JP3354028B2 - Distilled liquor production method - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a distilled liquor, and more particularly to a method for producing a distilled liquor capable of obtaining a high-quality distilled liquor with rich flavor and high yield.

[0002]

2. Description of the Related Art Distilled liquor is liquor obtained by distilling alcohol-containing moromi or liquid, such as shochu, whiskey, brandy,
Spirits, as well as Chinese spirits such as white sake (Paichu), Taiwanese rice sake, and Korean baked sake are known. As a distillation apparatus for shochu, which is one of the distilled liquors, a continuous distillation apparatus is used for shochu shells and a simple distillation apparatus is used for shochu class B. Distillation with a continuous distillation apparatus yields shochu with a very high degree of purification. On the other hand, in the method of producing shochu using a single distillation apparatus, a method of distillation under normal pressure or reduced pressure is performed, but since the fermented mash is distilled by evaporating and evaporating volatile components, the volatilization in the mash is performed. It is characterized in that the composition and content of the components change continuously, and the composition and content of the volatile components of the distillate also change continuously. Distilled liquor has a complicated flavor composed of raw materials, volatile components derived from fermentation or heating or storage aging during distillation, and the flavor component largely depends on the difference in distillation method. For example, in the atmospheric distillation method used for shochu, fermented moromi is heated at 80 ° C. or higher, and the components produced by a heating reaction such as furfural and melanoidin increase, which is not preferable. Therefore, a vacuum distillation method was developed. That is, in the vacuum distillation method, 40 to 70 ° C.
The amount of the components generated by heating is moderate because the distillation is performed by the heating, and a shochu mainly composed of raw materials and fermentation-derived flavor components is produced. Furthermore, in the vacuum distillation method, in order to obtain shochu of diversified quality with a characteristic flavor, by eliminating the first distillation and the last distillation of distillation, also known in the atmospheric distillation method, and by changing the degree of vacuum, the purpose and A method of obtaining shochu of a high quality is adopted. Flavor components other than ethanol contained in shochu include aliphatic aldehydes, higher alcohols, esters, organic acids, and furfural.
In terms of flavor, these are considered to form a balance of flavors in total, and from this point of view, in order to obtain shochu with good flavor, improvements have been made to the conventional single distillation apparatus and distillation methods have been further devised. .

[0003] On the other hand, ultrasonic waves include vibration, acoustic streaming, radiation pressure,
It is known that there is an action such as cavitation (cavitation phenomenon). For alcoholic beverages, use in raw material processing, fermentation, filtration / purification, aging processes, and the like is known. Tokuhei 3
No. 23149 discloses that ultrasonic vibration is applied to a vibrating member disposed in a dilute alcohol solution to generate cavitation, thereby causing the alcohol in the solution to be vaporized by the cavitation, and the vaporization of the alcohol. A method for sonicating a dilute alcohol solution is described, which comprises directing a gas to a predetermined location to condense and liquefy. According to this method,
Alcohol can be obtained without heating while keeping the yeast in the fermentation liquid alive, and the alcohol concentration in the liquid can be reduced, so that alcohol fermentation can be performed continuously. That is, there is an advantage that energy consumption can be reduced as compared with the conventional method of directly heating and evaporating to condense and liquefy, and an object of the invention is to substitute an energy source.
However, it has not been known that, in a conventionally known ordinary heating distillation method, ultrasonic treatment is performed at the time of heating in a distillation can or at the time of condensing steam in a condenser to improve the quality of distilled liquor.

[0004]

SUMMARY OF THE INVENTION In a conventional method for producing distilled liquor by heating distillation, a device is added during heating in a distillation can to promote the evaporation of the components of the distilled liquor, thereby improving the distillation efficiency and condensing. It has been desired to develop a method for producing a distilled liquor that improves the condensation efficiency in a vessel and obtains a distilled liquor with a rich flavor. SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing a distilled liquor capable of obtaining a high-quality distilled liquor with a rich flavor in view of the above-mentioned prior art.

[0005]

SUMMARY OF THE INVENTION In general, the present invention is characterized in that a method for producing a distilled liquor obtained by ordinary heat distillation includes a treatment by ultrasonication in the distillation step. The present invention relates to a method for producing distilled liquor.

As a result of intensive studies, the present inventors have found that, in a method for producing distilled liquor by ordinary heat distillation, a high-quality method for solving the above-mentioned problems by including a treatment of sonication in the distillation step. It has been found that it is possible to obtain a product.

Hereinafter, the present invention will be described in detail. The distilled liquor in the present invention refers to liquors obtained by distilling alcohol-containing substances, such as shochu, whiskey, brandy, and spirits, as well as Chinese liquor such as white sake (paichiu), Taiwanese rice liquor, and Korean liquor. Can be If you divide shochu in more detail, for example, rice shochu, wheat shochu,
There are potato shochu etc., depending on the distillation method, for example, there are shochu shells distilled by a continuous distillation apparatus, shochu oysters distilled by a single distillation apparatus, and in recent years, a mixture of Koo oysters is also known, In the present invention, the difference in raw materials and distillation methods does not matter.

[0008] The simple distillation apparatus comprises a distillation can for generating steam by heating fermented mash and liquid, a concentrating tower provided with baffle plates and a perforated plate shelf, a condenser for cooling steam, and the like. In the atmospheric distillation method, distillation is performed by direct heating, for example, by direct fire, steam injection and indirect heating. In the vacuum distillation method, distillation is performed by heating using indirect heating, for example, a heating coil, a steam jacket, a donut tube, and external heating. The direct heating method using steam has a higher heat transfer rate and higher distillation efficiency than the indirect heating method, but it has many entrainments, and the fermentation mash and liquid are diluted by steam to increase the amount of waste liquid. There are features. On the other hand, the indirect heating method is characterized by the fact that, compared to the direct heating method, sake quality has a strong flavor, a tendency to contain a lot of acids, a high distillation rate, and a small amount of waste liquid. In case of, you need stirring. Both heating methods have advantages and disadvantages, and it is important to improve the distillation efficiency to obtain distilled spirits with rich flavor. Further, in the condenser, the steam collides with the cooling surface and condenses, but the condensed liquid covers the cooling surface, lowering the heat conduction and lowering the condensation efficiency. Therefore, it is necessary to take measures by lowering the temperature of the cooling water or increasing the amount of cooling water. It is also important to improve the condensation efficiency in this condenser.

[0009] The characteristics of the method of producing distilled spirits from the viewpoint of the components to be distilled are, for example, in the case of a method of producing shochu using a simple distillation apparatus, the composition and content of volatile components in the fermented mash to be distilled. Distillation proceeds under continuously changing conditions to produce a distillate. Examples of the low boiling components of the volatile components of the distillate include acetaldehyde, ethyl acetate, ethanol, n-propanol, i-butanol, isoamyl acetate, n-butanol, i-amyl alcohol, ethyl caproate, and the like. As the boiling point component,
For example, hexyl alcohol, ethyl caprylate, heptyl alcohol, furfural, octyl alcohol, ethyl caprate, diethyl succinate, ethyl laurate, β-phenethyl alcohol, ethyl myristate,
Ethyl palmitate and the like. The composition and content of these volatile components greatly depend on the content ratio of various volatile components in the mash in the distillation can, and it is important to recover and distill these components quickly and in large quantities.

The ultrasonic treatment of the present invention may be performed on fermented mash or liquid in a distillation can, on steam generated by distillation, or when condensing steam in a condenser. Well, they may be used in combination. In this way, regardless of the direct heating or indirect heating, the evaporation of the components of the spirit is promoted to improve the distillation efficiency, and the condensation efficiency in the condenser is improved, and the quality of the spirit is enhanced. Can be obtained.

The type of the distillation apparatus may be either a continuous type or a single type, and is not particularly limited. Also in the single distillation apparatus, any of the atmospheric distillation method and the reduced pressure distillation method may be used, but preferably the reduced pressure distillation method is suitable from the viewpoint of the quality of the sake and the distillation rate. The condenser includes, for example, a coiled tube, a tube, a plate type, and the like, but is not particularly limited.

The conditions of the ultrasonic treatment used in the present invention are appropriately selected depending on the type and form of the material to be treated such as fermented mash, liquid and steam. The frequency is preferably at least 15 kHz, particularly preferably from 20 kHz to several hundreds from the viewpoint of processing effect.
MHz, and the intensity is preferably 0.0
More than 01 W / cm ² , particularly preferably more than 0.005 W / cm ² from the viewpoint of action and effect, and the treatment time is preferably several seconds to several tens hours, particularly preferably several tens seconds to several hours. Is selected as appropriate. The ultrasonic treatment may be performed continuously or intermittently. Further, the treatment may be performed directly and / or indirectly on the object. In the case of external heating, the heating liquid may be subjected to ultrasonic spraying in the distillation can. Cavitation due to ultrasonic waves in the object to be processed may or may not occur, and is not particularly limited. However, it is preferable that there is no cavitation because droplet entrainment is reduced. The temperature of the object is preferably 35 ° C.
Above, particularly preferably at least 40 ° C. In addition, reflux distillation (for example, continuous distillation or Japanese Patent Application No.
-Distillation described in -287183) and the present invention can be used in combination. As a vibrator that generates ultrasonic waves, a bolted Langevin-type vibrator that has a structure in which piezoelectric ceramics commonly used in ultrasonic cleaning machines are sandwiched between two metal blocks and fastened with bolts, and should be thin in structure A vibrator having a structure in which a piezoelectric ceramic which can be bonded to a glass equipment epoxy resin substrate is used. In order to generate a weak ultrasonic wave, a vibrator of a single piezoelectric ceramic may be used.

(Study 1) A model test was conducted to confirm the effect of ultrasonic treatment in the distillation can. 2 liters of sake mash (prepared by adding distilled water to ethanol 16%, v / v) obtained by a conventional method is placed in a pressure-resistant container, connected to a condenser, and the container is depressurized at a pressure of 300 torr. Distilled at 65 ° C. in a hot water bath. On the other hand, sake mash was ultrasonically distilled at a frequency of 38 kHz and an intensity of 0.4 W / cm ² . The control was distilled without sonication. The distillate during distillation under reduced pressure and its ethanol were measured to evaluate changes over time.
Table 1 shows the results.

[0014]

[Table 1] Table 1 Distillation process ─────────────────────────────────── Ultrasonic treatment category Control ethanol Ethanol treatment Distillate Concentration Recovery Volume Recovery Distillate Concentration Recovery Volume Recovery Time (%, (100%, v / v (%, (100%, v / v (min)) (ml) v / v) ethanol (%) (Ml) v / v) Ethanor (%) le ml) le ml) ────────────────────────────── ───── 0 10 104 71.0 73.8 23.1 100 71.0 71 22.2 20 202 69.8 141.4 44.2 195 67.1 130.9 40.9 30 285 66.8 190.4 59.5 276 63.0 173.8 54.3 40 360 63.5 228.7 71.4 351 59.1 207.6 64.9 50 433 61.9 260.8 81.5 427 54.8 234.2 73.2 60 504 56.4 284.2 88.8 493 51.8 255.2 79.8 70 569 52.2 297.2 92.8 560 48.3 270.6 84.6 80 633 48.3 306.2 95.6 625 45.1 281.7 88.0 90 697 45.5 314.9 98.4 690 42.1 290.8 91.0 100 755 39.3 296.7 92.7 110 819 36.7 300.5 93.9 120 883 34.2 302.4 94.5 130 947 32.1 303.4 9 4.9 ───────────────────────────────────

From Table 1, it was found that the distillation rate of ethanol was improved by the ultrasonic treatment as compared with the control, and the ethanol concentration in the obtained distillate was also increased. Under these experimental conditions, the sonication required 70 minutes for the ethanol recovery to reach 92.7-92.8% (ethanol concentration 52.
2%, v / v), control 100 minutes (ethanol concentration 39.
3%, v / v), the ultrasonic treatment reduces the heating time by about 30%. Therefore, it is possible to distill ethanol at a high yield in a short time, and the risk of burning due to heating is significantly reduced. This is presumed to be due to a special environment caused by vibration, acoustic streaming, radiation pressure, cavitation, etc. due to the ultrasonic treatment, and the transfer of volatile components into the gas phase was promoted.

(Study 2) Next, a model test was performed to confirm the effect of sonication on condensation. Sake 100
ml (ethanol 16%, v / v) into a round flask, add distilled water to 200 ml, distill it with a direct fire at normal pressure, and evaporate the water with a silicon tube (inner diameter 4 mmφ,
Using an outer diameter of 8 mmφ), the length to be cooled was set to 50 cm, and the mixture was placed in a water bath at 10 ° C, 15 ° C, 20 ° C, and 25 ° C, and condensed while stirring water. The sonication in the condensation was performed at a frequency of 38 kHz and an intensity of 0.4 W / cm ² . Controls condensed without sonication. 1 distillate
At the time when the volume reached 00 ml, ethanol was measured, and the ethanol recovery was calculated. Table 2 shows the results.

[0017]

[Table 2] Table 2 Ethanol recovery rate ──────────────────────────────── Ethanol recovery rate (%) Cooling temperature ─ ────────────────── (℃) Ultrasonic treatment category ─────────────────────── {10 100 100 15 100 97 97 20 98 92 25 25 91 85} ───

From Table 2, it was confirmed that, when the ultrasonic treatment was carried out, the vapor was condensed better than the control, and even when the cooling temperature was increased, the recovery rate of ethanol was high and the condensation efficiency was improved.

[0019]

EXAMPLES Hereinafter, the present invention will be described specifically with reference to examples, but the present invention is not limited to these examples.

Example 1 A non-polished white rice with a milling ratio of 75% was used and the blending ratio shown in Table 3 was used.
We brewed rice shochu by three-stage preparation. As steamed rice, steamed rice obtained by immersing, draining and steaming non-glutinous white rice by a conventional method was used.
Koji was prepared by inoculating spores of Aspergillus oryzae and koji making by a conventional method. The yeast used was Association No. 701. In the third stage, 1.6 g of spittase M (manufactured by Nagase Seikagaku Corporation) was added, and saccharification / fermentation was performed at 15 ° C. for 20 days. Table 4 shows the component analysis values of the fermented mash.

[0021]

[Table 3] Table 3 Preparation and mixing ─────────────────────────────────── 1 stage 2 stages 3 stages Total 米 Total rice (g) 430 780 1390 2600 Rice over rice (g) 310 660 1230 2200 Koji rice (g) 120 120 160 400 Pumping water (ml) 790 1110 2200 4100 Lactic acid (ml) 30 ─── ─── ────────────── ────────────── ─────────────────────

[0022]

[Table 4] Table 4 Component analysis value of fermented mash 成分 Component and index value Analytical value エ タ ノ ー ル ethanol (%, v / v) 17.2 pH 4.0 Acidity (0.1N NaOH ml / 10ml) 7.9 Amino nitrogen (mg%, w / v) 46.2 Sake degree +10.0 Straight sugar (%, w / v) 0.5% ───────────────────────────

Using 2 liters of fermented mash, distillation under reduced pressure was performed using a pot still. Decompression degree 300 torr, distillation temperature 65
C. and condensation were performed at a cooling water temperature of 15C. The present invention applies ultrasonic treatment to fermented mash at a frequency of 38 kHz and an intensity of 0.4 W / cm.
Distilled at ² . Controls were distilled without sonication. The middle distillate fraction was collected except for the first distillate and the second distillate (ethanol 10%, cut by v / v). The fractionated middle distillate fraction was diluted with distilled water so as to be ethanol 25%, v / v, and then subjected to component analysis. Table 5 shows the results.

[0024]

[Table 5] Table 5 Analytical values of distillates of middle distillates ───────────────────────────────── ── Ingredient of the present invention 対 Ethanol (%, v / v ) 25 25 Total ester (ppm) 270 205 Total aldehyde (ppm) 9.5 13.0 Acidity (0.1 N NaOH ml / 10 ml) 0.16 0.11 pH 6.5 6.8 ───────────────────────────── Low boiling point odor component (ppm) Acetaldehyde 15 19 Ethyl acetate 100 61 n-propanol 124 120 Isoamyl acetate 135 i-butanol 225 200 ethyl caproate 20 i-amyl alcohol 420 280 ────────────────────────────────

From Table 5, it can be seen that the product of the present invention has 1.3 times as much ester content and high acidity as the control, as compared with the control. The distillation time of the middle distillate section of the present invention was 75 minutes (distillation rate 94.6%), while the control was 105 minutes (distillation rate 92.1%). According to the present invention, the distillation time is shortened and the distillation yield is improved. Next, the product of the present invention was subjected to a sensory test in comparison with a control. Table 6 shows the results of the sensory test.

[0026]

[Table 6] Table 6 Results of sensory test ────────────────────────────────── Item Comparison with product of the present invention香 り Aroma 1.9 2.3 Taste 1.1 2.6 Overall 1 ７ 2.4 Evaluation opinion ○ Fermentation scent is rich ○ Fermentation scent is normal ○ Taste has taste and depth ○ Taste is pale and lacks depth ○ Excellent flavor balance ○ Normal flavor balance ────── ────────────────────────────

Note) Sensory test evaluation method 5-point method 1: good to 5: bad panelists 10 (average value)

Table 6 shows that the product of the present invention had a rich fermentation aroma, a deep taste, a lot of flavors, and an excellent flavor balance as compared with the control.

Example 2 A refined barley having a grain percentage of 70% was immersed, drained, steamed, and allowed to cool by a conventional method, inoculated with Shochu white koji mold, and koji-produced. The mixture was charged in a liter, shochu yeast was added to perform primary charging, and fermented at 20 ° C. for 7 days. Next, 10 kg of steamed barley prepared by a conventional method with a barley yield of 70% and 12.5 liters of pumped water were added to the primary mash as a secondary mash, followed by fermentation at 20 ° C. for 15 days. Table 7 shows the component analysis values of the fermentation.

[0030]

[Table 7] Table 7 Analytical values of fermented mash ───────────────────────────────── Ingredients and index value analysis Value ───────────────────────────────── ethanol (%, v / v) 15.5 Total sugar (%, w / v) 1.1 Straight sugar (%, w / v) 0.3 Total nitrogen (mg%, w / v) 27.3 Amino nitrogen (mg%, w / v) 15.3 Acidity (0. 1N NaOH ml / 10ml) 7.2 pH 4.2

According to the present invention, out of 25 liters of this fermented mash, 2 liters are distilled by a vacuum distillation method (the same conditions as in Example 1), and the ultrasonic treatment is performed at a frequency of 38 kHz and an intensity of 0.4 W / cm ² . The same procedure was used for moromi and also for condensation in a condenser. The control was distilled and condensed without sonication. Initial distillation and late distillation (ethanol 10
%, Cut by v / v), and the middle distillate fraction was collected and diluted with distilled water to 25% ethanol, v / v, and then subjected to component analysis. Table 8 shows the results.

[0032]

[Table 8] Table 8 Component analysis value of distillate of middle distillate component ───────────────────────────────── ─── Ingredients of the present invention ──────────────────────────────────── Ethanol (%, v / v) 25 25 Total ester (ppm) 186 152 Total aldehyde (ppm) 6.0 7.3 Acidity (0.1 N NaOH ml / 10 ml) 0.8 0.5 pH 6.5 6.8 ───────────────────────────────── Low boiling point odor component (ppm) Acetaldehyde 9 13 Ethyl acetate 140 110 n-propanol 192 140 isoamyl acetate 148 i-butanol 231 200 ethyl caproate 31 i-amyl alcohol 320 265 ──────────────────────────────────

As shown in Table 8, the product of the present invention tended to have more ester and higher acidity than the control. Further, the distillation time and the yield were almost the same as those of Example 1 in comparison with the present invention. Next, the product of the present invention was subjected to a sensory test in comparison with a control. Table 9 shows the results of the sensory test.

[0034]

[Table 9] Table 9 Results of sensory test ─────────────────────────────────── Item Items of the present invention ─────────────────────────────────── 香 り Aroma 2.3 2.7 Taste 2.2 2.9 Overall 2.2 2.8 Evaluation opinion ○ Fermentation scent is rich ○ Fermentation scent is normal ○ There is a wide range of tastes ○ The taste is monotonous ○ Excellent in flavor balance ○ Lack of flavor balance 欠──────────────────────────

Note) Sensory test evaluation method 5-point method 1: good to 5: bad panelists 10 (average value)

Table 9 shows that the product of the present invention had a rich fermentation aroma, had a wide range of tastes, and was excellent in flavor balance as compared with the control.

[0037]

As described above, the production of distilled liquor in accordance with the present invention enhances the good flavor components produced in the fermented moromi, and provides a high-quality distillation with a deep flavor and an excellent flavor balance. The present invention provides a method for producing distilled liquor, which is useful for quality and productivity, since liquor can be obtained, and the distillation time can be shortened, the condensation efficiency can be improved, and the distilled liquor can be obtained in good yield. is there.

──────────────────────────────────────────────────続 き Continuing from the front page (72) Inventor Takumi Takayama 2-58, Nanryo-cho, Uji-city, Kyoto (72) Inventor Morita Atsuyuki 31-1 Nakajima-Kawaradacho, Fushimi-ku, Kyoto, Kyoto No. (72) Inventor Tadashi Yano Tokoku 3-19-3 Takejodai, Sakai City, Osaka (56) References JP-A-51-13379 (JP, A) JP-A-56-138645 (JP, A) 58-152472 (JP, A) Fully open 1988-193535 (JP, U) Fully open 1988-193501 (JP, U) (58) Fields investigated (Int. Cl. ⁷ , DB name) C12G 1 / 00-3/12 B01D 1/00-5/00

Claims (2)

(57) [Claims] 1. A method for producing a distilled liquor obtained by ordinary heat distillation, comprising a treatment of sonication in the distillation step. 2. The production of a distilled liquor according to claim 1, wherein the ultrasonic treatment is performed when steam is generated during heating in the distillation can and / or when steam is condensed in the condenser. Method.