KR100773912B1 - Batch distillation for preparation of distilled spirits - Google Patents

Abstract

A batch distillation apparatus under reduced pressure for the preparation of distilled liquor(soju) is provided to remove unpleasant smell from the distilled liquor by using a multi-stage distillation column and a reflux cooling pipe, thereby preparing high quality of distilled liquor. A batch distillation apparatus under reduced pressure for preparation of distilled liquor comprises a heater(11), a distillation pot(12) on the heater, a neck communicated with the top of the distillation pot, a cooling pipe communicated with one side of the neck, a cooling submerged pipe(16), a fractionating vessel(17) under the cooling submerged pipe and a vacuum pump(20) installed in the fractionating vessel. The batch distillation apparatus contains a 5- to 20-stage distillation column(13) interconnected with the distillation pot instead of the neck, a reflux cooling pipe communicated with a top of the distillation column and a condensation cooling pipe(15) interconnected between the fractionating vessel and vacuum pump, wherein the distillation column is a bubble cap type, valve type, sieve type or shower type distillation column.

Description

Batch Distillation for Preparation of Distilled Spirits

1 is a schematic diagram showing the configuration of a conventional vacuum distillation unit.

It is a schematic diagram which shows the structure of the single pressure vacuum distillation machine of this invention.

Figure 3a is a longitudinal cross-sectional view of a distillation column consisting of 10 stages provided in the single stage vacuum distillation unit of the present invention.

Figure 3b is a transverse cross-sectional view of a distillation column consisting of 10 stages provided in the single stage reduced pressure distillation unit of the present invention.

<Description of the symbols for the main parts of the drawings>

1: heater 2: distillation pot

3: connector 4: cooling tube

5: cooling pipe 6: preparative

7: vacuum pump

11: burner 12: distillation pot

13: distillation column 14: reflux cooling tube

15: condensation cooling tube 16: cooling tube

17: Preparatory Container 1 18: Preparatory Container 2

19: condensation cooling tube 20: vacuum pump

The present invention relates to a single reduced pressure distillation machine for preparing distilled shochu. More specifically, the present invention relates to a distilled soju prepared by using a single stage distillation column equipped with a multi-stage distillation column on a distillation pot, and a reflux distillation unit for preparing a distilled soju and an electric single stage vacuum distillation unit having a reflux tube. .

Shochu distilled fermented liquor obtained by mixing the raw material (mainly grain), fermented strain and water containing starch, distilled distilled liquor prepared by continuous distillation according to the distillation method And distilled soju prepared using single column distillation.

Among them, dilute shochu is prepared by diluting the spirit produced by the continuous distillation method. The continuous distillation method is a method of distilling fermented liquor continuously by injection and heating, and using a continuous distillation unit equipped with a multi-stage distillation column to remove impurities, thereby finally obtaining a spirit having almost no impurities. Since it can be, the distilled soju prepared by the continuous distillation method has the disadvantage that there is no impurity and does not require the aging process, and that the flavor of the fermented alcohol is not included at all.

In contrast, distilled shochu is prepared by distillation by a single distillation method and aged for a long time. The single distillation method is also referred to as a batch distillation (batch distillation), usually a distillation pot containing a fermentation broth to be distilled and heated, a cooling tube made of a liquid by cooling the distilled gas and a liquefied distillate supernatant, middle stream and It is a method of distilling by heating under normal pressure or reduced pressure using the vacuum distillation which consists of an aliquot which divides into 3 parts of a wake liquid, and fractionates. When using this method, since not only the flavor components other than alcohol during distillation but also the unpleasant odor generated during the distillation process are distilled, consequently, not only the concentrated flavor of the fermented liquor, but also a large amount of the odor component are included. Distilled shochu is prepared. Since the distilled shochu prepared in this way requires a long-term aging process to remove the odor-producing ingredients, the disadvantages of cost increase due to long-term aging and the disadvantage of excessive flavor and unpleasant odor compared to dilute shochu. There is such a situation that is dismissed from the consumer.

Accordingly, in order to overcome the disadvantages of the above-mentioned distilled soju, various studies have been conducted. For example, Korean Patent Registration No. 458012 discloses a method for preparing distilled soju, which removes activated carbon and distills it, considering that the unpleasant component of fermented wine is derived from fungal strains, and Korean Patent Registration No. 561563 The method for preparing distilled shochu comprising distilling the fermented liquor prepared by fermentation with yeast after stepwise treatment with proteolytic enzymes, liquefaction enzymes and glycosylating enzymes, without the use of fungal strains that cause unpleasant components. Is disclosed. However, even if the fermented liquor is deodorized with activated charcoal, the unpleasant components already contained in the fermented liquor are azeotropic when distilled by fast distillation, and also have a disadvantage that a considerable portion remains even if the deodorized with activated carbon after distillation.

If it is possible to develop a method to effectively remove the unpleasant components contained in the distilled soju, the natural flavor of fermented liquor is expected to be able to develop high-quality soju with high palatability of consumers. It's not happening.

Thus, the inventors of the present invention, as a result of intensive research to develop a method for effectively removing the unpleasant components contained in the distilled shochu, a multi-stage distillation column is provided on the distillation pot, a refrigeration tube equipped with a reflux cooling tube on the distillation column. When distilling under reflux, it was confirmed that the unpleasant components included in the distillate could be removed, thereby completing the present invention.

After all, the main object of the present invention is to provide a single pressure distillation column equipped with a distillation column and a reflux condenser.

Another object of the present invention is to provide a distilled shochu from which an unpleasant component is removed, which is prepared using an electric single-pressure distillation distillation machine.

In general, the continuous distillation apparatus used in the continuous distillation method controls the reflux cooling tube provided on the distillation column such as the temperature of the cooling water and the amount of passage per unit time, such as the content of alcohol as well as the flavor content of the distilled steam. And since it is known that the degree of concentration of the impurities can be changed, the present inventors are provided with a distillation column and a reflux cooling tube for concentrating the alcohol component, flavor component and impurities of the fermented liquor, which can be refluxed under reduced pressure and distilled. A vacuum distillation machine was devised.

Hereinafter, the configuration of the single pressure distillation distillation apparatus of the present invention will be described in more detail with reference to the accompanying drawings.

1 is a schematic view showing the configuration of a conventional vacuum distillation unit, the conventional vacuum distillation unit is connected to the heater 1, the top of the distillation pot (2), the electric distillation pot (2) provided on the top of the heater (1) At the lower end of the neck (3), the cooling tube (4) in communication with the electrical connection tube (3), the cooling yarn tube (5) in communication with the lower end of the electrical cooling tube (4), And a vacuum pump 7 in communication with the aliquot 6 and the electric aliquot 6 communicating therewith.

Figure 2 is a schematic diagram showing the configuration of a single pressure reduced pressure distillation unit of the present invention, the single pressure reduced pressure distillation unit of the present invention is a heater 11, a distillation pot (12) provided at the upper end thereof, a distillation column (13) provided at the upper end thereof, A reflux cooling tube 14 communicating with the upper end thereof, a condensation cooling tube 15 communicating with the upper end thereof, a cooling yarn tube 16 communicating with the lower end thereof, a preparatory tube 1 (17) communicating with the lower end thereof, and communicating with the side thereof There is a preparatory tube 2 (18), and consists of a condensation cooling tube 19 and a vacuum pump 20 in communication with the upper end thereof. Comparing the structure of the single-pressure reduced-pressure distillation unit of the present invention with the structure of the conventional reduced-pressure distillation unit, (i) it includes a distillation column composed of 1 to 20 stages and a reflux cooling tube provided on the distillation column instead of the connecting tube, (ii) A) a pipe cooling tube for recooling the condensate condensed in the cooling tube; and (iii) a condensing cooling tube for recooling the vapor evaporated by the vacuum pump in the aliquot.

In particular, the multi-stage distillation column included in the single pressure distillation distillation apparatus of the present invention is not particularly limited thereto, but may include a bubble cap type, a valve type, a vegetarian type, and a shower type. It is preferable that it is comprised in the form used for normal distillation towers, such as these, and it is also possible to add the packing to these stages further. More preferably, each stage of the distillation column has a bubble column type including a bubble cap, an overflow pipe, and an air pipe, and the number of stages constituting the distillation column is not particularly limited thereto. However, it may be composed of 5 to 20 steps.

Figure 3a shows a longitudinal cross-sectional view of a distillation column consisting of 10 stages, Figure 3b shows a lateral cross section of a distillation column consisting of 10 stages. As shown in Figure 3a, there are a plurality of foams in each stage, and as shown in Figures 3a and 3b is provided so that the foam is located at the top of the vent pipe, the first-class pipe is located independently of the foam and the vent pipe.

When the fermentation liquor is put into the distillation pot 12 of the single-pressure reduced-pressure distillation apparatus of the present invention configured as described above, and the heater is heated to an appropriate temperature under reduced pressure, the distilled components are 1 to 4 through the multi-stage distillation column 13 and the reflux cooling tube 14. Distilled at a reflux ratio of 1, the condensed steam is first condensed to become a liquid phase in the condensation cooling tube (15), it is re-cooled to a temperature of 30 ℃ or less through the cooling yarn tube (16) and aliquots in preparative vessel 1 (17) The non-condensed volatile components and the volatile vapors present in the fractionated distillate are re-cooled while passing the cooling water at 15 ° C. through the condensation cooling tube 19 to be recovered in the preparative tube 2 (18), or the vacuum pump is removed. Eject through. In this case, the reflux ratio refers to the ratio of the total amount of distilled steam to the amount condensed in the distilled steam. For example, the reflux ratio is expressed as 4 when the total amount of distilled vapor is 100 and the condensed amount is 25.

As a result, the single-stage reduced pressure distillation apparatus of the present invention includes a heater, a distillation pot provided at the top of the heater, a connection tube (neck) in communication with the top of the distillation pot, a cooling tube in communication with an upper end of the connection tube, and the cooling tube. In the vacuum distillation for distillation shochu production consisting of a cooling pipe communicating with the lower end, a preparatory tube provided at the lower end of the cooling tube and a vacuum pump provided in the preparative tube, communicating with the top of the distillation pot instead of the connecting tube 5 to 20 stages of the distillation column and the reflux cooling tube in communication with the upper end of the distillation column, characterized in that it comprises a condensation cooling tube communicating between the preparative cylinder and the vacuum pump.

Using the above-described single pressure distillation distillation apparatus of the present invention, distilled soju can be prepared. The specific method is as follows: the fermented liquor is put into the distillation pot 12 of the single pressure distillation distillation vessel and Distilling the fermented liquor by heating to maintain a temperature and a vapor pressure of 700 to 740 mmHg; Adjust the temperature of the reflux cooling tube 14 to reflux the distilled steam at a reflux ratio of 2 to 4, adjust the temperature of the condensation cooling tube 15 to 30 to 40 ℃ to condensed distilled steam, the condensed liquid Adjusting the temperature of the cooling yarn tube 16 to 30 ° C. or less to prevent re-distillation; And, by the step of collecting the condensate passed through the cooling pipe 16 in the preparatory tube 1 (17), distilled liquor can be prepared by diluting the distillate, and then diluted appropriately.

At this time, in order to remove the unpleasant components contained in the distilled shochu, each distillate can be obtained by distillation while gradually reducing the reflux ratio. First, distillation at a reflux ratio of 3 to 4, to obtain a distillate containing a distillate containing 3 to 10% of the total alcohol content contained in the fermented liquor, then distilled at a reflux ratio of 2 to 3 contained in the fermented liquor A middle liquor, which is a distillate containing 70 to 80% of the total alcohol content, can be obtained, and finally, a distillate containing 5 to 15% of the total alcohol content included in the fermentation liquor by distillation at a reflux ratio of 2. It can be obtained, it is possible to recover 90 to 95% of the total alcohol content contained in the fermented wine as a whole through distillation. At this time, the first flow and the second flow may be further recovered with the alcohol content contained in the initial flow and the after distillation with the fermentation liquor during the next distillation, in this case, the recovery rate of the alcohol may be 95% or more.

The obtained supernatant and the downstream liquid include acetaldehyde, ethyl acetate, methanol, ethanol, n-propanol, i-butanol, i-amyl acetate, n-butanol, i-amyl alcohol, n-amyl alcohol, ethylheptonate, Although odorous components such as ethyl lactate, acetic acid, perfural, ethyl caprate, ethyl laurate, and 2-phenylethanol are included in a large amount, the midstream contains a very low content of odorous components. Therefore, it is preferable to dilute only the supernatant liquid and use it as a distilled distilled liquor stock solution, and the supernatant liquid and the wake liquid are used again to distill the distillation pot. At this time, the alcohol fraction of the midstream liquid is used as a stock solution of distilled shochu by fractionating 45 to 75%, and distilled soju can be prepared by diluting drinking water in the stock solution, or can be used as an additive liquor such as dilute shochu.

In addition, a certain amount of volatile components may be evaporated from the supernatant, the middle stream, and the wake collected in the preparative container 1 (17), and the evaporated components are cooled again through the condensation cooling tube 19 provided in the preparative container. It can be collected in preparative vessel 2 (18) in the form of a condensate or discharged to the outside through the vacuum pump 20, the condensate collected in the preparatory vessel 2 (18) is put into a distillation pot at the next distillation and distilled again Can be used to

By using the single-stage reduced pressure distillation apparatus of the present invention, since the distillate from which the unpleasant component is removed can be obtained, it can be widely used for the production of high quality shochu.

Hereinafter, the present invention will be described in more detail with reference to Examples. These examples are only for illustrating the present invention in more detail, it will be apparent to those of ordinary skill in the art that the scope of the present invention is not limited by these examples in accordance with the gist of the present invention. .

Example 1 Preparation of Distilled Spirits

4 kg of starch rice 74% of ordinary rice was immersed in water for 2 hours, water was removed, and steamed for 30 minutes under conditions of 1.5 atm to obtain gourd rice. The obtained soybean rice was cooled to 36 ° C, 0.1% (w / w) of Aspergillus kawachi (Higuchi, Japan) was mixed with respect to the total weight of the soybean rice, and then incubated at 38 ° C for 48 hours. Made entry

1 kg of previously prepared entry and 0.9 L of water were mixed, 100 ml of Sacchromyces cerevisiae (Japan Brewing Association, Japan) culture solution was added thereto, and shaken at 25 ° C. for 2 days to obtain juju. Subsequently, 3kg of entry into the basement bath and 4L of water were added thereto, and the obtained base hair was added and fermented at 25 ° C. for 2 days to prepare basement. Then, 18 kg of ordinary rice was cooked for 30 minutes under the condition of 1.5 atm, cooled to 25 ° C., 28 L of water was added thereto, mixed with the prepared base liquor, fermented at 20 ° C. for 18 days, and 18% (v 55 L of fermented wine having an alcohol concentration of / v) was obtained.

Example 2 Comparison of the Components of a Distillate Prepared Using a Single Vacuum Reducer and a Conventional Vacuum Reducer

The fermented liquor prepared in Example 1 was applied to the single vacuum distillation unit shown in FIG. 2 and the conventional vacuum distillation unit shown in FIG. 1 to obtain respective distillates, and the unpleasant odor contained in each distillate was obtained. By comparing the contents of the constituents, we tried to obtain a distillate containing the least amount of volatile and unpleasant constituents.

Example 2-1 : Obtaining a Distillate Using a Single Vacuum Distillation Unit

The fermentation liquor obtained in the above Example 1 was applied to the single pressure distillation apparatus of this invention, and the distillate was obtained.

First, 11L of fermented liquor having an alcohol concentration of 18% (v / v) obtained in Example 1 was put into a distillation pot of the present invention, a reduced pressure distillation unit shown in FIG. 2, under a pressure range of 700 to 740 mmHg, and 50 ° C. Distilled while heating with. Adjust the cooling water of the reflux cooling tube to reflux at a reflux ratio of 2 to 4, maintain the temperature of the condensation cooling tube at 40 ℃, while maintaining the temperature of the cooling tube at 30 ℃ to the outflow of 700mL per hour to the aliquot 1 Distilled. That is, distillation under reflux at 3.5 reflux yields 92 mL (3.4% of total alcohol content) of distillate containing 75% (v / v) alcohol as a supernatant, and distilled under reflux at 2.5 reflux to yield 1,910 mL (68% of the total alcohol content) of the distillate containing 70% of phosphorus (v / v) alcohol was obtained. The distillate was refluxed at a reflux ratio of 2 to obtain a 20% (v / v) alcohol as a wake. A distillate containing 1,280 mL (13% of the total alcohol content) was obtained, and the same distillation was repeated three times. Finally, 6,900 mL of a distillate containing 70% (v / v) of alcohol was obtained and used as a sample. Used.

Example 2-2 Obtaining a Distillate Using a Conventional Vacuum Distillation Unit

22L of the fermented liquor obtained in Example 1 was put into a distillation pot of the conventional vacuum distillation apparatus shown in FIG. 1 and distilled to obtain 700 mL of the effluent per hour in an aliquot without a reflux under the same temperature and pressure as in Example 2. 214 mL (4% of the total alcohol content) of distillate containing 76% (v / v) alcohol as a stream liquid was obtained, and 7,040 mL (total) of distillate containing 45% (v / v) alcohol as a middle stream liquid (total) 80% of the alcohol content) was obtained, and 2,100 mL (12% of the total alcohol content) of the distillate containing 22% (v / v) alcohol as a wake solution was obtained.

Example 2-3 : Content Analysis of Volatile Components and Ingredients Showing Unpleasantness

The distillate (experimental group), the supernatant, the middle stream and the wake, which were obtained by using the single pressure distillation apparatus of the present invention in Example 2-1, and the conventional vacuum distillation obtained in Example 2-2. The distillate (control), the supernatant, the middle stream, and the wake, respectively, were diluted with drinking water to obtain distilled shochu with an alcohol concentration of 20% (v / v), respectively. Column: capillary column (DB-WAX), detector: FID, injection temperature: 200 ° C. Detection temperature: 220 ° C., oven temperature: initial 40 ° C., final 190 ° C. Required time 8 minutes, carrier gas: helium, carrier gas flow rate : 4.9 ml / min) was analyzed for the content of the volatile components and unpleasant components contained in each distilled shochu (see Table 1).

Content of various components in each distillate fraction (unit: ppm) Volatile components  Control  Experimental group Supernatant Midstream Wake Supernatant Midstream Wake  Acetaldehyde    12    15      8    20    11     5  Ethyl acetate    50    26      0.8   106     7     3  Methanol     6     5.7      5.5     6     5     5  ethanol  5000  5000   5000  5000  5000  5000  n-propanol   250   220    100   200   180   200  i-butanol   220   200     40   130   103   130  i-amyl acetate     2.7     1.5      One     8     0.4     0  n-butanol    10.8     7.1      5     3     5     7  i-amyl alcohol   330   306      80   280   250   189  n-amyl alcohol     0.2     0.2      0.2     0.2     0.2     0.2  Ethylheptonate     One     1.4      1.8     One     0.3     2.7  Ethyl lactate     One     1.6      3     One     0.8     3.7  Acetic acid     3     3      4     0.6     One     1.4  Perfural    10    11     12     0     4     9.9  Ethyl caprate     0     5      4     0     4     4  Ethyl laurate     1.2     1.7      2     0     One     3.3  2-phenylethanol    10    18     19     1.5     1.3    30

As shown in Table 1, in the control group, volatile components (acetaldehyde, ethyl acetate and methanol) and unpleasant components (perfural, propanol, i-butanol, i-amyl acetate, n-butanol, i-amyl alcohol, n-amyl alcohol, ethylheptonate, ethyl lactate, vinegar acid, perfural, ethyl caprate, and 2-phenylethanol) were found to be included in similar amounts in the supernatant, the midstream, and the downstream. . In contrast, in the experimental group, methanol, ethanol and n-amyl alcohol were contained in similar amounts in the supernatant, the middle stream and the wake, but acetaldehyde, ethyl acetate and i-amyl acetate were concentrated in the supernatant. , Vinegar acid, perfural, ethyl laurate and 2-phenylethanol are concentrated in the wake liquid, and propanol, i-butanol, n-butanol, ethylheptonate and ethyl lactate in high content in the supernatant and wake liquid. It was confirmed that it is contained in a relatively low content in the middle stream.

From the above results, it was confirmed that the distilled shochu prepared with the midstream liquid obtained using the single-pressure distillation distillation apparatus of the present invention contained much less volatile components and each component exhibiting unpleasant odor than the other distilled shochu. It can be seen that it is preferable to use the distillate shochu as the stock solution obtained by using the single-pressure distillation distillation apparatus of the present invention.

In addition, it was found that by using the single-stage distillation distillation apparatus of the present invention, a high-quality distilled shochu from which the unpleasant component was removed can be produced.

Example 3 : Comparison of sensory evaluation of distilled soju prepared using a single reduced pressure distillation machine of the present invention and a conventional reduced pressure distillation machine

The distilled liquor with alcohol concentration of 20% (v / v) was diluted by diluting the middle stream (experimental group) obtained in Example 2-1 and the middle stream (control group) obtained in Example 2-2 with drinking water, respectively. After manufacturing, 10 males (20s: 2, 30s, 3s, 40s, 3s, 50s) were selected for five-point measurement of taste, aroma, preference, and general preference. Good, 4 points: Good, 3 points: Normal, 2 points: Bad, 1 point: Very bad), and the average value thereof was obtained (see Table 2).

Sensory Evaluation of Distilled Soju from Control and Experimental Groups incense flavor preference General Symbol Control 2.8 2.5 2.7 2.7 Experimental group 4.2 4.5 4.5 4.4

As shown in Table 2, it was confirmed that the distilled soju (experimental group) prepared using the pressure distillation of the present invention exhibited better sensory characteristics than the distilled soju (control group) prepared using a conventional vacuum distillation.

As described and demonstrated in detail in the above, the present invention is provided with a multi-stage distillation column on the distillation pot, a distillation type produced using a single pressure distillation distillation distillation distillation shochu prepared with reflux cooling tube on the distillation column Serve shochu. By using the single-stage reduced pressure distillation apparatus of the present invention, since the distillate from which the unpleasant component is removed can be obtained, it can be widely used for the production of high quality shochu.

Claims (4)

Heater, a distillation pot provided at the top of the heater, a connecting tube (neck) in communication with the upper end of the distillation pot, a cooling tube in communication with the upper end of the one side of the connection pipe, a cooling yarn in communication with the lower end of the cooling tube, the cooling In the distillation distillation distillation distillation column for distilled distilled liquor made up of a preparatory tube provided at the bottom of the pipe and a vacuum pump provided in the vial, the distillation tower and the 5 to 20 stages of the distillation tower communicating with the top of the distillation pot instead of the connecting pipe A reflux condenser for producing a distilled shochu, comprising a reflux condenser communicating with an upper end of the condenser, and a condensing condensing tube communicating between the aliquot and the vacuum pump. The method of claim 1, The distillation column is a bubble cap type, a valve type, a vegetarian type, or a shower type distillation column, characterized in that Single vacuum distillation for making distilled shochu. The method of claim 2, Each stage of the bubble cap type distillation column includes a bubble cap, an overflow pipe, and an air pipe. Single vacuum distillation for making distilled shochu. The fermented liquor is put into the distillation pot of the single pressure distillation apparatus of any one of Claims 1-3, and it heats so that the temperature of 50-60 degreeC and the steam pressure of 700-740mmHg may be distilled, and the electric distilled steam is refluxed. A distilled soju prepared by diluting a distillate having an alcohol concentration of 45 to 75% (v / v) collected through a condenser tube and condensed in the order of a cooling tube, a condensation cooling tube, and a cooling tube.

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