JP4584178B2 - Liquor purification method - Google Patents
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- JP4584178B2 JP4584178B2 JP2006109811A JP2006109811A JP4584178B2 JP 4584178 B2 JP4584178 B2 JP 4584178B2 JP 2006109811 A JP2006109811 A JP 2006109811A JP 2006109811 A JP2006109811 A JP 2006109811A JP 4584178 B2 JP4584178 B2 JP 4584178B2
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Description
本発明は、酒類、例えば穀物類などを原料として作られる醸造酒、蒸留酒等の精製方法に関し、特に穀物類を原料とした蒸留酒の精製方法に関する。 The present invention relates to a method for purifying brewed liquor, distilled liquor and the like made from alcoholic beverages such as cereals, and more particularly to a method for purifying distilled liquor using cereals as raw materials.
酒類には、主成分であるアルコールのほかに、香り成分、味成分、色素成分、ミネラル成分、アルデヒド類、無機塩類等が含まれている。これらの内のアルデヒド類、無機塩類は、精製によって除去することが好ましい。従来、酒類からアルデヒド類、無機塩類を除去するための精製装置として、イオン交換樹脂を用いた焼酎精製装置が知られている。特に、ＨＳＯ3形強塩基性アニオン交換樹脂を用いたアルデヒド除去装置と、このアルデヒド除去装置の後段に設けられたＨ形強酸性カチオン交換樹脂およびＯＨ形強塩基性アニオン交換樹脂の混床を用いた脱塩装置とからなる焼酎精製装置は広く用いられている（特許文献１）。この焼酎精製装置によれば、香りを若干は残しつつ、辛味、渋味、苦味を除去して軽快な飲み口の焼酎を得ることができる。 In addition to alcohol as a main component, alcoholic beverages include fragrance components, taste components, pigment components, mineral components, aldehydes, inorganic salts, and the like. Of these, aldehydes and inorganic salts are preferably removed by purification. Conventionally, a shochu refining device using an ion exchange resin is known as a refining device for removing aldehydes and inorganic salts from alcoholic beverages. In particular, an aldehyde removing apparatus using HSO 3 type strongly basic anion exchange resin and a mixed bed of H type strongly acidic cation exchange resin and OH type strongly basic anion exchange resin provided at the subsequent stage of this aldehyde removing apparatus are used. A shochu refining apparatus comprising a conventional desalting apparatus is widely used (Patent Document 1). According to this shochu refining apparatus, it is possible to remove the pungent, astringent and bitter tastes while leaving a little fragrance, and to obtain a light drinking shochu.
最近では、いろいろな種類の本格焼酎が市場に出まわるにつれて、特徴的な香りや味を有する本格焼酎を好む人が増えてきた。しかし、前述した特許文献１記載の焼酎精製装置は、香り成分や味成分の除去性能が高いため、香りを強く残したり、癖のある味を残したりした焼酎の精製にはほとんど用いられていなかった。その理由は、Ｈ形強酸性カチオン交換樹脂とＯＨ形強塩基性アニオン交換樹脂との混床を用いた脱塩装置を使用した場合、無機塩類の除去時に、香り成分である酢酸エチル等のエステル類や味を決める成分の一種である有機酸類も多く除去されてしまうからである。 Recently, as various kinds of authentic shochu are on the market, more and more people prefer authentic shochu with a characteristic aroma and taste. However, since the shochu refining apparatus described in Patent Document 1 described above has a high ability to remove scent components and taste components, it is rarely used for refining shochu that leaves a strong scent or a taste with a scent. It was. The reason is that when a desalting apparatus using a mixed bed of an H-type strongly acidic cation exchange resin and an OH-type strongly basic anion exchange resin is used, an ester such as ethyl acetate, which is a scent component, is removed when removing inorganic salts. This is because many organic acids, which are a kind of components that determine taste and taste, are also removed.
そのため、香りを強く残したり、癖のある味を残したりした焼酎を特許文献１記載の従来装置を用いて得ようとする場合は、エステル類や有機酸類の除去性能を下げるために、酒類とアルデヒド除去装置および脱塩装置のイオン交換樹脂層との接触時間を短くしたり、アルデヒド除去処理および脱塩処理を行った酒類と、これらの処理を行わない原液とを混合したりしていた。しかし、これらの方法では、アルデヒド類や無機塩類の除去が不十分になることがあった。 Therefore, when trying to obtain shochu with a strong aroma or a savory taste using the conventional apparatus described in Patent Document 1, in order to reduce the removal performance of esters and organic acids, The contact time with the ion exchange resin layer of an aldehyde removal apparatus and a desalination apparatus was shortened, or liquors which performed the aldehyde removal process and the desalination process were mixed with the undiluted | stock solution which does not perform these processes. However, in these methods, removal of aldehydes and inorganic salts may be insufficient.
これに対し、本発明者は、醸造酒、蒸留酒等の酒類から、独特の香りを強く残したり癖のある味を残したりしつつ、アルデヒド類と無機塩類を効果的に除去することができる酒類の精製方法として、酒類をＨＳＯ3形スチレン系強塩基性アニオン交換樹脂層に通液した後に、Ｈ形強酸性カチオン交換樹脂および遊離塩基形弱塩基性スチレン系またはアクリル系アニオン交換樹脂の混床層に通液する酒類の精製方法を提案している（特許文献２）。この方法によれば、精製後の酒類におけるエステルの残存量が格段に増える。 On the other hand, the present inventor can effectively remove aldehydes and inorganic salts from alcoholic beverages such as brewed liquor and distilled liquor while leaving a strong scent or a savory taste. As a method for purifying liquor, after passing the liquor through an HSO 3 type styrenic strong base anion exchange resin layer, a mixture of H type strong acid cation exchange resin and free base type weakly basic styrenic or acrylic anion exchange resin. A method for purifying liquors that pass through the floor layer has been proposed (Patent Document 2). According to this method, the residual amount of ester in the refined alcoholic beverages is remarkably increased.
しかし、特許文献２の精製方法でも、酒類の独特の深みのある香りが依然として除去されることがあった。 However, even with the purification method of Patent Document 2, the unique deep aroma of liquors may still be removed.
本発明は、前述した事情に鑑みてなされたもので、醸造酒、蒸留酒等の酒類から、独特の香りを特許文献２の精製方法よりもさらに強く残したり癖のある味を残したりしつつ、アルデヒド類と無機塩類を効果的に除去することができる酒類の精製方法を提供することを目的とする。 The present invention has been made in view of the above-mentioned circumstances, while leaving a unique fragrance stronger than the refining method of Patent Document 2 from liquors such as brewed liquor and distilled liquor, and leaving a savory taste. Another object of the present invention is to provide a method for purifying alcoholic beverages that can effectively remove aldehydes and inorganic salts.
本発明は、前記目的を達成するため、酒類をＨＳＯ3形アクリル系強塩基性アニオン交換樹脂層に通液した後に、Ｈ形強酸性カチオン交換樹脂と遊離塩基形アクリル系弱塩基性アニオン交換樹脂との混床層に通液することを特徴とする酒類の精製方法を提供する。 In order to achieve the above object, the present invention, after passing liquor through an HSO 3 type acrylic strong basic anion exchange resin layer, an H type strong acidic cation exchange resin and a free base type acrylic weak basic anion exchange resin A method for purifying alcoholic beverages, characterized by being passed through a mixed bed layer.
本発明の特徴は、前段のアルデヒド除去用のアニオン交換樹脂として、ＨＳＯ3形アクリル系強塩基性アニオン交換樹脂を用いるとともに、後段の脱塩用のアニオン交換樹脂として、遊離塩基形アクリル系弱塩基性アニオン交換樹脂を用いた点にある。これにより、本発明では、精製後の酒類における香り成分や味成分の残存量、特に香り成分の残存量を多くすることができ、酒類の個性をより多く残しつつ、アルデヒド類と無機塩類を効果的に除去することが可能となる。 The feature of the present invention is that an HSO 3 type acrylic strong base anion exchange resin is used as an anion exchange resin for removing aldehyde in the previous stage, and a free base type acrylic weak base is used as an anion exchange resin for desalting in the subsequent stage. This is in the point of using anionic anion exchange resin. Thereby, in the present invention, it is possible to increase the residual amount of the scent component and taste component in the refined liquor, in particular, the residual amount of the scent component, and to make the aldehydes and inorganic salts effective while leaving more personality of the liquor. Can be removed.
すなわち、本発明では、精製に用いるアニオン交換樹脂を全てアクリル系樹脂に変更することで、疎水性の高い香り成分の除去率が低下するために、処理液に香りが強く残るものと考えられる。しかしながら、香りや味は微量成分の含有やマスキング成分の有無による影響もあるために、この考えは推測の範囲を超えていない。 That is, in the present invention, by changing all the anion exchange resins used for purification to acrylic resins, the removal rate of highly hydrophobic fragrance components decreases, and therefore, it is considered that the scent remains strongly in the treatment liquid. However, since the aroma and taste are affected by the presence of a trace component and the presence or absence of a masking component, this idea does not exceed the scope of estimation.
以下、本発明につきさらに詳しく説明する。本発明では、前段のアルデヒド除去工程において、酒類をＨＳＯ3形（亜硫酸形）アクリル系強塩基性アニオン交換樹脂層に通液する。上記ＨＳＯ3形アクリル系強塩基性アニオン交換樹脂としては、例えば、アンバーライト（登録商標、以下同じ）ＩＲＡ４５８、ＩＲＡ９５８、レバチット（登録商標、以下同じ）ＡＰ−２４７Ａ、Ｐｕｒｏｌｉｔｅ（登録商標、以下同じ）Ａ−８５０等をＨＳＯ3形にしたものを用いることができる。 Hereinafter, the present invention will be described in more detail. In the present invention, the alcoholic beverage is passed through the HSO 3 type (sulfuric acid type) acrylic strong basic anion exchange resin layer in the preceding aldehyde removing step. Examples of the HSO 3 type acrylic strong basic anion exchange resin include Amberlite (registered trademark, hereinafter the same) IRA458, IRA958, Levacit (registered trademark, the same below) AP-247A, Purolite (registered trademark, the same below). A-850 or the like in HSO 3 form can be used.
本発明では、後段の脱塩工程において、酒類をＨ形強酸性カチオン交換樹脂と遊離塩基形アクリル系弱塩基性アニオン交換樹脂との混床層に通液する。上記Ｈ形強酸性カチオン交換樹脂としては、例えば、アンバーライトＩＲＡ１２０Ｂ、ＩＲＡ１２４、２００ＣＴ、２５２、ダイヤイオンＳＫ１Ｂ、ＳＫ１１２、ＰＫ２１２、ＰＫ２１６等を用いることができる。また、遊離塩基形アクリル系弱塩基性アニオン交換樹脂としては、例えば、アンバーライトＩＲＡ６７、ダイヤイオンＷＡ１０等を用いることができる。 In the present invention, in the subsequent desalting step, the liquor is passed through a mixed bed layer of H-type strongly acidic cation exchange resin and free base-type acrylic weakly basic anion exchange resin. As the H-type strongly acidic cation exchange resin, for example, Amberlite IRA120B, IRA124, 200CT, 252, Diaion SK1B, SK112, PK212, PK216, etc. can be used. As the free base acrylic weakly basic anion exchange resin, for example, Amberlite IRA67, Diaion WA10 or the like can be used.
後段の脱塩工程におけるＨ形強酸性カチオン交換樹脂：遊離塩基形アクリル系弱塩基性アニオン交換樹脂の容量比は、１：１〜１：４程度（ただし、容量比は強酸性カチオン交換樹脂はＮａ形基準、弱塩基性アニオン交換樹脂は遊離塩基形基準での比率）とすることが適当である。 The volume ratio of H-type strongly acidic cation exchange resin: free base type acrylic weakly basic anion exchange resin in the subsequent desalting step is about 1: 1 to 1: 4 (however, the volume ratio is strong acid cation exchange resin It is appropriate that the ratio is based on the Na base and the weak base anion exchange resin based on the free base form.
本発明において、各イオン交換樹脂層（ＨＳＯ3形アクリル系強塩基性アニオン交換樹脂層、Ｈ形強酸性カチオン交換樹脂と遊離塩基形アクリル系弱塩基性アニオン交換樹脂との混床層、以下同じ）への酒類の通液温度は、−１０〜４０℃の範囲とすることが望ましい。アルコール濃度にもよるが、通液温度が−１０℃未満になると、液が凍ったり、液の粘性が増したりするため、酒類と樹脂との効率的な接触が行えなくなって、アルデヒド類や無機塩類の除去性能が低下する。通液温度が４０℃を超えると、香り成分の蒸発や変性が起こるため望ましくない。 In the present invention, each ion exchange resin layer (HSO 3 type acrylic strong basic anion exchange resin layer, mixed bed layer of H type strong acidic cation exchange resin and free base type acrylic weak base anion exchange resin, and so on) It is desirable that the liquor passing temperature to) is in the range of -10 to 40 ° C. Depending on the alcohol concentration, if the liquid passing temperature is less than −10 ° C., the liquid freezes or the viscosity of the liquid increases, making it impossible to make efficient contact between the alcoholic beverage and the resin. Salt removal performance decreases. When the liquid passing temperature exceeds 40 ° C., evaporation and denaturation of the scent component occur, which is not desirable.
また、本発明において、酒類の各イオン交換樹脂層への通液速度は、全樹脂量に対してＳＶ０．１〜５０の範囲とすることが好ましい。通液速度がＳＶ０．１未満であると、単位時間あたりの処理液量が少なくなってしまう。通液速度がＳＶ５０を超えると、酒類と樹脂との効率的な接触が行えなくなって、アルデヒド類や無機塩類の除去性能が低下する。 Moreover, in this invention, it is preferable that the liquid flow rate to each ion exchange resin layer of liquor shall be the range of SV0.1-50 with respect to the total resin amount. When the liquid passing speed is less than SV0.1, the amount of the processing liquid per unit time is reduced. When the liquid passing speed exceeds SV50, it becomes impossible to make efficient contact between the liquor and the resin, and the performance of removing aldehydes and inorganic salts decreases.
本発明によれば、原液から主にアルデヒド類と無機塩類が除去されるが、そのほかにアミノ酸類も除去されるため、本発明はアミノ酸類が多く含まれる醸造酒の精製よりも蒸留酒の精製に適している。特に、減圧蒸留よりも香りが強く残る常圧蒸留による蒸留酒の精製に適している。しかし、近年では窒素成分をほとんど含まないほど精製した穀物原料を醸造した酒類、例えば吟醸酒などもあり、これらの場合には本発明による精製を行っても求める味によっては問題がないと考えられる。なお、上記酒類の穀物原料としては、例えば、麦、芋、米、そば、黒糖、ごま、とうもろこし、こうりゃん、粟および酒粕から選ばれる１種以上が挙げられる。 According to the present invention, aldehydes and inorganic salts are mainly removed from the stock solution, but in addition to this, amino acids are also removed. Therefore, the present invention is a method for purifying distilled liquor rather than purifying brewed liquor rich in amino acids. Suitable for In particular, it is suitable for the purification of distilled liquor by atmospheric distillation where the fragrance remains stronger than the vacuum distillation. However, in recent years, there are also alcoholic beverages such as ginjo sake that have been brewed from grain materials that have been refined so that they contain almost no nitrogen component. In these cases, there is no problem depending on the taste that is sought after purification by the present invention. . Examples of the cereal raw material for the liquor include one or more selected from wheat, rice bran, rice, buckwheat, brown sugar, sesame, corn, corn, koji, and sake lees.
以上のように、本発明によれば、酒類の原液の香りをより強く残したり、独特の癖のある味を残したりしつつ、酒類の原液からアルデヒド類および無機塩類を除去することができる。 As described above, according to the present invention, it is possible to remove aldehydes and inorganic salts from a liquor stock solution while leaving the scent of the liquor stock solution stronger or leaving a unique savory taste.
図１は本発明の実施に用いる酒類の精製装置の一例を示すフロー図である。図１において、１０は濾過器、１２はＨＳＯ3形アクリル系強塩基性アニオン交換樹脂の単床層１４を備えたイオン交換装置（アルデヒド除去装置）、１６はＨ形強酸性カチオン交換樹脂と遊離塩基形アクリル系弱塩基性アニオン交換樹脂との混床層１８を備えたイオン交換装置（脱塩装置）を示す。本例の精製装置は、酒類の原液２０を濾過器１０、アルデヒド除去装置１２、脱塩装置１６に順次通液することにより、アルデヒド類および無機塩類が除去された処理液２２を得るものである。
FIG. 1 is a flow diagram showing an example of an apparatus for purifying alcohol used in the practice of the present invention. In FIG. 1, 10 is a filter, 12 is an ion exchange device (aldehyde removal device) having a
以下に、実施例により本発明をさらに詳細に説明する。ただし、本発明はこれら実施例によって限定されるものではない。 Hereinafter, the present invention will be described in more detail with reference to examples. However, the present invention is not limited to these examples.
（実施例１）
日本の焼酎よりも香りの強い蒸留酒である二鍋頭酒（中国産白酒の一種）の原液を、ＨＳＯ3形アクリル系強塩基性アニオン交換樹脂層（アンバーライトＩＲＡ４５８にＮａＨＳＯ3溶液を通液してＨＳＯ3形にしたもの）６０ｍｌに通液した後に、Ｈ形強酸性カチオン交換樹脂（アンバーライトＩＲ１２０Ｂ）２０ｍｌと遊離塩基形アクリル系弱塩基性アニオン交換樹脂（アンバーライトＩＲＡ６７）４０ｍｌとの混床層に通液温度２０℃、通液速度３００ｍｌ／ｈｒで１５００ｍｌ通液した。原液と処理液の分析結果および官能評価を表１に示す。なお、官能評価では、６名のパネルによる官能試験によって香りおよび口当たりを評価した。
Example 1
Smell of strong spirits and is two pan head sake than Japanese shochu a stock solution of (a kind of Chinese white sake), HSO 3 form acrylic strongly basic anion exchange resin layer (was passed through the NaHSO 3 solution in amber light IRA458 HSO 3 form) After passing through 60 ml, mixed bed layer of 20 ml of H-form strongly acidic cation exchange resin (Amberlite IR120B) and 40 ml of free base acrylic weakly basic anion exchange resin (Amberlite IRA67) The solution was passed through 1500 ml at a fluid passage temperature of 20 ° C. and a fluid passage speed of 300 ml / hr. Table 1 shows the analysis results and sensory evaluation of the stock solution and the treatment solution. In the sensory evaluation, the scent and mouthfeel were evaluated by a sensory test with six panels.
（比較例１：特許文献２の方法）
実施例１と同じ二鍋頭酒の原液を、ＨＳＯ3形スチレン系強塩基性アニオン交換樹脂層（アンバーライトＩＲＡ４０４にＮａＨＳＯ3溶液を通液してＨＳＯ3形にしたもの）６０ｍｌに通液した後に、Ｈ形強酸性カチオン交換樹脂（アンバーライトＩＲ１２０Ｂ）２０ｍｌと遊離塩基形アクリル系弱塩基性アニオン交換樹脂（アンバーライトＩＲＡ６７）４０ｍｌとの混床層に実施例１と同じ条件通液した。原液と処理液の分析結果および官能評価を表１に示す。
(Comparative Example 1: Method of Patent Document 2)
A stock solution of the same two pan head liquor as in Example 1, after passed through a HSO 3 form styrenic strongly basic anion exchange resin layer (what was HSO 3 form was passed through the NaHSO 3 solution Amberlite IRA404) 60ml, The same conditions as in Example 1 were passed through a mixed bed layer of 20 ml of H-form strongly acidic cation exchange resin (Amberlite IR120B) and 40 ml of free base acrylic weakly basic anion exchange resin (Amberlite IRA67). Table 1 shows the analysis results and sensory evaluation of the stock solution and the treatment solution.
（比較例２：特許文献１の方法）
実施例１と同じ二鍋頭酒の原液を、ＨＳＯ3形スチレン系強塩基性アニオン交換樹脂層（アンバーライトＩＲＡ４０４にＮａＨＳＯ3溶液を通液してＨＳＯ3形にしたもの）６０ｍｌに通液した後に、Ｈ形強酸性カチオン交換樹脂（アンバーライトＩＲ１２０Ｂ）２０ｍｌと遊離塩基形スチレン系強塩基性アニオン交換樹脂（アンバーライトＩＲＡ４０２ＢＬ）４０ｍｌとの混床層に実施例１と同じ条件で通液した。原液と処理液の分析結果および官能評価を表１に示す。
(Comparative Example 2: Method of Patent Document 1)
A stock solution of the same two pan head liquor as in Example 1, after passed through a HSO 3 form styrenic strongly basic anion exchange resin layer (what was HSO 3 form was passed through the NaHSO 3 solution Amberlite IRA404) 60ml, The mixture was passed under the same conditions as in Example 1 through a mixed bed layer of 20 ml of H-form strongly acidic cation exchange resin (Amberlite IR120B) and 40 ml of free base styrenic strongly basic anion exchange resin (Amberlite IRA402BL). Table 1 shows the analysis results and sensory evaluation of the stock solution and the treatment solution.
本実験結果より、アルデヒド除去用アニオン交換樹脂としてＨＳＯ3形アクリル系強塩基性アニオン交換樹脂、脱塩用アニオン交換樹脂として遊離塩基形アクリル系弱塩基性アニオン交換樹脂を用いた本発明によれば、脱塩用アニオン交換樹脂としてＯＨ形強塩基性アニオン交換樹脂を用いた特許文献１の方法（比較例２）と同様にアルデヒド類や導電性の塩類を除去できること、また、アルデヒド除去用アニオン交換樹脂としてＨＳＯ3形スチレン系強塩基性アニオン交換樹脂を用いた特許文献２の方法（比較例１）に比べてより強く香りを残した処理を行えることがわかる。 From the results of this experiment, according to the present invention, an HSO 3 type acrylic strong basic anion exchange resin was used as an anion exchange resin for aldehyde removal, and a free base acrylic weak base anion exchange resin was used as an anion exchange resin for desalting. Aldehydes and conductive salts can be removed in the same manner as in the method of Patent Document 1 (Comparative Example 2) using an OH-type strongly basic anion exchange resin as an anion exchange resin for desalting, and anion exchange for aldehyde removal it can be seen that perform the processing to leave a stronger scent as compared to the method of Patent Document 2 using the HSO 3 form styrenic strongly basic anion exchange resin as a resin (Comparative example 1).
１０ 濾過器
１２ アルデヒド除去装置
１４ 強塩基性アニオン交換樹脂の単床層
１６ 脱塩装置
１８ 強酸性カチオン交換樹脂と弱塩基性アニオン交換樹脂の混床層
２０ 原液
２２ 処理液
DESCRIPTION OF
Claims (3)
The method for purifying an alcoholic beverage according to claim 2, wherein the raw material of the distilled alcoholic beverage is at least one selected from wheat, rice bran, rice, buckwheat, brown sugar, sesame, corn, corn, koji, and sake lees.
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| CN103421649B (en) * | 2013-09-03 | 2014-11-05 | 赵何平 | Tartary buckwheat daqu liquor |
| JP6404574B2 (en) * | 2014-02-14 | 2018-10-10 | オルガノ株式会社 | Method and apparatus for purifying distilled liquor |
| JP6718309B2 (en) * | 2016-05-26 | 2020-07-08 | オルガノ株式会社 | Method for purifying alcohol-containing liquid and apparatus for purifying alcohol-containing liquid |
| CN108441396A (en) * | 2018-06-07 | 2018-08-24 | 程可 | A kind of more grain wine brewing formula and processing technologies |
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