JP4606848B2 - Membrane filtration method of alcoholic beverage fermentation liquid - Google Patents
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Description
本発明はアルコール飲料醗酵液の清澄化を目的とした膜濾過方法に関する。 The present invention relates to a membrane filtration method for the purpose of clarifying an alcoholic beverage fermentation solution.
アルコール飲料であるワインを例にとると、ワインはその醗酵液を濾過等により清澄化することにより得られる。ワイン醗酵液は酵母及び蛋白をはじめとする原料由来の濁質を含んでおり、これらを除去する方法として珪藻土濾過法が用いられてきた。ところが、珪藻土濾過は大量の珪藻土を必要とし、同時に分離捕捉された不純物を含むスラッジが大量に排出される問題があった。また、スラッジは焼却処理ができないため産業廃棄物として埋め立て処分する必要があり、環境保全の観点からも珪藻土濾過法に代わる濾過技術が待ち望まれてきた。その後、代替技術として膜濾過法が注目され、現在では膜濾過法が広く用いられている（特許文献１：特表２０００２−５２５１９６号公報）。 Taking wine as an alcoholic beverage as an example, wine is obtained by clarifying the fermentation liquid by filtration or the like. Wine fermentation liquor contains turbidity derived from raw materials such as yeast and protein, and diatomaceous earth filtration has been used as a method for removing these. However, diatomaceous earth filtration requires a large amount of diatomaceous earth, and at the same time, there is a problem that a large amount of sludge containing impurities separated and trapped is discharged. Further, since sludge cannot be incinerated, it must be disposed of as industrial waste, and from the viewpoint of environmental conservation, a filtration technique that replaces the diatomaceous earth filtration method has been awaited. Thereafter, a membrane filtration method has attracted attention as an alternative technique, and at present, the membrane filtration method is widely used (Patent Document 1: Japanese Translation of PCT International Publication No. 20002-525196).
しかしながら、有機膜からなる膜濾過モジュールでワイン醗酵液を濾過すると、時として風味が変化する着香現象が生じる。着香現象が生じると、元々のワインにはない香りが着いてしまい、商品価値が大きく低下する。ところで、ワインに限らずアルコール飲料の着香に関しては化学分析では検出できない超微量成分が影響することが知られている。
これに対して人間の臭覚感度は高く、極く微量でも嗅ぎ出すことができるので通常、着香の有無は官能試験で判定される。有機膜の場合、シール材やポッティング材としてエポキシ樹脂やウレタン樹脂等が使用される。また、モジュール部材として各種プラスチック材料が用いられるが、官能試験において膜及びまたは前記部材に起因する風味の変化が指摘されることがある。かくして、ワインに限らずアルコール飲料の醗酵液の濾過に用いられる膜濾過モジュールは、着香の元を除去しておくことが強く求められる。
On the other hand, human olfaction sensitivity is high, and even a very small amount can be sniffed. In the case of an organic film, an epoxy resin or a urethane resin is used as a sealing material or a potting material. In addition, various plastic materials are used as the module member, but in the sensory test, changes in the flavor caused by the film and / or the member may be pointed out. Thus, the membrane filtration module used for the filtration of not only wine but also a fermented liquor of alcoholic beverages is strongly required to remove the flavoring source.
本発明は、アルコール飲料醗酵液の濾過に起因する着香を防止した膜濾過方法の提供を目的とする。 An object of this invention is to provide the membrane filtration method which prevented the aroma resulting from filtration of alcoholic beverage fermented liquid.
本発明者は、通液前に膜濾過モジュールをアルコール水溶液で洗浄することで、前記目的を達成しうることを見出し、本発明に到達した。
すなわち、本発明は下記の通りである。
（１）有機膜及びプラスチック製のモジュール部材を備えた膜濾過モジュールでアルコール飲料の醗酵液を濾過し、清澄化するに際し、該モジュールの前記有機膜及び前記モジュール部材をあらかじめ該飲料のアルコール濃度以上の洗浄用のアルコール水溶液で洗浄し、その後、洗浄に用いたアルコールを充分に水洗し、この水洗の際には、洗浄水を前記膜濾過モジュールの一次側及び二次側の両方から流し、連続的に排出すると共に、二次側の排出量を一次側の排出量よりも多量とすることを特徴とするアルコール飲料醗酵液の膜濾過方法、
（２）前記アルコール水溶液での洗浄時間が１５時間以上であることを特徴とする（１）に記載のアルコール飲料醗酵液の膜濾過方法、
（３）前記有機膜がポリフッ化ビニリデンであることを特徴とする（１）または（２）に記載のアルコール飲料醗酵液の膜濾過方法。
The present inventor has found that the object can be achieved by washing the membrane filtration module with an aqueous alcohol solution before passing the liquid, and has reached the present invention.
That is, the present invention is as follows.
(1) When filtering and clarifying the fermented liquor of an alcoholic beverage with the membrane filtration module provided with the organic membrane and the plastic module member, the said organic membrane and the said module member of this module are more than the alcohol concentration of this drink beforehand. After washing with an aqueous alcohol solution for washing, the alcohol used for washing is washed thoroughly with water , and when washing with water, the washing water is allowed to flow from both the primary side and the secondary side of the membrane filtration module. membrane filtration method a alcohol beverage fermentation broth of specific as well as discharged, characterized in that a large amount than emissions of the primary emission of the secondary side,
(2) The membrane filtration method for an alcoholic beverage fermentation liquid according to (1) , wherein the washing time with the aqueous alcohol solution is 15 hours or more,
(3) The membrane filtration method for an alcoholic beverage fermentation solution according to (1) or (2), wherein the organic membrane is polyvinylidene fluoride .
本発明の方法に依れば、アルコール飲料醗酵液の濾過に起因する着香を防止した膜濾過方法を提供することができる。 According to the method of the present invention, it is possible to provide a membrane filtration method that prevents flavoring due to filtration of an alcoholic beverage fermentation solution.
以下、本発明について、特にその好ましい形態を中心に、具体的に説明する。
本発明は、アルコール飲料の醗酵液を有機膜からなる膜濾過モジュールで濾過し、清澄化するに際し、該モジュールをあらかじめ該飲料のアルコール濃度以上のアルコール水溶液で洗浄することを特徴とするアルコール飲料醗酵液の膜濾過方法である。
本発明において、アルコール洗浄は循環洗浄を用いることもできるが、モジュールの一次側及び二次側にアルコール水溶液を充填する方法、いわゆる浸漬洗浄が好ましい。
浸漬洗浄は循環洗浄のようにポンプを使う必要がないため引火等の危険がない。また、タンクを必要としないので使用するアルコール水溶液が少量で済む。浸漬洗浄は特に振とうの必要もなく、室温で静置するだけよい。
Hereinafter, the present invention will be specifically described focusing on its preferred form.
The present invention is an alcoholic beverage fermentation characterized in that when a fermentation liquid of an alcoholic beverage is filtered through a membrane filtration module made of an organic membrane and clarified, the module is washed in advance with an aqueous alcohol solution having an alcohol concentration higher than that of the beverage. This is a liquid membrane filtration method.
In the present invention, circulation cleaning may be used for alcohol cleaning, but a method of filling an alcohol aqueous solution on the primary side and secondary side of the module, so-called immersion cleaning is preferable.
Immersion cleaning does not require the use of a pump unlike circulating cleaning, so there is no danger of ignition. In addition, since no tank is required, a small amount of alcohol aqueous solution is used. The immersion cleaning is not particularly necessary to be shaken, and can be left at room temperature.
次に、アルコールとしては、メタノール、エタノール、イソプロピルアルコールを単独で用いることもできるし、これらの混合液を用いることもできる。但し、再生アルコールはアルコール以外の溶剤が微量含まれている場合があるので注意が必要であり、ガスクロマトグラフィー分析等で確認することが好ましい。また、洗浄に用いるアルコール水溶液はその都度、更新することが好ましい。アルコール洗浄後は充分に水洗することが好ましく、特にメタノールやイソプロピルアルコール、または変性アルコールを用いた場合は残留がないよう、充分に水洗することが好ましい。水洗の終点は、ガスクロマトグラフィーやＴＯＣ分析で把握するのが便利であり、実際には事前に水洗量とアルコール残存濃度あるいはＴＯＣ減衰速度の関係を調べておき、これを目安にするのが効率的である。 Next, as alcohol, methanol, ethanol, isopropyl alcohol can also be used independently, and these liquid mixture can also be used. However, since the regenerated alcohol may contain a trace amount of a solvent other than the alcohol, it is necessary to pay attention, and it is preferable to confirm it by gas chromatography analysis or the like. Moreover, it is preferable to update the alcohol aqueous solution used for washing | cleaning each time. It is preferable to wash thoroughly with alcohol after washing with alcohol, and in particular, when methanol, isopropyl alcohol, or denatured alcohol is used, it is preferable to wash with sufficient water so that no residue remains. It is convenient to grasp the end point of water washing by gas chromatography or TOC analysis. Actually, it is efficient to investigate the relation between the amount of water washing and residual alcohol concentration or TOC decay rate in advance and use this as a guide. Is.
また、水洗の際は図１に示すように、洗浄水を一次側（内圧型モジュールの場合のチューブ側に相当）及び二次側（内圧型モジュールの場合のシェル側に相当）の両方から流し、連続的に排出することが好ましく、一次側と二次側の排出量の比は１：１０程度が好ましい。何故ならば、膜表面に付着しているアルコールを洗い流すのは比較的容易であるのに対して、膜の厚み方向に残留しているアルコールは基本的に希釈により除去することになるので、多量の水を通過させねばならない。また、水洗水としてはイオン交換水、飲料水等が使用できる。 When washing with water, as shown in FIG. 1, flush water flows from both the primary side (corresponding to the tube side in the case of the internal pressure type module) and the secondary side (corresponding to the shell side in the case of the internal pressure type module). It is preferable to discharge continuously, and the ratio of the discharge amount on the primary side and the secondary side is preferably about 1:10. This is because it is relatively easy to wash away alcohol adhering to the film surface, whereas alcohol remaining in the thickness direction of the film is basically removed by dilution. Of water must pass through. Moreover, ion-exchange water, drinking water, etc. can be used as flush water.
次に、アルコールの濃度は、好ましくはそれぞれの被処理飲料のアルコール濃度以上であり、それ以下の濃度では洗浄効果が小さい。また、アルコール濃度の上限は、膜及びモジュール部材の耐アルコール性を勘案して決定すればよい。また、洗浄時間は１５時間以上が好ましく、より好ましくは２０時間以上である。
本発明は、膜の材質や孔径、形状さらにはモジュールの構造や形態に関係なく、有機膜及びプラスチック製部材からなるＵＦ、ＭＦモジュールに広範に用いることができるが、特に膜材質がポリフッ化ビニリデンであるモジュールに効果的である。
なお、本発明の対象であるアルコール飲料としてはワインの他、ビール、清酒等が挙げられる。
Next, the alcohol concentration is preferably equal to or higher than the alcohol concentration of the respective beverages to be treated, and if the concentration is lower than that, the cleaning effect is small. The upper limit of the alcohol concentration may be determined in consideration of the alcohol resistance of the membrane and the module member. Further, the washing time is preferably 15 hours or longer, more preferably 20 hours or longer.
The present invention can be widely used for UF and MF modules made of an organic film and a plastic member regardless of the material, pore diameter and shape of the membrane, as well as the structure and form of the module. In particular, the membrane material is polyvinylidene fluoride. Effective for modules that are
In addition, as an alcoholic beverage which is the object of the present invention, beer, sake, and the like are listed in addition to wine.
（実施例１）
旭化成ケミカルズ（株）製、商品名マイクローザＭＦモジュールＵＳＰ−１４３（中空糸膜材質ポリフッ化ビニリデン、内径１．４ｍｍ、公称孔径０．１μ、膜面積０．１２ｍ２）の一次側及び二次側に２０ｖｏｌ％のエタノール水溶液を封入し、室温で２０ｈｒ静置した。次いで、エタノール水溶液を抜き出し、イオン交換水で１時間水洗した。このモジュールを膜濾過試験機に装着し、入口圧力０．１１ＭＰａ、出口圧力０．０９ＭＰａでワイン醗酵液（赤ワイン、アルコール濃度１１．９％、濁度５３ＮＴＵ）を循環濾過した。透過液を官能試験に供した結果、３人のパネラーとも判定は風味の変化なし（着香なし）だった。
Example 1
Asahi Kasei Chemicals Co., Ltd., trade name Microsa MF module USP-143 (hollow fiber membrane material polyvinylidene fluoride, inner diameter 1.4 mm, nominal pore diameter 0.1 μm, membrane area 0.12 m 2 ) primary side and secondary side 20 vol% ethanol aqueous solution was sealed in and left at room temperature for 20 hr. Next, the aqueous ethanol solution was extracted and washed with ion-exchanged water for 1 hour. This module was mounted on a membrane filtration tester, and a wine fermentation liquid (red wine, alcohol concentration 11.9%, turbidity 53 NTU) was circulated and filtered at an inlet pressure of 0.11 MPa and an outlet pressure of 0.09 MPa. As a result of subjecting the permeate to a sensory test, all three panelists judged no change in flavor (no flavoring).
（比較例１）
通液前にモジュールをエタノールで洗浄しなかった以外は実施例１と同様の試験を行った。官能試験の結果は、３人のパネラーの判定とも着香ありだった。
(Comparative Example 1)
The same test as in Example 1 was performed except that the module was not washed with ethanol before passing. The results of the sensory test were perfumed with the judgment of the three panelists.
（比較例２）
膜濾過モジュールとして旭化成ケミカルズ（株）製、商品名マイクローザＭＦモジュールＷＳＰ−１４３（中空糸膜材質ポリオレフィン、内径１．４ｍｍ、公称孔径０．１μ、膜面積０．０９ｍ２）を用い、通液前にモジュールをエタノール水溶液で洗浄しなかった以外は実施例１と同様の試験を行った。官能試験の結果は、３人中１人のパネラーの判定が着香ありだった。
(Comparative Example 2)
Asahi Kasei Chemicals Co., Ltd., trade name Microza MF module WSP-143 (hollow fiber membrane material polyolefin, inner diameter 1.4 mm, nominal pore diameter 0.1 μm, membrane area 0.09 m 2 ) was used as a membrane filtration module. The same test as in Example 1 was performed except that the module was not previously washed with an aqueous ethanol solution. As a result of the sensory test, one of the three panelists judged that there was a fragrance.
（比較例３）
エタノールの濃度を５ｖｏｌ％、封入時間を２０時間とした以外は実施例１と同様の試験を行った。官能試験の結果は、３人中２人のパネラーの判定が着香ありだった。
(Comparative Example 3)
The same test as in Example 1 was performed except that the ethanol concentration was 5 vol% and the encapsulation time was 20 hours. The sensory test showed that 2 out of 3 panelists were scented.
本発明は、アルコール飲料を膜濾過する工程で好適に用いることができる。 The present invention can be suitably used in the step of membrane filtering an alcoholic beverage.
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| JPH01270906A (en) * | 1988-04-21 | 1989-10-30 | Gessner & Co Gmbh | Microporous membrane for filtering beer |
| JPH06500236A (en) * | 1991-01-07 | 1994-01-13 | フェジェラション デ コーポラシイフ ミグロ | dealcoholization method |
| JPH08289759A (en) * | 1995-04-25 | 1996-11-05 | Ikedachiyou | Powder for extracting flavor of water-chestnut, extraction of flavor of water-chestnut and preparation of water-chestnut liqueur |
| JPH1146747A (en) * | 1997-08-05 | 1999-02-23 | Mercian Corp | Production of red wine |
| WO2001028667A1 (en) * | 1999-10-22 | 2001-04-26 | Asahi Kasei Kabushiki Kaisha | Heat-resistant microporous film |
| JP2002525196A (en) * | 1998-09-25 | 2002-08-13 | ポール・コーポレーション | Filtration system and method |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01270906A (en) * | 1988-04-21 | 1989-10-30 | Gessner & Co Gmbh | Microporous membrane for filtering beer |
| JPH06500236A (en) * | 1991-01-07 | 1994-01-13 | フェジェラション デ コーポラシイフ ミグロ | dealcoholization method |
| JPH08289759A (en) * | 1995-04-25 | 1996-11-05 | Ikedachiyou | Powder for extracting flavor of water-chestnut, extraction of flavor of water-chestnut and preparation of water-chestnut liqueur |
| JPH1146747A (en) * | 1997-08-05 | 1999-02-23 | Mercian Corp | Production of red wine |
| JP2002525196A (en) * | 1998-09-25 | 2002-08-13 | ポール・コーポレーション | Filtration system and method |
| WO2001028667A1 (en) * | 1999-10-22 | 2001-04-26 | Asahi Kasei Kabushiki Kaisha | Heat-resistant microporous film |
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