WO2017104638A1 - Alcohol production method and alcohol deaeration method - Google Patents

Alcohol production method and alcohol deaeration method Download PDF

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Publication number
WO2017104638A1
WO2017104638A1 PCT/JP2016/086998 JP2016086998W WO2017104638A1 WO 2017104638 A1 WO2017104638 A1 WO 2017104638A1 JP 2016086998 W JP2016086998 W JP 2016086998W WO 2017104638 A1 WO2017104638 A1 WO 2017104638A1
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Prior art keywords
fiber membrane
hollow fiber
membrane module
alcohol
liquor
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PCT/JP2016/086998
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French (fr)
Japanese (ja)
Inventor
洋平 菅沼
克彦 猪狩
浩二 川瀬
和美 大井
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Dic株式会社
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Priority to JP2017556054A priority Critical patent/JP6675593B2/en
Publication of WO2017104638A1 publication Critical patent/WO2017104638A1/en

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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
    • C12G1/00—Preparation of wine or sparkling wine
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages

Definitions

  • the present invention relates to a method for degassing alcoholic beverages having a degassing step and a method for producing alcoholic beverages using the method.
  • the problem to be solved by the present invention is to use a hollow fiber membrane module, suppress the resin odor, and degas the dissolved gas in the liquor, and use the hollow fiber membrane module to obtain a resin.
  • An object of the present invention is to provide a method for degassing alcoholic beverages, which suppresses odor and degassed dissolved gas in alcoholic beverages.
  • the inventors of the present application have used a hollow fiber membrane module in which the skin layer is in contact with liquor, thereby suppressing the resin odor and degassing the dissolved gas in the liquor.
  • the present inventors have found that it is possible to provide an air method and a method for producing alcoholic beverages, and have completed the present invention.
  • the present invention relates to a method for producing an alcoholic beverage comprising a step of degassing dissolved gas from alcoholic beverages using a hollow fiber membrane module, wherein the hollow fiber membrane used in the hollow fiber membrane module comprises a skin layer and a porous layer. And a skin layer is in contact with the liquor.
  • the present invention also relates to a method for producing an alcoholic beverage comprising a step of degassing dissolved gas from alcoholic beverages using a hollow fiber membrane module, wherein the hollow fiber membrane used in the hollow fiber membrane module comprises a skin layer and a porous layer. And a skin layer is in contact with the liquor.
  • the present invention while using a hollow fiber membrane module, while suppressing the resin odor and degassing the dissolved gas in the liquor, and using the hollow fiber membrane module, while suppressing the resin odor, it is possible to provide a method for degassing alcoholic beverages by degassing dissolved gases in the alcoholic beverages.
  • the present invention will be described in detail, but the present invention is not limited only to these embodiment examples.
  • the steps until the production of the original sake (new sake) by brewing are well known and are omitted.
  • the raw liquor obtained through the brewing process is passed through a filtration device to remove microorganisms and fine particles remaining in the raw liquor (filtering step), and then the gas components in the raw liquor are removed by a degassing device (degassing step). ).
  • the deaerated raw liquor is transferred to a storage container and stored.
  • the filtration step is roughly composed of two steps of filtration with activated carbon and filtration with a filter using a filtration device.
  • the filter used at this time depends on the balance with the filtration rate, it is preferable to use a filter that does not lower the quality of the liquor and has a fineness enough to remove microorganisms that cause contamination with bacteria. .
  • the raw liquor obtained through the filtration step is sent to a degassing device to remove dissolved gas.
  • the reaction of oxidases can be suppressed and the reaction with the oxidizable substance can be inhibited.
  • the amount of dissolved oxygen in the raw sake after deaeration is preferably in the range of 0.01 to 10 ppm, and more preferably in the range of 0.5 to 4 ppm.
  • the deaeration device that can be used in the present invention include an internal recirculation type hollow fiber membrane module and an external recirculation type hollow fiber membrane module, and the module is used to remove dissolved gas from liquors flowing in the hollow fiber membrane module. Deaerate.
  • the outer recirculation type hollow fiber membrane module is superior in degassing efficiency to the inner recirculation type hollow fiber membrane module, and can suppress the flow pressure loss of water to a very low level. Not only is it most preferable when performing a deaeration process, but it is preferable because the resin odor can be further reduced.
  • the hollow fiber membrane used in the hollow fiber membrane module used in the present invention is usually provided that the membrane structure is a laminate of at least a skin layer (dense layer) and a layer having a pore (porous layer).
  • the membrane structure is a laminate of at least a skin layer (dense layer) and a layer having a pore (porous layer).
  • the material of the hollow fiber membrane used in the present invention is preferably a membrane made of a highly hydrophobic material, for example, a polyolefin resin such as poly (4-methylpentene-1) resin.
  • the film structure is not particularly limited as long as at least a skin layer (dense layer) and a layer having pores (porous layer) are laminated, but preferably a skin layer (dense layer) and a fine layer are formed. It is preferably a heterogeneous film in which a support layer (porous layer) having pores is laminated, and a skin layer (dense layer) on the outside and a support layer (porous layer) having pores on the inside are laminated. More preferred is a heterogeneous film.
  • the pore diameter is not particularly limited, but is preferably in the range of 0 to 100 nm, more preferably in the range of 0.1 to 50 nm.
  • the hollow fiber membrane used in the hollow fiber membrane module used in the present invention has an oxygen transmission rate of 0.1 ⁇ 10 ⁇ 5 to 5000 ⁇ 10 ⁇ 5 [cm 3 (STP) / cm 2 ⁇ sec ⁇ cmHg].
  • the range is preferably 0.5 ⁇ 10 ⁇ 5 to 500 ⁇ 10 ⁇ 5 [cm 3 (STP) / cm 2 ⁇ sec ⁇ cmHg], more preferably 0.9 ⁇ 10 ⁇ 5.
  • a range of ⁇ 100 ⁇ 10 ⁇ 5 [cm 3 (STP) / cm 2 ⁇ sec ⁇ cmHg] is most preferable.
  • the deaeration performance of the module generally improves as the oxygen transmission rate of the hollow fiber membrane increases, but the liquid transmission rate increases accordingly, so select a membrane with a good balance between both characteristics. It is desirable to do.
  • the measurement of the oxygen transmission rate and the gas separation coefficient ⁇ are easily performed according to ASTM-D1434.
  • a hollow fiber heterogeneous membrane made of poly (4-methylpentene-1) resin is preferable because it is excellent in gas permeability of oxygen, nitrogen, carbon dioxide, etc. and has high water vapor barrier properties.
  • the inhomogeneous membrane is described in detail, for example, in JP-B-2-38250, JP-B-2-54377, JP-B-4-15014, JP-B-4-50053 and JP-A-5-6656. It is stated.
  • the hollow fiber membrane module used in the present invention is an internal reflux type
  • the pressure outside the hollow fiber membrane (gas phase side) of the internal reflux type hollow fiber membrane module is kept under reduced pressure, while inside the hollow fiber membrane (liquid phase side) Pass through and deaerate.
  • the hollow fiber membrane module used in the present invention is an external reflux type
  • the pressure inside the hollow fiber membrane (gas phase side) of the external reflux type hollow fiber membrane module is kept under reduced pressure while the outside of the hollow fiber membrane (liquid phase) Side)) to deaerate.
  • the liquid phase side is a skin layer (dense layer)
  • the gas phase side is a layer having pores (porous layer).
  • the pressure is important to adjust the gas-phase pressure in the hollow fiber membrane of the hollow fiber membrane module according to the flow rate used and the amount of dissolved oxygen after the target treatment. It is preferable to set the pressure to be equal to or higher than the saturated vapor pressure at the temperature of the liquor concerned.
  • the decompression means may be evacuated simply by a vacuum pump or the like, but may be evacuated by a vacuum pump while flowing an appropriate sweep gas.
  • a method using a sweep gas in combination is effective.
  • a vacuum pump known ones can be used, for example, an oil rotary pump, a diaphragm pump, a water flow aspirator, a water ring vacuum pump, a water ring vacuum pump with a booster, a roots type, a scroll type, etc. And dry type vacuum pumps.
  • the oil rotary pump may be used with an oil / water separator, the water seal of the water ring pump may be cooled with a chiller, etc., or a liquid with low vapor pressure may be used. It can be implemented as appropriate, for example, by attaching an air ejector to a water-sealed vacuum pump.
  • the temperature of the alcohol to be deaerated is preferably 10 ° C to 50 ° C, more preferably 20 ° C to 50 ° C.
  • the module structure and the filling method of the hollow fiber membrane may be configured so that turbulent flow does not occur in the degassed water.
  • the diameter is preferably 70 ⁇ m to 370 ⁇ m, more preferably 150 ⁇ m to 280 ⁇ m.
  • the inner diameter of the hollow fiber membrane is preferably in the range of 30 ⁇ m to 310 ⁇ m, and more preferably in the range of 80 ⁇ m to 220 ⁇ m.
  • the membrane area is preferably in the range of 0.018 m 2 to 120 m 2 , more preferably in the range of 1.8 to 40 m 2 , and even more preferably in the range of 7 to 20 m 2 .
  • the hollow fiber membrane module used in the present invention has the characteristics that it can easily suppress the turbulent flow of the liquid to be degassed, has excellent pressure resistance, has a simple structure, and is easy to manufacture.
  • the hollow fiber cocoon-shaped sheet there is no limitation on the form of the hollow fiber cocoon-shaped sheet, and there is no particular limitation on the nonwoven fabric, knitted fabric, woven fabric, etc.
  • the hollow fiber membrane is a weft or warp, and other yarns such as monofilament yarn or multifilament yarn made of polyester, etc. Is a knitted or woven fabric organized as warp or weft.
  • FIG. 1 shows an example of an apparatus for degassing alcoholic beverages (raw liquor) using an external reflux type hollow fiber membrane module suitably used in the present invention.
  • reference numeral 11 is a pressure reducing valve
  • reference numeral 12 is a hollow fiber gas permeable membrane
  • reference numeral 13 is a vacuum pump
  • reference numeral 14 is a flow switch
  • reference numeral 15 is an electromagnetic valve
  • reference numeral 16 is a constant flow valve.
  • Alcohol (raw liquor) passes through the pressure reducing valve 11 and is introduced into the external reflux type hollow fiber membrane module 12.
  • the inside of the hollow fiber membrane of the external reflux type hollow fiber membrane module 12 is decompressed by the vacuum pump 13, and dissolved gas is removed from the liquor (raw liquor) flowing outside the hollow fiber membrane.
  • the deaerated liquor (raw liquor) is supplied to the outside of the apparatus through the flow switch 14.
  • the flow switch 14 is activated by the flow of alcoholic beverages (raw liquor) through the degassing device, the vacuum pump 13 is turned on, and the electromagnetic valves 15 and 15 are opened.
  • the liquor (raw liquor) that has passed through the deaerator 2 is transferred to the storage container 3 and aged.
  • the liquor is less susceptible to fragrance, taste, and color degradation compared to the case where it is not degassed, and in the skin layer.
  • the resin odor is reduced as compared with the case of degassing by contacting with the porous layer.
  • the above effect is exhibited by bringing the dissolved gas in water or an aqueous solution into contact with the skin layer and degassing, so the type of alcohol is not particularly limited.
  • % Or more of the beverage it should be diluted to include a beverage with an alcohol content of 1% or more, or a powdered product that can be dissolved to give a beverage with an alcohol content of 1% or more, Either sparkling liquor represented by beer or sparkling liquor, brewed liquor represented by fruit liquor such as sake or wine such as Japanese liquor, distilled liquor represented by whiskey or shochu, or mixed liquor may be used. Distilled liquors are preferred, and brewed liquors are particularly preferred.
  • the evaluation method in this example was performed as follows unless otherwise specified. About sensory evaluation, the resin odor and the touch were evaluated. In addition, the resin odor is “scent associated with plastic, paper pack odor” (Jin Utsunomiya, three others, “quality evaluation terms and standard samples regarding flavor in sensory evaluation analysis of sake”, [online], 2006, Incorporated administrative agency Liquor Research Institute, page 3, table 1, "resin odor", search date September 25, 2015, http://www.nrib.go.jp/data/pdf/seikoumihou.pdf) It shall be defined as feeling evaluation.
  • the sensory evaluation results are shown by summing up the evaluation results of five panelists trained using a standard sample (40 ml of sake in a 50 ml polypropylene centrifuge tube and placed in boiling water for 10 minutes).
  • the strength when a resin odor was sensed was evaluated on a scale of 1 (not felt), 2 (not felt almost), 3 (somewhat felt), 4 (feeled), 5 (strong), 6 (feels very strong). .
  • the case where the average value was 1 or more and less than 2 was evaluated as ⁇ , the case where it was 2 or more and less than 3 as ⁇ , the case where it was 3 or more and less than 4 as ⁇ , and the case where it was 4 or more as ⁇ .
  • Example 1 The external reflux type hollow fiber membrane module is made of DIC Corporation "EF-020G-A30" (skin layer (outer layer) and a porous layer (inner side) having a hollow fiber pore diameter of 5 to 20 nm laminated with an asymmetric membrane. Using 4-methylpentene-1 resin hollow fiber membrane), the module was washed with ultrapure water for 72 hours before the test, and the inside of the module was dried with sterile air. Further, it was washed with clean water (23 ° C.) for 3 minutes.
  • the above-mentioned external reflux type hollow fiber membrane module was incorporated using a deaeration device “Kyowa type membrane deaeration device” manufactured by Kyowa Corporation. After passing through the module, the sake (DOI before degassing, DOI 8.5 ppm made by Doi Sake Brewery) was deaerated (absolute pressure 2.4 kPa), and the resulting raw sake (dehydrated) Sensory evaluation of DO value 0.8 ppm after gas treatment was performed. The sensory evaluation results are shown in Table 1.
  • Comparative Example 2 The procedure was the same as Comparative Example 1 except that “washed with clean water for 3 minutes” instead of “cleaned with clean water for 3 hours”. In addition, DO value after the deaeration process of the obtained raw sake was 2.0 ppm. The sensory evaluation results are shown in Table 1.
  • Comparative Example 3 The procedure was the same as Comparative Example 1 except that “washed with caustic soda (2 wt% product) for 2 hours” instead of “washed with clean water for 3 minutes”. In addition, DO value after the deaeration process of the obtained raw sake was 2.0 ppm. The sensory evaluation results are shown in Table 1.
  • Comparative Example 5 The same procedure as in Comparative Example 1 was performed except that “washed with warm water (38 ° C.) for 2 hours” instead of “washed with clean water for 3 minutes”. In addition, DO value after the deaeration process of the obtained raw sake was 2.0 ppm. The sensory evaluation results are shown in Table 1.
  • Example 1 From the sensory evaluation analysis described above, in Example 1, it is possible to obtain a sake without adding an unpleasant odor such as a plastic odor by simply washing the hollow fiber membrane module in contact with the original liquor in the skin layer (dense layer) with simple water washing. I understood. The sensory evaluation test also revealed that the drastic decrease in dissolved gas resulted in a softer touch than the original liquor and improved liquor quality. In contrast, the comparative product using the hollow fiber membrane module in contact with the raw liquor in the porous layer could not remove the resin odor no matter what washing method was tried.

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Abstract

The purpose of the present invention is to provide: an alcohol production method in which, by using a hollow-fiber membrane module, a resin smell is suppressed and a dissolved gas in an alcohol is deaerated; and an alcohol deaeration method in which, by using a hollow-fiber membrane module, a resin smell is suppressed and a dissolved gas in an alcohol is deaerated. More specifically, an alcohol production method including a step for deaerating a dissolved gas from an alcohol by using a hollow-fiber membrane module, wherein the method is characterized in that the hollow-fiber membrane used in the hollow-fiber membrane module includes a skin layer and a porous layer, and the skin layer comes into contact with the alcohol and becomes wet. The present invention provides an alcohol deaeration method in which a dissolved gas is deaerated from an alcohol by using a hollow-fiber membrane module, wherein the method is characterized in that the hollow-fiber membrane used in the hollow-fiber membrane module includes a skin layer and a porous layer, and the skin layer comes into liquid contact with the alcohol.

Description

酒類の製造方法および酒類の脱気方法Liquor production method and liquor degassing method
　本発明は、脱気工程を有する酒類の脱気方法および当該方法を用いる酒類の製造方法に関する。 The present invention relates to a method for degassing alcoholic beverages having a degassing step and a method for producing alcoholic beverages using the method.
　従来から醸造酒、特に清酒において好ましくない香りである老香の発生や着色が、清酒成分の酸化に由来することが知られている。更には、充てん時に火入れ処理を行わない生酒においては、通常の火入れ酒に比べて二倍程度の溶存酸素を含んでおり、品質の劣化も火入れ酒に比べて早いことが知られている。該酸化は清酒中の溶存酸素濃度を低減することで抑制され、製造時の好ましい品質を長期間持続させることができることが知られている（例えば特許文献１参照）。また、こうした効果を得るためには清酒中の溶存酸素濃度は出来るだけ低く、例えば約０．５ｐｐｍ以下であることが望ましいとされるが、清酒中の溶存酸素濃度と好ましい品質の保存性の相関について、具体的に比較検討されたデータは示されてない。そこで、溶存酸素を特定の濃度範囲に抑え、生酒中の酵素類の活動を抑え込むことによって、長期保存して酒類の香り、味、色の劣化を抑える、醸造酒の製造方法が提供されている（例えば特許文献２参照）。 Conventionally, it has been known that the generation and coloring of scent, which is an unfavorable scent in brewed sake, especially refined sake, is derived from oxidation of the sake components. Furthermore, it is known that fresh sake that is not subjected to a quenching process when filled contains about twice as much dissolved oxygen as a normal sparked sake, and the deterioration in quality is faster than that of a sparked sake. It is known that the oxidation is suppressed by reducing the concentration of dissolved oxygen in sake, and that a desirable quality during production can be maintained for a long time (see, for example, Patent Document 1). In order to obtain such an effect, the dissolved oxygen concentration in sake should be as low as possible, for example, about 0.5 ppm or less. However, the correlation between the dissolved oxygen concentration in sake and the preservative quality is preferable. There is no specific data that has been compared. Therefore, there is provided a method for producing brewed liquor that keeps dissolved oxygen within a specific concentration range and suppresses the activities of enzymes in fresh liquor, thereby suppressing deterioration of the aroma, taste, and color of the liquor for a long period of time. (For example, refer to Patent Document 2).
特開平６－１４１８４０号公報JP-A-6-141840 特開２０００－３０８４８２号公報JP 2000-308482 A
　しかし、当該方法は溶存酸素を中空糸膜を用いた脱気モジュールで脱気することについては、具体的な記載がなく、このため通常の多孔質膜を有する中空糸膜を用いた脱気モジュールで脱気すると、酒類と樹脂製の多孔質層とが接液することで、樹脂臭が移り香として残るという問題があった。 However, there is no specific description about degassing dissolved oxygen with a degassing module using a hollow fiber membrane in the method, and therefore, a degassing module using a hollow fiber membrane having a normal porous membrane. When degassing, the liquor and the resin porous layer come into contact with each other, so that there is a problem that the resin odor is transferred and remains as an incense.
　そこで本発明が解決しようとする課題は、中空糸膜モジュールを用い、樹脂臭を抑えつつ、且つ酒類中の溶存気体を脱気する、酒類の製造方法、および、中空糸膜モジュールを用い、樹脂臭を抑えつつ、且つ酒類中の溶存気体を脱気する、酒類の脱気方法を提供することにある。 Therefore, the problem to be solved by the present invention is to use a hollow fiber membrane module, suppress the resin odor, and degas the dissolved gas in the liquor, and use the hollow fiber membrane module to obtain a resin. An object of the present invention is to provide a method for degassing alcoholic beverages, which suppresses odor and degassed dissolved gas in alcoholic beverages.
　本願発明者らは種々の検討を行った結果、スキン層が酒類と接液する中空糸膜モジュールを用いることで、樹脂臭を抑えつつ、且つ酒類中の溶存気体を脱気する、酒類の脱気方法および酒類の製造方法を提供することができることを見出し、本発明を完成するに至った。 As a result of various studies, the inventors of the present application have used a hollow fiber membrane module in which the skin layer is in contact with liquor, thereby suppressing the resin odor and degassing the dissolved gas in the liquor. The present inventors have found that it is possible to provide an air method and a method for producing alcoholic beverages, and have completed the present invention.
　すなわち、本発明は、中空糸膜モジュールを用いて酒類から溶存気体を脱気する工程を有する酒類の製造方法であって、前記中空糸膜モジュールに用いられる中空糸膜がスキン層と多孔質層とを有し、かつ、スキン層が酒類と接液することを特徴とする酒類の製造方法に関する。 That is, the present invention relates to a method for producing an alcoholic beverage comprising a step of degassing dissolved gas from alcoholic beverages using a hollow fiber membrane module, wherein the hollow fiber membrane used in the hollow fiber membrane module comprises a skin layer and a porous layer. And a skin layer is in contact with the liquor.
　また、本発明は、中空糸膜モジュールを用いて酒類から溶存気体を脱気する工程を有する酒類の製造方法であって、前記中空糸膜モジュールに用いられる中空糸膜がスキン層と多孔質層とを有し、かつ、スキン層が酒類と接液することを特徴とする酒類の脱気方法に関する。 The present invention also relates to a method for producing an alcoholic beverage comprising a step of degassing dissolved gas from alcoholic beverages using a hollow fiber membrane module, wherein the hollow fiber membrane used in the hollow fiber membrane module comprises a skin layer and a porous layer. And a skin layer is in contact with the liquor.
　本発明によれば、中空糸膜モジュールを用い、樹脂臭を抑えつつ、且つ酒類中の溶存気体を脱気する、酒類の製造方法、および、中空糸膜モジュールを用い、樹脂臭を抑えつつ、且つ酒類中の溶存気体を脱気する、酒類の脱気方法を提供することができる。 According to the present invention, while using a hollow fiber membrane module, while suppressing the resin odor and degassing the dissolved gas in the liquor, and using the hollow fiber membrane module, while suppressing the resin odor, In addition, it is possible to provide a method for degassing alcoholic beverages by degassing dissolved gases in the alcoholic beverages.
 以下、本発明について詳細に説明するが、本発明はこれらの実施形態例のみに限定されるものではない。また、本発明の酒類の製造方法において、醸造により原酒（新酒）を製造するまでの工程は周知なため、省略する。醸造工程を経て得られた原酒は濾過装置に通し、原酒中に残存する微生物、微粒子などを除去し（濾過工程）、その後、脱気装置により、原酒中の気体成分を除去する（脱気工程）。脱気された原酒は、貯蔵容器に移し、貯蔵する。    Hereinafter, the present invention will be described in detail, but the present invention is not limited only to these embodiment examples. Further, in the method for producing an alcoholic beverage of the present invention, the steps until the production of the original sake (new sake) by brewing are well known and are omitted. The raw liquor obtained through the brewing process is passed through a filtration device to remove microorganisms and fine particles remaining in the raw liquor (filtering step), and then the gas components in the raw liquor are removed by a degassing device (degassing step). ). The deaerated raw liquor is transferred to a storage container and stored.
　濾過工程は、濾過装置を用い、活性炭による濾過およびフィルターによる濾過の二工程で概略構成されている。まず、活性炭による濾過を行うことで、後工程における原酒の香り、味、色を矯正し、その後の劣化を抑制する。次に、フィルターによる濾過を行うことで、活性炭に吸着されなかった微生物、微粒子などを除去する。この時用いられるフィルターは、濾過速度との兼ね合いにもよるが、酒質を低下させず、かつ雑菌汚染の原因となる微生物を除去できる程度の目の細かさを有するものを使用することが好ましい。 The filtration step is roughly composed of two steps of filtration with activated carbon and filtration with a filter using a filtration device. First, by filtering with activated carbon, the aroma, taste, and color of the original sake in the subsequent process are corrected, and subsequent deterioration is suppressed. Next, by performing filtration using a filter, microorganisms, fine particles, and the like that have not been adsorbed on the activated carbon are removed. Although the filter used at this time depends on the balance with the filtration rate, it is preferable to use a filter that does not lower the quality of the liquor and has a fineness enough to remove microorganisms that cause contamination with bacteria. .
　次に脱気工程は、濾過工程を経て得られた原酒を、脱気装置に送り、溶存気体を除去する。この時、原酒中の溶存酸素を減少させることで、酸化酵素類の反応を抑制し、被酸化性物質との反応を阻害することができる。 Next, in the degassing step, the raw liquor obtained through the filtration step is sent to a degassing device to remove dissolved gas. At this time, by reducing the dissolved oxygen in the raw liquor, the reaction of oxidases can be suppressed and the reaction with the oxidizable substance can be inhibited.
　脱気後の原酒中の溶存酸素量は０．０１～１０ｐｐｍの範囲であることが好ましく、さらに０．５～４ｐｐｍの範囲であることがより好ましい。本発明に用いることのできる脱気装置としては、内部環流型中空糸膜モジュールや外部環流型中空糸膜モジュールが挙げられ、当該モジュールを用いて、中空糸膜モジュール内を流れる酒類から溶存気体を脱気する。この内、外部環流型中空糸膜モジュールは、内部環流型中空糸膜モジュールよりも脱気効率に優れ、且つ水の流動圧力損失を極めて低水準に抑えることが可能であり、特に多量の酒類を脱気処理する場合に最も好ましいだけでなく、より樹脂臭を低減できるため好ましい。 The amount of dissolved oxygen in the raw sake after deaeration is preferably in the range of 0.01 to 10 ppm, and more preferably in the range of 0.5 to 4 ppm. Examples of the deaeration device that can be used in the present invention include an internal recirculation type hollow fiber membrane module and an external recirculation type hollow fiber membrane module, and the module is used to remove dissolved gas from liquors flowing in the hollow fiber membrane module. Deaerate. Of these, the outer recirculation type hollow fiber membrane module is superior in degassing efficiency to the inner recirculation type hollow fiber membrane module, and can suppress the flow pressure loss of water to a very low level. Not only is it most preferable when performing a deaeration process, but it is preferable because the resin odor can be further reduced.
　本発明に用いる中空糸膜モジュールに使用する中空糸膜は、膜構造が、少なくともスキン層（緻密層）、細孔を有する層（多孔質層）とが積層しているものであれば、通常、脱気モジュールとして用いられるものを制限なく使用できるが、さらに以下のものが好適に用いられる。 The hollow fiber membrane used in the hollow fiber membrane module used in the present invention is usually provided that the membrane structure is a laminate of at least a skin layer (dense layer) and a layer having a pore (porous layer). Although what is used as a deaeration module can be used without a restriction | limiting, the following are used suitably.
　本発明に用いる中空糸膜の素材は、疎水性の高い素材よりなる膜が好ましく、例えばポリ（４－メチルペンテン－１）樹脂等のポリオレフィン系樹脂が好ましい。また膜構造は、少なくともスキン層（緻密層）と、細孔を有する層（多孔質層）とが積層していれば特に限定されるものではないが、好ましくはスキン層（緻密層）と細孔を有する支持層（多孔質層）とが積層した不均質膜であることが好ましく、さらに、外側にスキン層（緻密層）、内側に細孔を有する支持層（多孔質層）とが積層した不均質膜であることがより好ましい。当該細孔の孔径は特に限定されないが、０～１００ｎｍの範囲が好ましく、０．１～５０ｎｍの範囲がより好ましい。 The material of the hollow fiber membrane used in the present invention is preferably a membrane made of a highly hydrophobic material, for example, a polyolefin resin such as poly (4-methylpentene-1) resin. The film structure is not particularly limited as long as at least a skin layer (dense layer) and a layer having pores (porous layer) are laminated, but preferably a skin layer (dense layer) and a fine layer are formed. It is preferably a heterogeneous film in which a support layer (porous layer) having pores is laminated, and a skin layer (dense layer) on the outside and a support layer (porous layer) having pores on the inside are laminated. More preferred is a heterogeneous film. The pore diameter is not particularly limited, but is preferably in the range of 0 to 100 nm, more preferably in the range of 0.1 to 50 nm.
　本発明に用いる中空糸膜モジュールに使用する中空糸膜は、膜の酸素透過速度が０．１×１０－５～５０００×１０－５［ｃｍ３（ＳＴＰ）／ｃｍ２・ｓｅｃ・ｃｍＨｇ］の範囲のものが好ましく、さらに０．５×１０－５～５００×１０－５［ｃｍ３（ＳＴＰ）／ｃｍ２・ｓｅｃ・ｃｍＨｇ］の範囲のものがより好ましく、さらに０．９×１０－５～１００×１０－５［ｃｍ３（ＳＴＰ）／ｃｍ２・ｓｅｃ・ｃｍＨｇ］の範囲のものが最も好ましい。 The hollow fiber membrane used in the hollow fiber membrane module used in the present invention has an oxygen transmission rate of 0.1 × 10 −5 to 5000 × 10 −5 [cm 3 (STP) / cm 2 · sec · cmHg]. The range is preferably 0.5 × 10 −5 to 500 × 10 −5 [cm 3 (STP) / cm 2 · sec · cmHg], more preferably 0.9 × 10 −5. A range of ˜100 × 10 −5 [cm 3 (STP) / cm 2 · sec · cmHg] is most preferable.
　また、本発明に用いる中空糸膜モジュールに使用する中空糸膜は、酸素と窒素の分離係数α=（ＱＯ２：酸素透過量／ＱＮ２：窒素透過量＝ １～５の範囲のものが好ましく、さらに１～４．５の範囲のものがより好ましく、さらに３．０～４．２の範囲のものが特に好ましい。当該範囲内であれば、実質的に液体として水およびアルコールを透過させず、かつ、溶存酸素濃度を数ｐｐｂ以下まで脱気することが容易になり好ましい。 The hollow fiber membrane used in the hollow fiber membrane module used in the present invention preferably has a separation factor of oxygen and nitrogen α = (QO 2 : oxygen permeation amount / QN 2 : nitrogen permeation amount = 1 to 5). Further, a range of 1 to 4.5 is more preferable, and a range of 3.0 to 4.2 is particularly preferable, and within this range, water and alcohol are not substantially permeated as a liquid. In addition, it is easy to deaerate the dissolved oxygen concentration to several ppb or less, which is preferable.
　なお、モジュールの脱気性能は中空糸膜の隔膜の酸素透過速度が高くなるにつれ一般に向上するが、これに伴い液体の透過速度も大きなものとなるため、両特性のバランスに優れた隔膜を選択することが望ましい。 The deaeration performance of the module generally improves as the oxygen transmission rate of the hollow fiber membrane increases, but the liquid transmission rate increases accordingly, so select a membrane with a good balance between both characteristics. It is desirable to do.
　また、酸素透過速度の測定及び気体分離係数αはＡＳＴＭ－Ｄ１４３４に準拠して容易に行われる。 Also, the measurement of the oxygen transmission rate and the gas separation coefficient α are easily performed according to ASTM-D1434.
　特にポリ（４－メチルペンテン－１）樹脂を素材とする中空糸不均質膜は酸素、窒素、炭酸ガス等のガス透過性に優れ且つ水蒸気バリヤー性が高く好ましい。本不均質膜については、例えば特公平２－３８２５０号公報、特公平２－５４３７７号公報、特公平４－１５０１４号公報、特公平４－５００５３号公報及び特開平５－６６５６号公報等に詳しく述べてある。 In particular, a hollow fiber heterogeneous membrane made of poly (4-methylpentene-1) resin is preferable because it is excellent in gas permeability of oxygen, nitrogen, carbon dioxide, etc. and has high water vapor barrier properties. The inhomogeneous membrane is described in detail, for example, in JP-B-2-38250, JP-B-2-54377, JP-B-4-15014, JP-B-4-50053 and JP-A-5-6656. It is stated.
　本発明で用いる中空糸膜モジュールが内部環流型の場合、内部還流型中空糸膜モジュールの中空糸膜外（気相側）の圧力を減圧下に保ちつつ、中空糸膜内（液相側）から通液して脱気する。
　一方、本発明で用いる中空糸膜モジュールが外部環流型の場合、外部還流型中空糸膜モジュールの中空糸膜内（気相側）の圧力を減圧下に保ちつつ、中空糸膜外（液相側）から通液して脱気する。いずれの場合も、液相側がスキン層（緻密層）、気相側が細孔を有する層（多孔質層）となるようにする。 When the hollow fiber membrane module used in the present invention is an internal reflux type, the pressure outside the hollow fiber membrane (gas phase side) of the internal reflux type hollow fiber membrane module is kept under reduced pressure, while inside the hollow fiber membrane (liquid phase side) Pass through and deaerate.
On the other hand, when the hollow fiber membrane module used in the present invention is an external reflux type, the pressure inside the hollow fiber membrane (gas phase side) of the external reflux type hollow fiber membrane module is kept under reduced pressure while the outside of the hollow fiber membrane (liquid phase) Side)) to deaerate. In either case, the liquid phase side is a skin layer (dense layer), and the gas phase side is a layer having pores (porous layer).
　中空糸膜モジュールの中空糸膜内の気相側圧力は、使用流量と目的とする処理後の溶存酸素量に合わせて調整することが重要であるが、蒸気によるアルコールの透過を抑えるため、脱気する酒類のその温度での飽和蒸気圧以上の圧力に設定することが好ましい。 It is important to adjust the gas-phase pressure in the hollow fiber membrane of the hollow fiber membrane module according to the flow rate used and the amount of dissolved oxygen after the target treatment. It is preferable to set the pressure to be equal to or higher than the saturated vapor pressure at the temperature of the liquor concerned.
　その際、減圧手段は単に真空ポンプ等で排気しても良いが、適当なスイープガスを流しながら真空ポンプで排気しても良い。特定の溶存気体を除去する場合には、スイープガスを併用する方法は有効である。例えば、溶存酸素や炭酸ガスのみを除去する事が重要な場合には、スイープガスとして窒素ガス、アルゴンガス等が有効に用いられる。真空ポンプを用いる場合には公知のものを用いることができ、例えば、油回転式ポンプ、ダイヤフラム式ポンプ、水流アスピレータ、水封式真空ポンプ、ブースター付水封式真空ポンプ、ルーツ型及びスクロール型等のドライ型真空ポンプ等が挙げられる。また、油回転式ポンプに油水分離装置を付属して使用してもよく、また水封式ポンプの封水をチラー等で冷却したり、蒸気圧の低い封液を使用してもよく、また水封式真空ポンプに空気エゼクターを付属して使用する等適宜実施できる。 At that time, the decompression means may be evacuated simply by a vacuum pump or the like, but may be evacuated by a vacuum pump while flowing an appropriate sweep gas. When removing a specific dissolved gas, a method using a sweep gas in combination is effective. For example, when it is important to remove only dissolved oxygen or carbon dioxide, nitrogen gas, argon gas, or the like is effectively used as the sweep gas. When using a vacuum pump, known ones can be used, for example, an oil rotary pump, a diaphragm pump, a water flow aspirator, a water ring vacuum pump, a water ring vacuum pump with a booster, a roots type, a scroll type, etc. And dry type vacuum pumps. The oil rotary pump may be used with an oil / water separator, the water seal of the water ring pump may be cooled with a chiller, etc., or a liquid with low vapor pressure may be used. It can be implemented as appropriate, for example, by attaching an air ejector to a water-sealed vacuum pump.
　脱気する酒類の温度に特に制限はないが、液温は高いほうが好ましい。液温を高くすることにより多量の酒類を効率良く脱気することができるばかりでなく、液温上昇により必然的に飽和水蒸気圧も上昇し、したがって膜の気相側の真空圧力を高めることができ、これにより真空装置の負荷を軽減することができ極めて好ましい。脱気する液温は１０℃～５０℃が好ましくさらに好ましくは２０℃～５０℃である。 There is no particular limitation on the temperature of the alcohol to be deaerated, but a higher liquid temperature is preferable. By increasing the liquid temperature, not only can a large amount of liquor be efficiently degassed, but the increase in liquid temperature inevitably increases the saturated water vapor pressure, thus increasing the vacuum pressure on the gas phase side of the membrane. This makes it possible to reduce the load on the vacuum apparatus, which is extremely preferable. The liquid temperature for deaeration is preferably 10 ° C to 50 ° C, more preferably 20 ° C to 50 ° C.
　モジュールの構造及び中空糸膜の充填方法は脱気される水に遍流が発生しないように構成されておれば良く、例えば特許公開平２－１０２７１４号公報等に好適ないくつかのモジュール構造が開示されている。 The module structure and the filling method of the hollow fiber membrane may be configured so that turbulent flow does not occur in the degassed water. For example, there are several module structures suitable for Japanese Patent Publication No. 2-102714. It is disclosed.
　本発明に用いる中空糸膜モジュールに適用する中空糸膜の寸法は、中空糸膜の外径が小さい方が、その簾巻き体の径が小さくとも大きな膜面積を得ることができ、従って、外径は７０μm～３７０μmであることが好ましく、さらに１５０μm～２８０μmであることがより好ましい。一方、中空糸膜の内径は３０μｍ～３１０μｍの範囲が好ましく、さらに８０μｍ～２２０μｍの範囲がより好ましい。膜面積は０．０１８ｍ２～１２０ｍ２の範囲であることが好ましく、１．８～４０ｍ２の範囲がより好ましく、さらに７～２０ｍ２の範囲が特に好ましい。 As for the dimensions of the hollow fiber membrane applied to the hollow fiber membrane module used in the present invention, the smaller the outer diameter of the hollow fiber membrane, the larger the membrane area can be obtained even if the diameter of the wound body is small. The diameter is preferably 70 μm to 370 μm, more preferably 150 μm to 280 μm. On the other hand, the inner diameter of the hollow fiber membrane is preferably in the range of 30 μm to 310 μm, and more preferably in the range of 80 μm to 220 μm. The membrane area is preferably in the range of 0.018 m 2 to 120 m 2 , more preferably in the range of 1.8 to 40 m 2 , and even more preferably in the range of 7 to 20 m 2 .
　本発明に用いる中空糸膜モジュールは、脱気する液体の遍流を容易に抑制でき、且つ耐圧性に優れ、構造が単純であり、また製造が容易である特徴を有する。中空糸簾状シートの形態に制限はなく不織布体、編み物、織物等特に制限はないが、好ましくは、中空糸膜を緯糸または経糸とし、他の糸たとえばポリエステル等からなるモノフィラメント糸またはマルチフィラメント糸を経糸または緯糸として組織された編み物または織物である。 The hollow fiber membrane module used in the present invention has the characteristics that it can easily suppress the turbulent flow of the liquid to be degassed, has excellent pressure resistance, has a simple structure, and is easy to manufacture. There is no limitation on the form of the hollow fiber cocoon-shaped sheet, and there is no particular limitation on the nonwoven fabric, knitted fabric, woven fabric, etc. Preferably, the hollow fiber membrane is a weft or warp, and other yarns such as monofilament yarn or multifilament yarn made of polyester, etc. Is a knitted or woven fabric organized as warp or weft.
　本発明において好適に使用される外部還流型中空糸膜モジュールを用いた酒類（原酒）からの脱気装置の一例を図１に示す。図中符号１１は減圧弁、符号１２は中空糸状気体透過膜、符号１３は真空ポンプ、符号１４はフロースイッチ、符号１５は電磁弁、符号１６は定流量弁である。 FIG. 1 shows an example of an apparatus for degassing alcoholic beverages (raw liquor) using an external reflux type hollow fiber membrane module suitably used in the present invention. In the figure, reference numeral 11 is a pressure reducing valve, reference numeral 12 is a hollow fiber gas permeable membrane, reference numeral 13 is a vacuum pump, reference numeral 14 is a flow switch, reference numeral 15 is an electromagnetic valve, and reference numeral 16 is a constant flow valve.
　酒類（原酒）は、減圧弁１１を通り、外部還流型中空糸膜モジュール１２に導入される。外部還流型中空糸膜モジュール１２の中空糸膜内は、真空ポンプ１３によって減圧され、中空糸膜外を流れる酒類（原酒）から溶存気体が除去される。脱気処理された酒類（原酒）は、フロースイッチ１４を通って装置外に供給される。このフロースイッチ１４は、脱気装置中を酒類（原酒）が流れることで作動し、真空ポンプ１３のスイッチを入れ、電磁弁１５、１５を開けるようになっている。脱気装置２を通過した酒類（原酒）を貯蔵容器３に移し、熟成させる。 Alcohol (raw liquor) passes through the pressure reducing valve 11 and is introduced into the external reflux type hollow fiber membrane module 12. The inside of the hollow fiber membrane of the external reflux type hollow fiber membrane module 12 is decompressed by the vacuum pump 13, and dissolved gas is removed from the liquor (raw liquor) flowing outside the hollow fiber membrane. The deaerated liquor (raw liquor) is supplied to the outside of the apparatus through the flow switch 14. The flow switch 14 is activated by the flow of alcoholic beverages (raw liquor) through the degassing device, the vacuum pump 13 is turned on, and the electromagnetic valves 15 and 15 are opened. The liquor (raw liquor) that has passed through the deaerator 2 is transferred to the storage container 3 and aged.
　以上の通り、酒類（原酒）は、中空糸膜モジュールにより溶存酸素量が抑えられているので、脱気していない場合と比較して香り、味、色の劣化を起こし難く、さらにスキン層で酒類と接液して脱気することにより、多孔質層で接液して脱気する場合と比較して樹脂臭も低減されたものとなっている。本願発明は、製造工程において、水または水溶液中の溶存気体をスキン層と接液させて脱気させることで上記効果を発揮することから、酒類の種類は特に限定されず、例えば、アルコール分１％以上の飲料であればよく、薄めてアルコール分１％以上の飲料とすることができるもの、または、溶解してアルコール分１％以上の飲料とすることができる粉末状のものを含むものとし、ビールや発泡酒に代表される発泡性酒類、日本酒等の清酒やワイン等の果実酒に代表される醸造酒類、ウィスキーや焼酎に代表される蒸留酒類、混成酒類いずれでもよいが、この中でも醸造酒類、蒸留酒類が好ましく、特に醸造酒類が好ましく挙げられる。 As described above, since the amount of dissolved oxygen is suppressed by the hollow fiber membrane module, the liquor (raw liquor) is less susceptible to fragrance, taste, and color degradation compared to the case where it is not degassed, and in the skin layer. By degassing by contacting with alcohol, the resin odor is reduced as compared with the case of degassing by contacting with the porous layer. In the present invention, in the production process, the above effect is exhibited by bringing the dissolved gas in water or an aqueous solution into contact with the skin layer and degassing, so the type of alcohol is not particularly limited. % Or more of the beverage, it should be diluted to include a beverage with an alcohol content of 1% or more, or a powdered product that can be dissolved to give a beverage with an alcohol content of 1% or more, Either sparkling liquor represented by beer or sparkling liquor, brewed liquor represented by fruit liquor such as sake or wine such as Japanese liquor, distilled liquor represented by whiskey or shochu, or mixed liquor may be used. Distilled liquors are preferred, and brewed liquors are particularly preferred.
　以下、本発明を実施例により具体的に説明するが、本発明はこれら実施例にのみ限定されるものではない。 Hereinafter, the present invention will be specifically described by way of examples. However, the present invention is not limited to these examples.
（官能評価の方法および評価基準）
　本実施例においての評価方法は、特に断りのない限り、以下の通りに行った。
　官能評価について、樹脂臭と舌触りを評価した。
　なお、樹脂臭とは、「プラスチックを連想する香り、紙パック臭」（宇都宮仁、他３名、”清酒の官能評価分析における香味に関する品質評価用語及び標準見本”、〔ｏｎｌｉｎｅ〕、２００６年、独立行政法人酒類総合研究所、第３頁第１表「樹脂臭」、検索日平成２７年９月２５日、http://www.nrib.go.jp/data/pdf/seikoumihou.pdf）を感じる評価と定義するものとする。 (Method and criteria for sensory evaluation)
The evaluation method in this example was performed as follows unless otherwise specified.
About sensory evaluation, the resin odor and the touch were evaluated.
In addition, the resin odor is “scent associated with plastic, paper pack odor” (Jin Utsunomiya, three others, “quality evaluation terms and standard samples regarding flavor in sensory evaluation analysis of sake”, [online], 2006, Incorporated administrative agency Liquor Research Institute, page 3, table 1, "resin odor", search date September 25, 2015, http://www.nrib.go.jp/data/pdf/seikoumihou.pdf) It shall be defined as feeling evaluation.
　官能評価の結果は標準見本（５０ｍｌポリプロピレン製遠心管に４０ｍｌ清酒を入れ、１０分間沸騰水中につけたもの）を用いて訓練されたパネラー５名の評価結果を集計して示した。 
　樹脂臭を感知したときの強度を１（感じない）、２（ほとんど感じない）、３（やや感じる）、４（感じる）、５（強い）、６（とても強く感じる）の６段階で評価した。集計した平均値が１以上～２未満の場合を◎、２以上～３未満の場合を○、３以上～４未満の場合を△、４以上の場合を×とした。 The sensory evaluation results are shown by summing up the evaluation results of five panelists trained using a standard sample (40 ml of sake in a 50 ml polypropylene centrifuge tube and placed in boiling water for 10 minutes).
The strength when a resin odor was sensed was evaluated on a scale of 1 (not felt), 2 (not felt almost), 3 (somewhat felt), 4 (feeled), 5 (strong), 6 (feels very strong). . The case where the average value was 1 or more and less than 2 was evaluated as ◎, the case where it was 2 or more and less than 3 as ◯, the case where it was 3 or more and less than 4 as Δ, and the case where it was 4 or more as ×.
　また、脱気処理前の原酒に対する脱気処理後の原酒の舌触りの柔かさを官能評価し、１（とても感じる）、２（感じる）、３（やや感じる）、４（感じない）の４段階で評価した。集計した平均値が１以上～２未満の場合を○、２以上～３未満の場合を△、３以上～４以下の場合を×とした。集計した平均値が１以上～２未満の場合を◎、２以上～３未満の場合を○、３以上～４未満の場合を△、４の場合を×とした。 In addition, sensory evaluation of the softness of the original sake after deaeration treatment with respect to the original sake before deaeration treatment, 4 levels of 1 (feel very), 2 (feel), 3 (somewhat feel), 4 (not feel) It was evaluated with. The case where the average value was 1 or more and less than 2 was evaluated as ○, the case where it was 2 or more and less than 3 as Δ, and the case where it was 3 or more and 4 or less as x. The case where the aggregated average value was 1 or more and less than 2 was evaluated as ◎, the case where it was 2 or more and less than 3 as ○, the case where it was 3 or more and less than 4 as Δ, and the case where it was 4 as x.
（実施例１）
　外部還流型中空糸膜モジュールは、ＤＩＣ株式会社製「ＥＦ－０２０Ｇ－Ａ３０」（スキン層（外層）と中空糸孔径５～２０ｎｍの多孔質層（内側）とが積層した非対称膜を有するポリ－4－メチルペンテン－１樹脂製中空糸膜）を用い、試験前に超純水で７２時間洗浄後、モジュール内部を無菌エアーで乾燥した。さらに、上水（２３℃）で３分間洗浄した。 Example 1
The external reflux type hollow fiber membrane module is made of DIC Corporation "EF-020G-A30" (skin layer (outer layer) and a porous layer (inner side) having a hollow fiber pore diameter of 5 to 20 nm laminated with an asymmetric membrane. Using 4-methylpentene-1 resin hollow fiber membrane), the module was washed with ultrapure water for 72 hours before the test, and the inside of the module was dried with sterile air. Further, it was washed with clean water (23 ° C.) for 3 minutes.
　株式会社協和コーポレーション製脱気装置「協和式膜脱気装置」を用い、上記外部還流型中空糸膜モジュールを組み込んだ。モジュール通液後、日本酒（土井酒造場製「開運　特別本醸造　火入酒」脱気処理前ＤＯ値８．５ｐｐｍ）を脱気処理（絶対圧２．４ｋＰａ）した後、得られた原酒（脱気処理後ＤＯ値０．８ｐｐｍ）の官能評価を行った。官能評価結果を表１に示した。 The above-mentioned external reflux type hollow fiber membrane module was incorporated using a deaeration device “Kyowa type membrane deaeration device” manufactured by Kyowa Corporation. After passing through the module, the sake (DOI before degassing, DOI 8.5 ppm made by Doi Sake Brewery) was deaerated (absolute pressure 2.4 kPa), and the resulting raw sake (dehydrated) Sensory evaluation of DO value 0.8 ppm after gas treatment was performed. The sensory evaluation results are shown in Table 1.
（比較例１）
　外部還流型中空糸膜モジュールＤＩＣ株式会社製「ＥＦ－０２０Ｇ－Ａ３０」の替りに、内部還流型中空糸膜モジュール三菱レイヨン社製「２０Ｍ３４００Ａ」（非多孔質の超薄膜を多孔質層でサンドイッチ状に挟み込んだ三層複合構造を有するポリエチレン製対称膜）を用いたこと以外は実施例１と同様に行った。なお、得られた原酒の脱気処理後ＤＯ値は２．０ｐｐｍであった。官能評価結果を表１に示した。 (Comparative Example 1)
Instead of “EF-020G-A30” manufactured by DIC Corporation, external reflux type hollow fiber membrane module “20M3400A” manufactured by Mitsubishi Rayon Co., Ltd. (non-porous ultra-thin film sandwiched between porous layers) This was carried out in the same manner as in Example 1 except that a polyethylene symmetrical film having a three-layer composite structure sandwiched between the two was used. In addition, DO value after the deaeration process of the obtained raw sake was 2.0 ppm. The sensory evaluation results are shown in Table 1.
（比較例２）
　「上水で３分間洗浄した」の替りに「上水で３時間洗浄した」こと以外は比較例１と同様に行った。なお、得られた原酒の脱気処理後ＤＯ値は２．０ｐｐｍであった。官能評価結果を表１に示した。 (Comparative Example 2)
The procedure was the same as Comparative Example 1 except that “washed with clean water for 3 minutes” instead of “cleaned with clean water for 3 hours”. In addition, DO value after the deaeration process of the obtained raw sake was 2.0 ppm. The sensory evaluation results are shown in Table 1.
（比較例３）
　「上水で３分間洗浄した」の替りに「苛性ソーダ（2ｗｔ％品）で２時間洗浄した」こと以外は比較例１と同様に行った。なお、得られた原酒の脱気処理後ＤＯ値は２．０ｐｐｍであった。官能評価結果を表１に示した。 (Comparative Example 3)
The procedure was the same as Comparative Example 1 except that “washed with caustic soda (2 wt% product) for 2 hours” instead of “washed with clean water for 3 minutes”. In addition, DO value after the deaeration process of the obtained raw sake was 2.0 ppm. The sensory evaluation results are shown in Table 1.
（比較例４）
　「上水で３分間洗浄した」の替りに「オゾン水で１時間洗浄した」こと以外は比較例１と同様に行った。なお、得られた原酒の脱気処理後ＤＯ値は２．０ｐｐｍであった。官能評価結果を表１に示した。 (Comparative Example 4)
It carried out similarly to the comparative example 1 except having been "washed with ozone water for 1 hour" instead of "washed with clean water for 3 minutes." In addition, DO value after the deaeration process of the obtained raw sake was 2.0 ppm. The sensory evaluation results are shown in Table 1.
（比較例５）
　「上水で３分間洗浄した」の替りに「温水（３８℃）で２時間洗浄した」こと以外は比較例１と同様に行った。なお、得られた原酒の脱気処理後ＤＯ値は２．０ｐｐｍであった。官能評価結果を表１に示した。 (Comparative Example 5)
The same procedure as in Comparative Example 1 was performed except that “washed with warm water (38 ° C.) for 2 hours” instead of “washed with clean water for 3 minutes”. In addition, DO value after the deaeration process of the obtained raw sake was 2.0 ppm. The sensory evaluation results are shown in Table 1.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
　以上の官能評価分析より、実施例１ではスキン層（緻密層）で原酒と接する中空糸膜モジュールを簡単な水洗浄を行うのみで、プラスチック臭などの異臭の添加がない日本酒が得られることが分かった。また、溶存気体の大幅な減少によって、原酒よりも舌触りが柔らかく、酒質が向上したことも官能評価試験から明らかになった。これに対して、多孔質層で原酒と接する中空糸膜モジュールを用いた比較品は、例え、どのような洗浄方法を試みたとしても、樹脂臭の除去ができなかった。 From the sensory evaluation analysis described above, in Example 1, it is possible to obtain a sake without adding an unpleasant odor such as a plastic odor by simply washing the hollow fiber membrane module in contact with the original liquor in the skin layer (dense layer) with simple water washing. I understood. The sensory evaluation test also revealed that the drastic decrease in dissolved gas resulted in a softer touch than the original liquor and improved liquor quality. In contrast, the comparative product using the hollow fiber membrane module in contact with the raw liquor in the porous layer could not remove the resin odor no matter what washing method was tried.

Claims (8)

  1. 中空糸膜モジュールを用いて酒類から溶存気体を脱気する工程を有する酒類の製造方法であって、前記中空糸膜モジュールに用いられる中空糸膜がスキン層と多孔質層とを有し、かつ、スキン層が酒類と接液することを特徴とする酒類の製造方法。 A method for producing liquor comprising a step of degassing dissolved gas from liquor using a hollow fiber membrane module, wherein the hollow fiber membrane used in the hollow fiber membrane module has a skin layer and a porous layer, and A method for producing an alcoholic beverage, wherein the skin layer is in contact with the alcoholic beverage.
  2. 膜面積が０．０１８ｍ２～１２０ｍ２の範囲である請求項１記載の酒類の製造方法。 The method for producing an alcoholic beverage according to claim 1, wherein the membrane area is in the range of 0.018 m 2 to 120 m 2 .
  3. 酸素透過量と窒素透過量の比（ＱＯ２／ＱＮ２）が、１～５の範囲である請求項１記載の酒類の製造方法。 The method for producing an alcoholic beverage according to claim 1, wherein the ratio of oxygen permeation amount to nitrogen permeation amount (QO 2 / QN 2 ) is in the range of 1 to 5.
  4. 中空糸膜が４－メチル－ペンテン－１からなる請求項１記載の酒類の製造方法。 The method for producing an alcoholic beverage according to claim 1, wherein the hollow fiber membrane comprises 4-methyl-pentene-1.
  5. 脱気後の溶存酸素量は０．０１～１０ｐｐｍの範囲である請求項１記載の酒類の製造方法。 The method for producing an alcoholic beverage according to claim 1, wherein the amount of dissolved oxygen after deaeration is in the range of 0.01 to 10 ppm.
  6. 脱気前に、脱気する酒類で中空糸膜モジュール内を共洗いする工程を有する請求項１記載の酒類の製造方法。 The method for producing an alcoholic beverage according to claim 1, further comprising a step of co-washing the inside of the hollow fiber membrane module with an alcoholic beverage to be degassed before degassing.
  7. 酒類が清酒、ワイン、ウィスキーまたは焼酎である請求項１記載の酒類の製造方法。 The method for producing an alcoholic beverage according to claim 1, wherein the alcoholic beverage is sake, wine, whiskey or shochu.
  8. 中空糸膜モジュールを用いて酒類から溶存気体を脱気する、酒類の脱気方法であって、前記中空糸膜モジュールに用いられる中空糸膜がスキン層と多孔質層とを有し、かつ、スキン層が酒類と接液することを特徴とする酒類の脱気方法。 A degassing method for liquors, wherein a dissolved gas is degassed from liquor using a hollow fiber membrane module, wherein the hollow fiber membrane used in the hollow fiber membrane module has a skin layer and a porous layer, and A method for degassing alcoholic beverages, wherein the skin layer comes into contact with alcoholic beverages.
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JP6979556B1 (en) * 2020-12-18 2021-12-15 恵二 渡辺 Residual and deterioration control system for naturally effervescent carbon dioxide in alcoholic beverages

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JPH06141840A (en) * 1992-11-05 1994-05-24 Miura Kenkyusho:Kk Production of sake @(3754/24)rice wine) or the like
JPH06335623A (en) * 1993-05-28 1994-12-06 Dainippon Ink & Chem Inc Deaerating film and deaerating method
JPH07116483A (en) * 1993-10-26 1995-05-09 Dainippon Ink & Chem Inc Manufacture of hollow fiber dual membrane
JPH07170952A (en) * 1993-12-21 1995-07-11 Toppan Printing Co Ltd Method for filling beverage
JPH10165165A (en) * 1996-12-09 1998-06-23 Mitsubishi Rayon Co Ltd Storage of liquors
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JPH0436178A (en) * 1990-05-31 1992-02-06 Miura Co Ltd Method for preventing liquid beverage from oxidizing
JPH06141840A (en) * 1992-11-05 1994-05-24 Miura Kenkyusho:Kk Production of sake @(3754/24)rice wine) or the like
JPH06335623A (en) * 1993-05-28 1994-12-06 Dainippon Ink & Chem Inc Deaerating film and deaerating method
JPH07116483A (en) * 1993-10-26 1995-05-09 Dainippon Ink & Chem Inc Manufacture of hollow fiber dual membrane
JPH07170952A (en) * 1993-12-21 1995-07-11 Toppan Printing Co Ltd Method for filling beverage
JPH10165165A (en) * 1996-12-09 1998-06-23 Mitsubishi Rayon Co Ltd Storage of liquors
US6402818B1 (en) * 2000-06-02 2002-06-11 Celgard Inc. Degassing a liquid with a membrane contactor
US20150258500A1 (en) * 2014-03-13 2015-09-17 Celgard, Llc Asymmetric membranes and related methods

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6979556B1 (en) * 2020-12-18 2021-12-15 恵二 渡辺 Residual and deterioration control system for naturally effervescent carbon dioxide in alcoholic beverages

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