein the atmospheric reflux distillation of the distillate is performed under a general atmospheric pressure.
Distilled shochu prepared by the method of claim 1.

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