JP3644467B2 - Manufacturing method for purified persimmon - Google Patents
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- JP3644467B2 JP3644467B2 JP19157596A JP19157596A JP3644467B2 JP 3644467 B2 JP3644467 B2 JP 3644467B2 JP 19157596 A JP19157596 A JP 19157596A JP 19157596 A JP19157596 A JP 19157596A JP 3644467 B2 JP3644467 B2 JP 3644467B2
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Description
【０００１】
【発明の属する技術分野】
本発明は古くから清酒その他の酒類製造時の清澄化目的に用いられ、食品、化粧品、製紙、又は繊維産業の分野においても広く使用されている柿渋の精製方法に関し、さらに詳しくは従来製品の問題点、即ち▲１▼特有の臭気があり、細菌的にも不衛生である、▲２▼不純物の影響で保存中に皮膜を形成し欠減が生じる、▲３▼柿の品種、収穫時期によりタンニン濃度が異なり、タンニン濃度を一定にした安定商品を供給するにはブレンドという方法しかなく、製造上限界がある、等を全て解消し、しかもタンニン濃度を自由に調整して、濃縮品も加水調整品も製造することができる精製柿渋及びその安価で効率的な製造法に関する。
【０００２】
【従来の技術】
従来の柿渋の製造技術は古くから伝えられてきた方法で、まず原料渋柿を搾汁して汁液を得、これを容器に入れて常温で放置し自然に静置発酵させて搾汁中の糖質を微生物により資化させて取り除き、その後熟成を行っていた。この工程中に揮発性の有機酸（酢酸；Ｍｗ６０、プロピオン酸；Ｍｗ７４、酪酸；Ｍｗ８８）が副製し、これらが柿渋臭気の原因となっていた。さらに加熱殺菌をし（火入れを行い）、通常２〜３年間常温度で放置熟成させたものが商品となっていた。この商品は凝集性を示す成分を残してその他の高分子不純物を沈殿除去したもので、有機酸、無機物など多量の低分子物質を含んでいるため、常法の濃縮法では限界があり、従って製品としての柿渋濃度はボーメ５〜６°でタンニンの力価は１５０程度のものであった。しかも製造期間も長く必要とした。
【０００３】
ここで言うタンニン力価は、コロイド滴定法（国税庁所定分析法注解、ｐ３３７、（財）日本醸造協会発行、昭和５６年）に従って測定した値である。即ち、タンニン力価は負コロイドである柿タンニンにそれ以上の正コロイドであるメチルグリコールキトサンを一定量加えて反応させ、余ったメチルグリコールキトサン量を負コロイドであるポリビニル硫酸カリウムで滴定し、盲検値との差し引きをもって柿タンニン量とする定量法で求められ、柿渋原液１ｍｌ当たりのＮ／４００ポリビニル硫酸カリウム滴定値をもって表示する。
【０００４】
柿渋は天然物からの製造であるから、その品質も厳密にはかなり多様性で、性質面でも差異がある。柿渋は熟成中に化学的な変化を伴い、官能的にも色、香り、粘調性等が異なり、減圧濃縮しても特有の臭気は完全に除去できない。自然発酵の代わりに柿渋を殺菌した後、酵母（ Saccharomyces bayanus ）を加えて発酵させて糖質を資化させる改良方法が開発されているが、発酵時に発泡が著しく製造装置的に問題がある。また柿の産地、収穫年次及び熟度などによって糖組成が異なるために、糖質の資化性が一様でなく、全ての原料で完全無臭化することが難しい等の問題がある。しかも前述した如く低分子の含有不純物が多いために、常法の濃縮法では高タンニン力価のものが安定して製造できなかった。
【０００５】
【発明が解決しようとする課題】
そのため、発酵法による糖質の資化除去、減圧濃縮に代わって、溶媒抽出法、クロマトグラム法による吸着・分離方法、イオン交換法、逆浸透法、凍結濃縮法などを検討したが、いずれもいくつかの欠点があって実用的ではなかった。即ち、溶媒抽出法では有機溶媒を多量に使用するため作業上危険が伴い、クロマトグラム法やイオン交換法では回収率が悪くコスト高となり、逆浸透法や凍結濃縮法では柿渋臭気が完全に除去できない等の欠点があった。
【０００６】
本発明はかかる従来技術の欠点を解消するために創案されたものであり、その目的は膜孔径による分子サイズのふるい分けを機能とする限外濾過膜を使用して、溶媒である水と共に低分子物質を除去することにより柿渋特有の臭気を取り除き、かつ濃度を自由に調整して濃縮品も加水調整品も得ることができる精製柿渋及びその安価で効率的な製造方法を提供することにある。
【０００７】
【課題を解決するための手段】
本発明者はかかる目的を達成するために限外濾過膜を使用して柿渋の低分子成分を除去する方法について鋭意検討した結果、遂に本発明の完成に至った。
【０００８】
即ち、本発明は渋柿より搾汁して得られた原料柿渋搾汁液を好ましくは５５〜１００℃、より好ましくは７０〜９０℃に加熱し、その液を、分子量が３０００より小さい物質を透過させる限外濾過膜を使用して、好ましくは２０〜９５℃で、より好ましくは４０〜６０℃で循環濾過することによって、水と共に低分子成分を除去する工程を含むことを特徴とする精製柿渋の製造法である。
【０００９】
また、本発明は酢酸、プロピオン酸、酪酸を含む揮発性有機酸、グルコース、フルクトースを含む糖質及び無機物を含む、分子量１０００以下の低分子成分が除去されていることを特徴とする精製柿渋である。
【００１０】
【発明の実施の形態】
本発明で使用する原料柿渋搾汁液は、原料渋柿として、岐阜県産の田村柿、京都府産の天王柿、愛媛県産の愛宕柿、福島県産の会津柿などを使用し、まずタニナカ式粉砕機により柿実を細かくした後、庄田式圧搾機（スクリュープレス）で搾汁して固液分離を行うことによって得られるものである。このとき副産物として生成される残渣の粕は廃棄される。ここで得られる搾汁液は柿渋の主成分である柿タンニンとともに臭気の原因となる揮発性有機酸、無機物及び糖質等が多く含まれている。
【００１１】
次に、こうして得られた柿渋搾汁液を加熱して殺菌し、熱凝固性の物質を凝固させた後、例えば濾過又は遠心分離により透明な濾液とする。このときの加熱温度は５５〜１００℃、好ましくは７０〜９０℃で３０秒以上保持することが好ましい。柿渋は主に清酒の清澄剤として使用されているため、清酒の腐敗菌である火落ち菌の混入を防止するため５５℃以上の加熱殺菌が必要であり、またそれ以外の酵母菌や細菌を効率よく殺菌するため瞬間殺菌として７０℃以上で１〜２分間保持することが好ましい。
【００１２】
濾過法では、濾過助剤として使用されている珪藻土を柿渋搾汁液重量の０．２〜５％の割合で搾汁液に添加して濾過するか、あるいは前もってプレコートした濾過機を用いることが好ましい。
また遠心分離法では、高速に回転するバケットの中に柿渋搾汁液を送り込み、回転によって生じる遠心力により連続的に固液分離する。この方法は珪藻土濾過が困難な場合に使用する。
【００１３】
次に、こうして得られた透明な濾液を、限外濾過膜を使用して循環濾過することにより、低分子成分を除去する。限外濾過膜としては、酢酸セルロース、ポリフッ化ビニリデン、ポリアクリロニトリル、ポリカーボネート、ポリオレフィンなどの合成高分子多孔質膜、耐熱性、耐ｐＨ性及び耐薬品性があり、熱殺菌できるポリエーテルスルホン膜やポリスルホン膜、あるいは有機溶剤耐性のポリイミド膜やセラミック膜が挙げられる。
【００１４】
限外濾過における濾過プロセスとしては、加圧濾過法、減圧濾過法などがあり、濾過タイプとしては一過式、多段一過式、循環方式などがあるが、工業的に安価に効率良く生産するには循環濾過方式が好ましい。このときの液温は２０〜９５℃、好ましくは３０〜８０℃、さらに好ましくは４０〜６０℃に保持する。かかる温度範囲で循環濾過すると濾過効率が良くかつ雑菌混入が防止でき、膜自体のダメージも少なくすることができる。
【００１５】
本発明者は対象とする原料柿渋の性状や限外濾過の操作条件を考慮し検討した結果、▲１▼柿タンニンの分子量は約４５００以上である、▲２▼耐熱性がある、▲３▼低いｐＨでも耐性がある（柿渋のｐＨは３〜４）、▲４▼柿タンニン分子の膜面への付着が少ない、▲５▼高温でアルカリ洗浄できる（柿渋の付着はアルカリ洗浄が最も効果的である）、等を満足しなければならないことがわかった。これらの条件を満足する柿渋の精製法として、分画分子量３０００以上でポリエーテルスルホン膜、ポリスルホン膜又はセラミック膜で作られている中空糸モジュールの限外濾過膜を使用した濾過装置を用いた、加圧濾過法による循環濾過が最も好ましいことを見出した。
【００１６】
以上のように限外濾過膜を使用して柿渋を精製することによって、柿渋に溶存している臭気原因物質である多量の揮発性有機酸、無機物、糖質等の分画分子量以下の低分子物質は効率良く膜を透過し、一方で柿タンニンは膜で阻止され、適宜濃縮することによってタンニン濃度（コロイド力価）２００以上の無臭の柿渋製品を得ることができる。また得られた柿渋製品は加水又は濃縮調整することによって１３０以上の製品規格値のタンニン濃度（コロイド力価）の範囲で所望の製品を得ることができる。
【００１７】
【実施例】
本発明を以下の実施例によって具体的に説明するが、本発明はこれらに限定されるものではない。
なお、実施例中のタンニン力価は国税庁所定分析法注解、ｐ３３７（（財）日本醸造協会発行、昭和５６年）に従って測定し、有機酸は高速液体クロマトグラフィー（ Shim - pack SCR −１０２Ｈ 島津製作所（株）製）によって分析した。また臭気の測定はパネラー１０名による官能検査で行い、１０名全員が明らかに臭気を感じた場合に「柿渋臭」と表示し、１０名全員が明らかに臭気を感じなかった場合に「完全無臭」と表示した。さらにタンニン回収率は（タンニン力価×柿渋容量）を限外濾過前及び限外濾過後について計算し、それらの値から１００×〔（限外濾過後）／（限外濾過前）〕を計算して求めた。
【００１８】
実施例 １
渋柿（岐阜県産の田村柿、平成５年収穫）１０００Ｋｇを庄田式圧搾機を用いて搾汁液６００ｌを得た。これをプレートヒーターにて８０℃に昇温後、１分間保持し、火入れの後、珪藻土６Ｋｇを添加し、撹拌によるボデイエイドを行い、濾過圧搾機（薮田式、９０Ｆ、５ｍ2 ）を用いて透明な液とした。
【００１９】
この濾液（固形分濃度５％、タンニン力価１３０、酸度２．１、ｐＨ３．７）３００ｌをポリエーテルスルホン膜の中空糸モジュール（ダイセル化学工業（株）製；分画分子量；１００００、８９φ×１１２９Ｌ×５本、総膜面積２５ｍ2 ）の限外濾過装置を用いて０．８〜１．２Ｋｇ／ｃｍ2 のゲージ圧で５０〜６０℃に保温しながら循環させた。加水、濃縮を繰り返し、３時間後に透過希薄液３９８０ｌ、濃縮柿渋液１４０ｌが得られた。この時の透過速度は５３．１ｌ／ｍ2 ・ｈｒであった。この濃縮柿渋製品（タンニン力価２６０）と加水調整した柿渋製品（タンニン力価１３０）を従来方法による柿渋製品（上記の透明な液）と比較したデータを表１に示した。タンニン回収率は９３％であった。
【００２０】
【表１】
実施例 ２
渋柿（京都府産の天王柿、平成３年収穫）１０００Ｋｇを庄田式圧搾機を用いて搾汁液６４０ｌを得た。これをプレートヒーターにて９０℃に昇温後、１分間保持し、火入れの後、珪藻土７Ｋｇを添加し、撹拌によるボデイエイドを行い、濾過圧搾機（薮田式、９０Ｆ、５ｍ2 ）を用いて透明な液とした。
【００２２】
この濾液（固形分濃度８％、タンニン力価１６０、酸度１．８、ｐＨ３．９）３２０ｌをポリスルホン膜の中空糸モジュール（（株）クラレ製；分画分子量；１３０００、１１４φ×１１００Ｌ×５本、総膜面積２５ｍ2 ）の限外濾過装置を用いて０．８〜１．２Ｋｇ／ｃｍ2 のゲージ圧で４５〜５５℃に保温しながら循環させた。加水、濃縮を繰り返し、３時間後に透過希薄液３３７０ｌ、濃縮柿渋液１５０ｌが得られた。この時の透過速度は４４．９ｌ／ｍ2 ・ｈｒであった。この濃縮柿渋製品（タンニン力価３２０）と加水調整した柿渋製品（タンニン力価１６０）を従来方法による柿渋製品（上記の透明な液）と比較したデータを表２に示した。タンニン回収率は９４％であった。
【００２３】
【表２】
実施例 ３
渋柿（愛媛県産の愛宕柿、平成４年収穫）１０００Ｋｇを庄田式圧搾機を用いて搾汁液６２０ｌを得た。これをプレートヒーターにて７０℃に昇温後、２分間保持し、火入れの後、珪藻土７Ｋｇを添加し、撹拌によるボデイエイドを行い、濾過圧搾機（薮田式、９０Ｆ、５ｍ2 ）を用いて透明な液とした。
【００２５】
この濾液（固形分濃度６％、タンニン力価１４０、酸度１．５、ｐＨ４．１）３１０ｌをポリスルホン膜の中空糸モジュール（（株）クラレ製；分画分子量；１３０００、１１４φ×１１００Ｌ×５本、総膜面積２５ｍ2 ）の限外濾過装置を用いて０．８〜１．２Ｋｇ／ｃｍ2 のゲージ圧で４５〜５５℃に保温しながら循環させた。加水、濃縮を繰り返し、３時間後に透過希薄液３４４０ｌ、濃縮柿渋液２００ｌが得られた。この時の透過速度は４５．９ｌ／ｍ2 ・ｈｒであった。この濃縮柿渋製品（タンニン力価２００）と加水調整した柿渋製品（タンニン力価１４０）を従来方法による柿渋製品（上記の透明な液）と比較したデータを表３に示した。タンニン回収率は９２％であった。
【００２６】
【表３】
実施例 ４
渋柿（福島県産の会津柿、平成６年収穫）１０００Ｋｇを庄田式圧搾機を用いて搾汁液６００ｌを得た。これをプレートヒーターにて９０℃に昇温後、１分間保持し、火入れの後、珪藻土６Ｋｇを添加し、撹拌によるボデイエイドを行い、濾過圧搾機（薮田式、９０Ｆ、５ｍ2 ）を用いて透明な液とした。
【００２８】
この濾液（固形分濃度７％、タンニン力価１００、酸度１．３、ｐＨ４．２）３ｌをセラミック膜モノリスモジュール（日本ガイシ（株）製；分画分子量；１００００、３０φ／４φ−１９，１０００Ｌ×１本、総膜面積０．２４ｍ2 ）の限外濾過装置を用いて０．８〜１．２Ｋｇ／ｃｍ2 のゲージ圧で５０〜６０℃に保温しながら循環させた。加水、濃縮を繰り返し、３時間後に透過希薄液３６ｌ、濃縮柿渋液１．４ｌが得られた。この時の透過速度は５０．０ｌ／ｍ2 ・ｈｒであった。この濃縮柿渋製品（タンニン力価２００）と加水調整した柿渋製品（タンニン力価１００）を従来方法による柿渋製品（上記の透明な液）と比較したデータを表４に示した。タンニン回収率は９３％であった。
【００２９】
【表４】
実施例 ５
渋柿（京都府産の天王柿、平成７年収穫）１０００Ｋｇを庄田式圧搾機を用いて搾汁液５９０ｌを得た。これをプレートヒーターにて８０℃に昇温後、１分間保持し、火入れの後、遠心分離機（斎藤遠心機工業社製：ＡＤＳ−３００１ＣＳ、５．５ｋｗ、７３００ｒｐｍ）を用いて透明な液とした。
【００３１】
この液（固形分濃度９％、タンニン力価１６０、酸度２．８、ｐＨ３．８）２９０ｌを、ポリエーテルスルホン膜の中空糸モジュール（ダイセル化学工業（株）製；分画分子量；３００００、８９φ×１１２９Ｌ×５本、総膜面積２５ｍ2 ）の限外濾過装置を用いて０．８〜１．２Ｋｇ／ｃｍ2 のゲージ圧で４０〜５０℃に保温しながら循環させた。加水、濃縮を繰り返し、３時間後に透過希薄液３１７０ｌ、濃縮柿渋液２００ｌが得られた。この時の透過速度は４２．３ｌ／ｍ2 ・ｈｒであった。この濃縮柿渋製品（タンニン力価２００）と加水調整した柿渋製品（タンニン力価１６０）を従来方法による柿渋製品（上記の透明な液）と比較したデータを表５に示した。タンニン回収率は８６％であった。
【００３２】
【表５】
実施例 ６
酒類清澄剤としての有効性について、表１に記載した柿渋製品を用いて清酒原酒・割り水・火入れ後の清酒のオリ下げ試験を行い、その比較検討を行った。
オリ下げ試験は、清酒製造技術（（財）日本醸造協会発行、ｐ３０９〜３１５、昭和６０年）に従い、従来方法、本発明方法（加水調整品）、本発明方法（濃縮品）の結果をそれぞれ表６、７、８に示した。
【００３４】
【表６】
【表７】
【表８】
実施例 ７
酒類清澄剤としての有効性について、表２に記載した柿渋製品を用いて味醂熟成もろみ・搾汁・火入れ後の味醂のオリ下げ試験を行い、その比較検討を行った。
オリ下げ試験は、清酒製造技術（（財）日本醸造協会発行、ｐ３０９〜３１５、昭和６０年）に従い、従来方法、本発明方法（加水調整品）、本発明方法（濃縮品）の結果をそれぞれ表９、１０、１１に示した。
【００３８】
【表９】
【表１０】
【表１１】
【発明の効果】
本発明の方法は柿渋の主成分である柿タンニンとその他の成分（揮発性有機酸等）の特異的な分子量差に着目して、耐熱性、耐ｐＨ性、耐薬品性に優れたポリエーテルスルホン膜又はポリスルホン膜の中空糸モジュール、更にはセラミック膜を使用した膜分離システムを用いることで、簡便に効率良く無臭の柿タンニンを分離精製することができる。
清澄剤（食品添加物）として多量に添加した場合でも、酒類（食品）の風味を損なうことがなく、また環境的、衛生的にみても、今後食品産業において幅広い利用が見込まれる。
更に、清澄剤（食品添加物）のみならず、その他の産業分野にも広く開発が進み、天然素材としての柿渋の利用価値が高まってくると考えられる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for refining persimmon astringents that has been used for clarification during the production of sake and other alcoholic beverages for a long time and has been widely used in the fields of food, cosmetics, papermaking, and textile industries. In other words, there is a characteristic odor of (1), which is unsanitary from bacteria, (2) a film is formed during storage due to the influence of impurities, and loss occurs. (3) Depending on the variety and harvest time of 柿The only way to supply stable products with different tannin concentrations and with a constant tannin concentration is by blending, which eliminates all manufacturing limitations, etc. The present invention relates to a purified persimmon fruit that can also be used to produce a conditioned product and its inexpensive and efficient manufacturing method.
[0002]
[Prior art]
The traditional production method of persimmon astringents is a method that has been reported for a long time. First, the raw astringent persimmons are squeezed to obtain the juice, which is then placed in a container and allowed to stand at room temperature for natural standing fermentation, and the sugar in the squeezed The quality was assimilated and removed by microorganisms, and then aged. During this process, volatile organic acids (acetic acid; Mw60, propionic acid; Mw74, butyric acid; Mw88) were by-produced, and these caused astringent aroma. Further, the product was sterilized by heating (fired) and usually left and aged at normal temperature for 2 to 3 years. This product is a product obtained by precipitating and removing other polymer impurities while leaving a cohesive component, and contains a large amount of low-molecular substances such as organic acids and inorganic substances. As a product, the astringent astringent concentration was 5-6 ° Baume, and the tannin titer was about 150. Moreover, a long manufacturing period was required.
[0003]
The tannin titer mentioned here is a value measured according to a colloid titration method (National Tax Agency prescribed analysis method, p337, published by Japan Brewing Association, 1981). In other words, the tannin titer was determined by adding a certain amount of methyl colloidal chitosan, which is a positive colloid, to tannin, which is a negative colloid, and reacting, and titrating the remaining amount of methyl glycol chitosan with polyvinyl potassium sulfate, which is a negative colloid. It is obtained by a quantitative method to obtain the amount of tannin by subtracting from the test value, and is displayed as a titration value of N / 400 potassium potassium sulfate per ml of persimmon astringent stock solution.
[0004]
As persimmon astringents are manufactured from natural products, their quality is strictly diverse and their properties are different. Amber astringents undergo chemical changes during aging, differing in color, fragrance, viscosity, etc. in terms of sensuality, and even when concentrated under reduced pressure, the characteristic odor cannot be completely removed. An improved method has been developed in which yeast (Saccharomyces bayanus) is sterilized instead of natural fermentation, and then fermented by adding yeast (Saccharomyces bayanus) to assimilate carbohydrates. However, foaming during fermentation is extremely problematic. In addition, since the sugar composition varies depending on the production area, harvest year and maturity of koji, there is a problem that the assimilation of sugar is not uniform and it is difficult to completely de-bromide all raw materials. In addition, since there are many low-molecular impurities as described above, a high-tannin titer could not be stably produced by the conventional concentration method.
[0005]
[Problems to be solved by the invention]
Therefore, instead of fermenting saccharides by fermentation and concentrating under reduced pressure, we examined solvent extraction, adsorption / separation by chromatogram, ion exchange, reverse osmosis, freeze concentration, etc. There were some drawbacks and it was not practical. In other words, the solvent extraction method uses a large amount of organic solvent, which is dangerous to the work, and the chromatogram method and ion exchange method have a poor recovery rate and high cost. The reverse osmosis method and freeze concentration method completely remove the astringent odor. There were drawbacks such as inability to do so.
[0006]
The present invention was devised in order to eliminate such disadvantages of the prior art, and the object thereof is to use an ultrafiltration membrane that functions to screen molecular size by membrane pore diameter, and to use low molecular weight together with water as a solvent. It is an object of the present invention to provide a purified persimmon astringent that can remove the odor peculiar to persimmon by removing the substance and can freely adjust the concentration to obtain a concentrated product and a hydrated product, and its inexpensive and efficient production method.
[0007]
[Means for Solving the Problems]
In order to achieve this object, the present inventor conducted intensive studies on a method for removing low molecular weight components of persimmon using an ultrafiltration membrane, and finally completed the present invention.
[0008]
That is, in the present invention, the raw material koji agar juice obtained by squeezing from a koji is preferably heated to 55 to 100 ° C., more preferably 70 to 90 ° C., and the liquid is allowed to permeate a substance having a molecular weight of less than 3000. Using a ultrafiltration membrane, preferably at 20 to 95 ° C., more preferably at 40 to 60 ° C., to remove low-molecular components together with water by circulating filtration. It is a manufacturing method.
[0009]
Further, the present invention is a purified strawberry astringent characterized by removing low molecular components having a molecular weight of 1000 or less, including volatile organic acids including acetic acid, propionic acid, butyric acid, glucose, carbohydrates including fructose, and inorganic substances. is there.
[0010]
DETAILED DESCRIPTION OF THE INVENTION
The raw material astringent juice used in the present invention uses, as raw material astringents, Tamura coffee from Gifu Prefecture, Tenno coffee from Kyoto Prefecture, Ehime from Ehime Prefecture, Aizu coffee from Fukushima Prefecture, etc. This is obtained by finely squeezing fruit with a pulverizer and then squeezing with a Shoda type press (screw press) to separate the solid and liquid. At this time, residual residue generated as a by-product is discarded. The juice obtained here contains a large amount of volatile organic acids, inorganic substances, carbohydrates, and the like that cause odor, along with tannin, which is the main component of persimmon.
[0011]
Next, the persimmon juice juice obtained in this way is heated and sterilized to coagulate the thermocoagulable substance, and then made into a transparent filtrate by, for example, filtration or centrifugation. The heating temperature at this time is preferably 55 to 100 ° C., and preferably 70 to 90 ° C. for 30 seconds or more. As persimmon astringent is mainly used as a clarifier for sake, it must be sterilized by heating at 55 ° C or higher in order to prevent the contamination of fire rot, which is a rot of sake. In order to sterilize efficiently, it is preferable to hold at 70 ° C. or higher for 1 to 2 minutes as instant sterilization.
[0012]
In the filtration method, it is preferable to add diatomaceous earth, which is used as a filter aid, to the squeezed juice at a ratio of 0.2 to 5% of the weight of the persimmon juice, or to use a pre-coated filter.
In the centrifugal separation method, the persimmon juice juice is fed into a bucket that rotates at high speed, and solid-liquid separation is continuously performed by centrifugal force generated by rotation. This method is used when diatomaceous earth filtration is difficult.
[0013]
Next, the low-molecular component is removed by circulating filtration of the transparent filtrate thus obtained using an ultrafiltration membrane. Examples of ultrafiltration membranes include synthetic polymer porous membranes such as cellulose acetate, polyvinylidene fluoride, polyacrylonitrile, polycarbonate, and polyolefin, and polyethersulfone membranes that have heat resistance, pH resistance and chemical resistance and can be heat-sterilized. Examples include polysulfone membranes, organic solvent-resistant polyimide membranes, and ceramic membranes.
[0014]
As filtration processes in ultrafiltration, there are pressure filtration methods, vacuum filtration methods, etc., and filtration types include single-pass, multi-stage single-pass, and circulation methods. A circulation filtration method is preferable. The liquid temperature at this time is kept at 20 to 95 ° C, preferably 30 to 80 ° C, more preferably 40 to 60 ° C. When the circulation filtration is performed in such a temperature range, the filtration efficiency is good, contamination with germs can be prevented, and damage to the membrane itself can be reduced.
[0015]
As a result of studying the properties of the raw material koji and the ultrafiltration operation conditions, the present inventor has found that (1) the molecular weight of tannin is about 4500 or more, (2) heat resistant, and (3) Resistant even at low pH (pH of the persimmon astringent is 3-4), (4) Less adhesion of tannin molecules to the film surface, (5) Alkaline cleaning at high temperature (alkaline cleaning is most effective for adhesion of persimmon ), Etc., and so on. As a purification method for persimmons that satisfy these conditions, a filtration device using an ultrafiltration membrane of a hollow fiber module made of a polyethersulfone membrane, a polysulfone membrane or a ceramic membrane with a molecular weight cut-off of 3000 or more was used. We have found that circulation filtration by pressure filtration is most preferred.
[0016]
By refining persimmon astringent using an ultrafiltration membrane as described above, a large amount of volatile organic acids, inorganic substances, carbohydrates, and other low molecular weight molecules with a fractional molecular weight or less that are dissolved in persimmon The substance efficiently permeates the membrane, while the persimmon tannin is blocked by the membrane, and by appropriately concentrating, an odorless persimmon astringent product having a tannin concentration (colloid titer) of 200 or more can be obtained. Moreover, the obtained persimmon astringent product can be obtained by adding water or concentrating it to obtain a desired product within a tannin concentration (colloid titer) of 130 or more product specification values.
[0017]
【Example】
The present invention will be specifically described by the following examples, but the present invention is not limited thereto.
In addition, the tannin titer in the examples is measured according to the National Tax Agency's prescribed analysis method, p337 (published by Japan Brewing Association, 1981), and the organic acid is measured by high performance liquid chromatography (Shim-pack SCR-102H Shimadzu Corporation). Analysis). The odor is measured by a sensory test by 10 panelists. When all 10 persons clearly feel odor, it is displayed as “astringent odor”. When all 10 persons clearly do not feel odor, Is displayed. Furthermore, the tannin recovery rate is calculated as (tannin titer x strawberry astringency) before and after ultrafiltration, and 100 × [(after ultrafiltration) / (before ultrafiltration)] is calculated from these values. And asked.
[0018]
Example 1
Using a Shoda type press, 600 liters of juice was obtained using 1000 kg of shibu-an (Tamura coffee from Gifu prefecture, harvested in 1993). This was heated to 80 ° C. with a plate heater and held for 1 minute. After burning, 6 kg of diatomaceous earth was added, body aid was carried out by stirring, and transparent using a filter press (Iwata type, 90F, 5 m 2 ). It was a liquid.
[0019]
300 l of this filtrate (solid content concentration 5%, tannin titer 130, acidity 2.1, pH 3.7) was a polyethersulfone membrane hollow fiber module (manufactured by Daicel Chemical Industries, Ltd .; fractional molecular weight; 10000, 89φ × The sample was circulated while maintaining a temperature of 50 to 60 ° C. with a gauge pressure of 0.8 to 1.2 Kg / cm 2 using an ultrafiltration device having 1129 L × 5 and a total membrane area of 25 m 2 . Water and concentration were repeated, and after 3 hours, a permeated dilute solution 3980 l and a concentrated persimmon juice solution 140 l were obtained. The transmission speed at this time was 53.1 l / m 2 · hr. Table 1 shows data obtained by comparing the concentrated persimmon astringent product (tannin titer 260) and the water-adjusted persimmon astringent product (tannin titer 130) with the conventional persimmon astringent product (the above transparent liquid). The tannin recovery rate was 93%.
[0020]
[Table 1]
Example 2
Using a Shoda-type press, 640 l of juicing liquid was obtained using 1000 kg of shibu-an (Tenno-don from Kyoto Prefecture, harvested in 1991). This was heated to 90 ° C. with a plate heater and held for 1 minute. After igniting, 7 kg of diatomaceous earth was added, body aid was carried out by stirring, and transparent using a filter press (Akita type, 90 F, 5 m 2 ). It was a liquid.
[0022]
This filtrate (solid content concentration 8%, tannin titer 160, acidity 1.8, pH 3.9) 320 l was a polysulfone membrane hollow fiber module (manufactured by Kuraray Co., Ltd .; molecular weight cut off; 13000, 114φ × 1100 L × 5) And circulated while keeping the temperature at 45 to 55 ° C. at a gauge pressure of 0.8 to 1.2 Kg / cm 2 using an ultrafiltration device having a total membrane area of 25 m 2 ). Water and concentration were repeated, and after 3 hours, 3370 liters of permeated dilute solution and 150 liters of concentrated persimmon juice liquid were obtained. The transmission speed at this time was 44.9 l / m 2 · hr. Table 2 shows data comparing the concentrated persimmon astringent product (tannin titer 320) and the water-adjusted persimmon astringent product (tannin titer 160) with the conventional persimmon astringent product (the above transparent liquid). The tannin recovery rate was 94%.
[0023]
[Table 2]
Example 3
Using a Shoda type squeezing machine, 620 l of juicing liquid was obtained using 1000 kg of astringent (Ehime from Ehime Prefecture, harvested in 1992). This was heated to 70 ° C. with a plate heater and held for 2 minutes. After burning, 7 kg of diatomaceous earth was added, body aid was carried out by stirring, and transparent using a filter press (Akita type, 90 F, 5 m 2 ). It was a liquid.
[0025]
This filtrate (solid content concentration 6%, tannin titer 140, acidity 1.5, pH 4.1) 310 l of polysulfone membrane hollow fiber module (manufactured by Kuraray Co., Ltd .; molecular weight cut off; 13000, 114φ × 1100 L × 5) And circulated while keeping the temperature at 45 to 55 ° C. at a gauge pressure of 0.8 to 1.2 Kg / cm 2 using an ultrafiltration device having a total membrane area of 25 m 2 ). Water and concentration were repeated, and after 3 hours, a permeated dilute liquid 3440 l and a concentrated persimmon astringent liquid 200 l were obtained. The transmission speed at this time was 45.9 l / m 2 · hr. Table 3 shows data comparing the concentrated persimmon astringent product (tannin titer 200) and the water-adjusted persimmon astringent product (tannin titer 140) with the conventional persimmon astringent product (the above transparent liquid). The tannin recovery rate was 92%.
[0026]
[Table 3]
Example 4
Using a Shoda type press, 600 l of juice was obtained using 1000 kg of shibu-an (Aizu coffee produced in Fukushima Prefecture, 1994 harvest). This was heated to 90 ° C. with a plate heater and held for 1 minute. After burning, 6 kg of diatomaceous earth was added, body aid was carried out by stirring, and transparent using a filter press (Iwata type, 90F, 5 m 2 ). It was a liquid.
[0028]
3 l of this filtrate (solid content concentration 7%, tannin titer 100, acidity 1.3, pH 4.2) was mixed with a ceramic membrane monolith module (manufactured by NGK KK; fractional molecular weight; 10,000, 30φ / 4φ-19, 1000 L) The sample was circulated while maintaining a temperature of 50 to 60 ° C. with a gauge pressure of 0.8 to 1.2 Kg / cm 2 using an ultrafiltration device having × 1 piece and a total membrane area of 0.24 m 2 ). Water and concentration were repeated, and after 3 hours, 36 liters of permeated diluted liquid and 1.4 liters of concentrated persimmon liquid were obtained. The transmission speed at this time was 50.0 l / m 2 · hr. Table 4 shows data comparing the concentrated persimmon astringent product (tannin titer 200) and the water-adjusted persimmon astringent product (tannin titer 100) with the conventional persimmon astringent product (the above transparent liquid). The tannin recovery rate was 93%.
[0029]
[Table 4]
Example 5
Using a Shoda type press, 590 l of juicing liquid was obtained using 1000 kg of shibu-mushroom (Tenno-don from Kyoto Prefecture, harvested in 1995). This was heated to 80 ° C. with a plate heater, held for 1 minute, and after burning, a transparent liquid was obtained using a centrifuge (manufactured by Saito Centrifugal Co., Ltd .: ADS-3001CS, 5.5 kw, 7300 rpm). did.
[0031]
290 l of this liquid (solid content concentration 9%, tannin titer 160, acidity 2.8, pH 3.8) is a polyethersulfone membrane hollow fiber module (manufactured by Daicel Chemical Industries, Ltd .; fractional molecular weight: 30000, 89φ) The sample was circulated while keeping the temperature at 40 to 50 ° C. with a gauge pressure of 0.8 to 1.2 Kg / cm 2 using an ultrafiltration device of × 1129 L × 5 and a total membrane area of 25 m 2 . Water and concentration were repeated, and after 3 hours, 3170 l of a permeated dilute solution and 200 l of a concentrated persimmon juice solution were obtained. The transmission speed at this time was 42.3 l / m 2 · hr. Table 5 shows data obtained by comparing the concentrated persimmon astringent product (tannin titer 200) and the water-adjusted persimmon astringent product (tannin titer 160) with the conventional persimmon astringent product (the above transparent liquid). The tannin recovery rate was 86%.
[0032]
[Table 5]
Example 6
About the effectiveness as a liquor clarifier, the orientation reduction test of Sake Sake, split water, and sake after burning was conducted using the persimmon astringent products listed in Table 1, and the comparison was made.
In accordance with the sake brewing technology (published by the Japan Brewing Association, p309-315, 1985), the orientation reduction test shows the results of the conventional method, the method of the present invention (hydrolyzed product), and the method of the present invention (concentrated product), respectively. The results are shown in Tables 6, 7, and 8.
[0034]
[Table 6]
[Table 7]
[Table 8]
Example 7
About the effectiveness as a liquor clarifier, the orientation reduction test of miso ripening mash, squeezed, and miso after burning was conducted using the persimmon astringent products listed in Table 2, and the comparison was examined.
In accordance with the sake brewing technology (published by the Japan Brewing Association, p309-315, 1985), the orientation reduction test shows the results of the conventional method, the method of the present invention (hydrolyzed product), and the method of the present invention (concentrated product), respectively. The results are shown in Tables 9, 10, and 11.
[0038]
[Table 9]
[Table 10]
[Table 11]
【The invention's effect】
The method of the present invention is a polyether excellent in heat resistance, pH resistance and chemical resistance, paying attention to a specific molecular weight difference between tannin, which is a main component of persimmon, and other components (such as volatile organic acids). By using a membrane separation system using a sulfone membrane or polysulfone membrane hollow fiber module and further a ceramic membrane, it is possible to easily and efficiently separate and purify odorless tannins.
Even if it is added in a large amount as a clarifier (food additive), it does not impair the flavor of alcoholic beverages (food), and it is expected to be widely used in the food industry in the future from the viewpoint of environment and hygiene.
Furthermore, it is considered that the development value of not only clarifiers (food additives) but also other industrial fields has been widely developed, and the utility value of persimmon astringent as a natural material will increase.
Claims (6)
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| JP19157596A JP3644467B2 (en) | 1996-07-01 | 1996-07-01 | Manufacturing method for purified persimmon |
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| US11221179B2 (en) | 2018-10-26 | 2022-01-11 | E. & J. Gallo Winery | Low profile design air tunnel system and method for providing uniform air flow in a refractance window dryer |
| JP7412154B2 (en) * | 2019-12-09 | 2024-01-12 | 株式会社ダイセル | Method for producing polyphenols |
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