JPS6236178A - Extraction and separation of organic component from grape cluster brewing residue - Google Patents
Extraction and separation of organic component from grape cluster brewing residueInfo
- Publication number
- JPS6236178A JPS6236178A JP60172492A JP17249285A JPS6236178A JP S6236178 A JPS6236178 A JP S6236178A JP 60172492 A JP60172492 A JP 60172492A JP 17249285 A JP17249285 A JP 17249285A JP S6236178 A JPS6236178 A JP S6236178A
- Authority
- JP
- Japan
- Prior art keywords
- carbon dioxide
- extraction
- container
- residue
- organic components
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は葡萄酒醸造工程において、生葡萄果房を搾汁し
たときて生成する搾り粕または生葡萄果房を醗酵させた
のち圧搾したときに生成する粕を産業面において有効利
用を図ることを目的として開発したものであって、いわ
ゆる産業廃棄物として取り扱っている葡萄果房醸造残渣
物から有機質成分を効果的に抽出・分離する方法に関す
る。なお、詳しく述べれば、葡萄果房醸造残渣物に含ま
れている油脂分、エステル類、アルコール類、有機酸、
グリセライド類、ビタミン類、糖分及び芳香物質等の有
機質成分を混合物として抽出分離する方法である。[Detailed Description of the Invention] Industrial Field of Application The present invention relates to the pomace lees produced when fresh grape bunches are squeezed in the wine brewing process, or the pomace produced when fresh grape bunches are fermented and then pressed. This invention was developed with the aim of making effective use of lees in industry, and relates to a method for effectively extracting and separating organic components from grape bunch brewing residue, which is treated as so-called industrial waste. In addition, in detail, the oils and fats, esters, alcohols, organic acids,
This method extracts and separates organic components such as glycerides, vitamins, sugars, and aromatic substances as a mixture.
従来の技術
従来、葡萄の醸造工程において生成する葡萄果房醸造残
渣物を、例えば、アセトン、アルコール類などの有機溶
媒抽出法とイオン交換法等の組み合わせにより、前記残
渣物中に含まれるアントシアニン系色素の分離に一部利
用されているが、その残渣物中に含まれている有機質成
分の有効利用法については、いまだ提案されていないの
が実情である。BACKGROUND ART Conventionally, grape bunch brewing residue produced in the grape brewing process is extracted by extracting the anthocyanin-based residue contained in the residue by a combination of an organic solvent extraction method such as acetone or alcohol and an ion exchange method. Although it is partially used to separate pigments, the reality is that no method has yet been proposed for effectively utilizing the organic components contained in the residue.
発明が解決しようとする問題点
ところで、生葡萄の醸造工程で生成する上記醸造残渣物
には、熱劣化しやすい物質や酸化されやすい物質が含ま
れているため、通常用いられている乾燥方法では実施上
採用されない問題がある。また既述せるアセトン、アル
コール類などの溶媒単体での抽出方法ではアントシアニ
ン色素を含んだ油脂分、エステル類等の有機質混合成分
として抽出され、前記色素が実用上に制約を生じて問題
となる。Problems to be Solved by the Invention By the way, the above-mentioned brewing residue produced during the fermentation process of fresh grapes contains substances that are easily degraded by heat and substances that are easily oxidized, so it cannot be solved by the normally used drying method. There are problems in implementation that prevent it from being adopted. In addition, in the extraction method using a single solvent such as acetone or alcohols as described above, the organic mixed components such as fats and oils and esters containing anthocyanin pigments are extracted, and the pigments pose a problem in practical use.
本発明の技術的課題は次の項目を満足させることにある
。The technical problem of the present invention is to satisfy the following items.
■ 上記醸造残渣物を熱劣化させずに、かつ空気と接触
させずに乾燥させる前処理工程を経たこと。■ The above-mentioned brewing residue was subjected to a pretreatment process in which it was dried without thermal deterioration and without contact with air.
■ 二酸化炭素と既述せる有機溶媒の混合溶媒を超臨界
混合ガス状態にしたことによって、上記乾燥葡萄果房醸
造残渣物からアントシアニン系色素以外の有機質成分を
選択的かつ短時間に好収量で抽出させること。■ Organic components other than anthocyanin pigments can be selectively extracted in a short time and in good yields from the dried grape bunch brewing residue by making the mixed solvent of carbon dioxide and the organic solvent mentioned above into a supercritical mixed gas state. to let
■ 熱劣化しやすい物質や酸化されやすい物質を自然体
のままで抽出すると共に、揮発性成分の香気成分から油
脂類、トリグリセライド等の高沸点成分までの広い範囲
の成分を抽出分離することができること。■ It is possible to extract substances that are easily degraded by heat and substances that are easily oxidized in their natural state, and also to extract and separate a wide range of components from volatile aroma components to high boiling point components such as fats and oils and triglycerides.
このように、本発明は上記項目を満足させる葡萄果房醸
造残渣物から有機質成分を抽出・分離する方法を提供す
ることにある。Thus, the present invention provides a method for extracting and separating organic components from grape bunch brewing residue that satisfies the above items.
問題を解決するだめの手段
本発明者等は、葡萄酒の醸造工程で生成する葡萄果房醸
造残渣物が殆んど産業廃棄物として処分されている現状
に着目し、上記残渣物に含有するアントシアニン系色素
以外の有機質成分を自然体のまま抽出分離する方法につ
いて鋭意研究を行なった結果、次に述べる事実を見出し
た。Means to Solve the Problem The present inventors focused on the current situation in which most of the grape bunch brewing residue produced in the wine brewing process is disposed of as industrial waste, and determined that the anthocyanins contained in the residue are As a result of intensive research into methods for extracting and separating organic components other than pigments in their natural form, we discovered the following facts.
第１Ｋ、上記含水残渣物の乾燥前処理工程では、残渣物
を凍結もしくは真空条件にしたときに残渣物中の水分が
蒸発するときの蒸発潜熱により凍結したあと真空状態で
４０〜６０ Ｇの穏和な加熱併用を施すことによって残
渣物の氷（固体）が水（液体）の状態を経ずに水蒸気（
気体）になる現象（氷の昇華）を用い、水分を除去する
乾燥法（真空凍結乾燥法）により乾燥させること、ある
いは二酸化炭素ガス、窒素ガス等の不活性ガスの存在下
で残渣物を４０〜６０Ｃに加温しながら真空加熱乾燥さ
せることにより乾燥残渣物中の熱劣化しやすい物質およ
び酸化されやすい物質は自然体のままで存在しているこ
とが確認された。この乾燥前処理を行うことは、残渣物
に含有する有機質成分を抽出しやすくする作用をもたせ
ることでもある。1st K, in the pre-drying step of the above-mentioned water-containing residue, the residue is frozen or subjected to a vacuum condition, and the residue is frozen by the latent heat of evaporation when the water in the residue evaporates, and then the residue is heated to a moderate temperature of 40 to 60 G in a vacuum condition. By applying a combination of heating and heating, the ice (solid) residue changes to water vapor (
The residue can be dried by a drying method (vacuum freeze-drying method) that removes moisture using the phenomenon of turning into a gas (sublimation of ice), or by drying the residue in the presence of an inert gas such as carbon dioxide gas or nitrogen gas. By vacuum heating and drying while heating to ~60C, it was confirmed that the substances easily deteriorated by heat and the substances easily oxidized in the dried residue were present in their natural state. Performing this pre-drying treatment also has the effect of making it easier to extract organic components contained in the residue.
第２に、抽出工程で液化二酸化炭素に抽出促進助剤であ
るエチルアルコール、エチルエーテル、ｎ−ブタン等の
低沸点溶媒又はこれらの混合溶媒を添加したのち、加温
してその超臨界混合ガスとしたものを用いて前記乾燥葡
萄果房醸造残渣物からアントシアニン系色素以外の有機
質成分を選択的に好収率で抽出できることを基本原理と
して見出し、さらに抽出物を含んだ超臨界混合ガスは二
酸化炭素の臨界点近傍から三重点近傍までのガス状態領
域条件下に減圧して、抽出物の含んだ抽出促進助剤を分
離させることにより揮発性の香気成分から高沸点有機質
成分までの広範囲成分を効率良く分離することを知見し
、この発明を完成させるに至った。Second, in the extraction process, a low boiling point solvent such as ethyl alcohol, ethyl ether, n-butane, or a mixed solvent thereof, which is an extraction accelerator, is added to the liquefied carbon dioxide, and then heated to form a supercritical mixed gas. The basic principle was that organic components other than anthocyanin pigments could be selectively extracted in good yield from the dried grape bunch brewing residue using a A wide range of components from volatile aroma components to high-boiling organic components can be extracted by separating the extraction accelerators contained in the extract under reduced pressure under conditions in the gas state region from near the critical point to near the triple point of carbon. They found that efficient separation was possible and completed this invention.
すなわち、本発明の第一の発明は、葡萄果房醸造残渣物
を真空凍結乾燥処理もしくは不活性ガス雰囲気下で乾燥
処理してから抽出用高圧容器に入れ、次いで、抽出促進
助剤である低沸点溶媒と、該容器を加温しながら超臨界
点以上の二酸化炭素を添加して、超臨界二酸化炭素混合
ガス状態を保持し、抽出促進助剤を含んだ超臨界二酸化
炭素混合ガス相に前記残渣物中の有機質成分を選択抽出
させることを特徴とする葡萄果房醸造残渣物から有機質
成分を抽出する方法であり、第二の発明は、葡萄果房醸
造残渣物を真空凍結乾燥処理もしくは不活性ガス雰囲気
下で乾燥処理してから抽出用高圧容器に入れ、次いで、
抽出促進助剤である低沸点溶媒と、該容器を加温しなが
ら超臨界点以上の二酸化炭素を添加して、超臨界二酸化
炭素混合ガス状態を保持し、抽出促進助剤を含んだ超臨
界二酸化炭素混合ガス相に前記残渣物中の有機質成分を
移行させる抽出工程と、前記抽出高圧容器の一側に接続
される導管から超臨界二酸化炭素もしくは前記抽出促進
助剤を含む超臨界二酸化炭素混合ガスを圧入し、上記抽
出条件を保持しながら該容器に接続される導出管よりそ
の抽出条件で得られた有機質成分を含んだ超臨界二酸化
炭素混合ガス相を取り出し、前記導出管に設けた減圧装
置を介して二酸化炭素の臨界点近傍から三重点近傍のガ
ス状態まで減圧して密閉分離容器内に連続移送して該容
器内で二酸化炭素ガスと有機質成分を含む抽出促進助剤
を分離し、二酸化炭素ガスは該容器から放出して有機質
成分を含んだ抽出促進助剤を分離する工程とからなるこ
とを特徴とする葡萄果房醸造残渣物から有機質成分を抽
出分離する方法である。That is, in the first aspect of the present invention, grape bunch brewing residue is subjected to vacuum freeze-drying treatment or drying treatment under an inert gas atmosphere, and then placed in a high-pressure container for extraction. A boiling point solvent and carbon dioxide above the supercritical point are added while heating the container to maintain a supercritical carbon dioxide mixed gas state, and the above is added to the supercritical carbon dioxide mixed gas phase containing the extraction promotion aid. A second invention is a method for extracting organic components from grape bunch brewing residue, which is characterized by selectively extracting organic components in the residue. After drying in an active gas atmosphere, it is placed in a high-pressure container for extraction, and then
A low boiling point solvent, which is an extraction accelerator, and carbon dioxide above the supercritical point are added while heating the container to maintain a supercritical carbon dioxide mixed gas state. an extraction step in which the organic components in the residue are transferred to a carbon dioxide mixed gas phase; and a supercritical carbon dioxide mixture containing supercritical carbon dioxide or the extraction promotion aid from a conduit connected to one side of the extraction high-pressure container. Gas is injected under pressure, and while maintaining the above extraction conditions, a supercritical carbon dioxide mixed gas phase containing organic components obtained under the extraction conditions is taken out from the outlet pipe connected to the container, and a reduced pressure is provided in the outlet pipe. Reduce the pressure of carbon dioxide from near its critical point to a gas state near its triple point through a device and continuously transfer it into a sealed separation container to separate carbon dioxide gas and an extraction promoting aid containing organic components in the container, This is a method for extracting and separating organic components from grape bunch brewing residue, which comprises a step of releasing carbon dioxide gas from the container to separate an extraction promoting aid containing organic components.
作用
以下に本発明で述べられる抽出方法と分離方法てしたが
って各方法の作用を説明する。Effects The extraction method and separation method described in the present invention and the effects of each method will be explained below.
１）抽出方法について
抽出用高圧容器内に生の葡萄果房を未醗酵処理もしくは
醗酵処理したのち、搾汁もしくは圧搾した含水葡萄果房
醸造残渣物を真空凍結乾燥もしくは不活性ガス雰囲気下
で乾燥処理してから入れ、抽出促進助剤を添加した後、
この容器を二酸化炭素（ＣＯ２）の臨界温度（３１，Ｉ
Ｃ）以上に加温しなからＣＯ２の臨界点（圧カフ５．
２８ｋｇ／ｃｒｌ、温度３１．Ｉ Ｃ）以上の超臨界Ｃ
Ｏｚガスを圧入もしくは圧入後、適当時間保持すること
によって、乾燥葡萄果房醸造残渣物からアントシアニン
系色素以外の有機質成分を超臨界ＣＯ２混合ガス相に移
行させることにある。1) Regarding the extraction method: After unfermenting or fermenting raw grape bunches in a high-pressure container for extraction, the juice or squeezed water-containing grape bunches are fermented, and the brewing residue is freeze-dried in vacuum or dried under an inert gas atmosphere. After processing and adding extraction accelerator,
This container is heated to the critical temperature of carbon dioxide (CO2) (31, I
C) Do not heat above the critical point of CO2 (pressure cuff 5.
28kg/crl, temperature 31. I C) or higher supercritical C
The purpose is to transfer organic components other than anthocyanin pigments from the dried grape bunch brewing residue to the supercritical CO2 mixed gas phase by injecting Oz gas or holding it for an appropriate period of time after injecting Oz gas.
上記せる有機質成分を抽出する抽出溶媒は液化二酸化炭
素と抽出促進助剤の液化混合ガスを高圧ポンプにて加圧
後、加熱して超臨界ＣＯ２混合ガスにしてから抽出用高
圧容器内に添加するか、もしくは抽出促進助剤は高圧ポ
ンプにて加圧し、一方液化二酸化炭素は高圧ポンプにて
加圧後、加熱して超臨界ＣＯ２ガスだしてから両者を配
管内で混合すること忙よって超臨界ＣＯ２混合ガスとし
て抽出用容器に添加するかのいずれかを使用する。The extraction solvent for extracting the organic components mentioned above is a liquefied mixed gas of liquefied carbon dioxide and an extraction promotion aid, which is pressurized using a high-pressure pump, heated to form a supercritical CO2 mixed gas, and then added into the high-pressure container for extraction. Alternatively, the extraction accelerator is pressurized with a high-pressure pump, while the liquefied carbon dioxide is pressurized with a high-pressure pump, heated to produce supercritical CO2 gas, and then mixed in a pipe. Either CO2 is added to the extraction vessel as a mixed gas or used.
■）分離方法について
抽出用高圧容器の一側の導入管から超臨界二酸化炭素も
しくは上記抽出促進助剤を含む超臨界二酸化炭素混合ガ
スを圧入し、上記抽出方法の工程の抽出条件を保持しな
がら該容器の導出管よりその抽出条件で得られた有機質
成分を含んだ超臨界二酸化炭素混合ガス相を取り出し、
この導出管の途中に設けた減圧装置を介して二酸化炭素
の臨界点近傍から三重点近傍のガス状態まで減圧して密
閉分離容器内忙連続移送して該容器内で二酸化炭素ガス
と有機質成分を含んだ抽出促進助剤を分離し、二酸化炭
素ガスは該容器から放出してアントシアニン系色素以外
の有機質成分を含んだ抽出促進助剤を分離させる方法で
ある。■) Regarding the separation method, supercritical carbon dioxide or a supercritical carbon dioxide mixed gas containing the above-mentioned extraction promoting agent is injected from the introduction pipe on one side of the high-pressure extraction container, while maintaining the extraction conditions of the above-mentioned extraction method steps. Take out the supercritical carbon dioxide mixed gas phase containing organic components obtained under the extraction conditions from the outlet pipe of the container,
Through a pressure reducing device installed in the middle of this outlet pipe, the pressure of carbon dioxide is reduced from near the critical point to the gas state near the triple point, and the gas is continuously transferred into a sealed separation container to remove carbon dioxide gas and organic components. In this method, the contained extraction promoting aid is separated, and carbon dioxide gas is released from the container to separate the extraction promoting aid containing organic components other than the anthocyanin pigment.
ところで、本発明においては、既述せるように含水葡萄
果房醸造残渣物には熱劣化しやすく且つ酸化されやすい
有機質成分が含まれているため、真空凍結乾燥もしくは
不活性ガス雰囲気下の穏和な温度条件下で真空もしくは
減圧乾燥させて自然体の有機質成分として固定させてか
ら、二酸化炭素と抽出促進助剤との超臨界混合ガスを抽
出溶媒とすることによってアントシアニン系色素以外の
有機質成分を自然体のままで抽出分離することができる
。その理由については現段階においては明らかでない。By the way, in the present invention, as mentioned above, the hydrous grape bunch brewing residue contains organic components that are easily degraded by heat and easily oxidized, so it is not necessary to freeze-dry it by vacuum freeze-drying or mildly under an inert gas atmosphere. After drying in vacuum or under reduced pressure under temperature conditions to fix them as natural organic components, organic components other than anthocyanin pigments are fixed as natural organic components by using a supercritical gas mixture of carbon dioxide and an extraction accelerator as an extraction solvent. It can be extracted and separated as it is. The reason for this is not clear at this stage.
また、上記有機質成分と抽出促進助剤を含んだ混合二酸
化炭素から分離する必要がある。この場合には、本発明
の抽出工程に既述せる分離工程が併用される。この分離
工程でＯＣ〜三重点近傍までの低温度条件で行うことに
より、有機質成分と抽出促進助剤を含んだ混合物から二
酸化炭素ガスを放出することにより、分離成分が放出ガ
ス中にほとんど移行させずに高い分離率で抽出成分を分
離することができると共に、分離条件（温度、圧力、流
速等）を変えることによって揮発性成分から高沸点成分
までの広い範囲の成分を分離することができる。Further, it is necessary to separate the carbon dioxide from the mixed carbon dioxide containing the organic components and the extraction accelerator. In this case, the separation step described above is used in combination with the extraction step of the present invention. By performing this separation process at low temperatures from OC to near the triple point, carbon dioxide gas is released from the mixture containing organic components and extraction promoting aids, and most of the separated components are transferred into the released gas. Extract components can be separated at a high separation rate without any heat loss, and a wide range of components from volatile components to high-boiling components can be separated by changing the separation conditions (temperature, pressure, flow rate, etc.).
このように、既述せる抽出工程と分離工程との組み合わ
せからなっていることが、この発明の一つの特徴でもあ
る。Thus, one of the features of the present invention is that it consists of a combination of the extraction step and separation step described above.
また、本発明の方法によれば、後に述べる実施例が示す
ように、得られた抽出物中にアントシアニン色素が含有
しないことも重要な特長である。Further, according to the method of the present invention, as shown in the Examples described later, an important feature is that the obtained extract does not contain anthocyanin pigments.
発明の効果
本発明によれば、この発明で述べられる乾燥方法で乾燥
した葡萄果房醸造残渣物からアントシアニン系色素以外
の有機質成分を選択的に効率よく抽出することができる
。Effects of the Invention According to the present invention, organic components other than anthocyanin pigments can be selectively and efficiently extracted from the grape bunch brewing residue dried by the drying method described in the present invention.
さらに、本発明は上記せる乾燥過程を含む抽出工程と分
離工程の組み合わせによって行うため、葡萄果房醸造残
渣物に含まれている有機質成分を自然体のままで固定し
、この発明の実施例が示すような顕著な抽出・分離効果
をもたらす。また、特に有害抽出促進助剤を使用しない
ので安全であり、工業化した際に、爆発などの危険もな
く、安全操業の上からも大きなメリットがあると共に、
有機質成分は化粧品、薬品。Furthermore, since the present invention is carried out by a combination of the extraction process including the drying process described above and the separation process, the organic components contained in the grape bunch brewing residue are fixed in their natural state, and the embodiments of the present invention show that It brings about remarkable extraction and separation effects. In addition, it is safe because it does not use harmful extraction accelerators, and when it is industrialized, there is no risk of explosion, and it has great advantages in terms of safe operation.
Organic ingredients are used in cosmetics and drugs.
食品等の有用な原料を提供するものである。It provides useful raw materials for foods, etc.
なお、必要により乾燥済みの残渣物を保存する場合には
、不活性ガスを封入したガス不透過性包装などに入れ、
できれば５Ｃ以下で冷蔵することが品質保全の上から望
ましい。If necessary, if you want to store the dried residue, put it in a gas-impermeable package filled with inert gas.
If possible, it is desirable to refrigerate at 5C or lower to maintain quality.
以下にこの発明の実施例を挙げて具体的に説明するが、
この発明はこれに限定されるものではない。また、各図
面中の類似部分は同一符号をもって示しである。The present invention will be specifically explained below with reference to examples.
This invention is not limited to this. Further, similar parts in each drawing are indicated by the same reference numerals.
実施例１
第１図に示す真空凍結乾燥器（１）に真空ポンプ（ＶＰ
）の糸路が連結され、この系路上に除湿器（ｌａ）と開
閉パルプ（ｖ２）が設けられる。含水葡萄果房醸造残渣
物１ ｋｇをバスケラ） （ｌｂ）内に入れて真空凍結
乾燥器内に収納した後、蓋体（ｌｃ）をその乾燥器（１
）に施蓋して密閉し、この乾燥器（１）の側壁に設けた
不活性ガス導入管（ｌｄ）のパルプ（ｖｌ）を閉じた後
、前記パルプ（Ｖ２）を開にして真空ポンプ（ＶＰ）を
駆°動し、乾燥器（１）内の真空度を５ ｘ １Ｏ−２
Ｔｏｒｒ程度まで真空引きして前記残渣物中の水分を氷
結した。この真空状態を維持しながら、この乾燥器（１
）の底部に内装される加熱器（１ｅ）でこの器内を５０
Ｃ、２０時間加熱を行うことによって、バスケット（１
ｂ）内に収納された残渣物中の水分を４３係から５係ま
で乾燥させた後、前記真空ポンプを停止するとともにパ
ルプ（ｖ２）を閉じて、不活性ガス導入管（ｌｄ）から
パルプ（■１）を介して不活性ガス（例えば二酸化炭素
ガス）を上記乾燥器内に圧入させて、その器内を常圧と
なし、得られた乾燥残渣物は空気曝露をさけて速に併設
される抽出用高圧容器（２）内にその乾燥残渣物５００
ノを移し入れ、さらにエタノール３００ｍ１！を添加し
、ブロー弁（ＢＶ） 、圧力計（Ｐ）を備えた頂蓋（２
ａ）をその容器（２）に施した後、液化二酸化炭素を充
填した高圧ボンベ（３）に接続せる系路上に設けたポン
プ（ＰＯ）にて液化二酸化炭素を液圧縮し、さらに温水
加熱方式の気化器（３ａ）を用いて４０Ｕに加熱された
超臨界二酸化炭素ガスをパルプ（■３）を経て、この容
器（２）の外周部に設けたジャケラ） （２ｂ）に４５
Ｃの温水を流通して保温された状態で該容器に圧入し、
該容器（２）内の圧力が２００ ｋｙｔ７７Ｇに到達し
てからポンプ（Ｐｏ）を停止した。その条件下で３時間
放置したのち、ポンプ（Ｐｏ）を４時間駆動して該容器
（２）内に超臨界二酸化炭素ガスを圧入することにより
、その容器内の圧力が２００ｋｇ／ｍＧを超えると、容
器（２）の導出管（２Ｃ）の管路に設けた調圧弁（ＣＶ
Ｉ）から抽出物および抽出促進助剤を含んだ二酸化炭素
ガスが導管（２ｄ）を経て排出され、さらに前記弁（Ｃ
ＶＩ）Ｋ接続される導管（２ｅ）を経て分離容器（４）
の外周部に設けたジャケット（４ｂ）に１０Ｃの水を流
通しながらその容器（４）へ移し入れられ、該容器内で
抽出物を含んだ抽出促進助剤と二酸化炭素ガスが分離さ
れ、二酸化炭素ガスの圧力が３０ｋｐ／ＣＩｆｌＧを超
えると容器（４）に設けた導出管（４Ｃ）の管路に備え
た調圧弁（ＣＶ２）の導管（４ｄ）から二酸化炭素ガス
を排出するとともに、前記弁（ＣＶ２ ）に接続する導
出管（４ｃ）を経て系外に排出される。Example 1 A vacuum pump (VP) was installed in the vacuum freeze dryer (1) shown in Figure 1.
) are connected, and a dehumidifier (la) and an open/close pulp (v2) are installed on this system. After putting 1 kg of hydrous grape bunch brewing residue into a Vasquera (lb) and storing it in a vacuum freeze dryer, the lid (lc) was placed in the dryer (lb).
), and after closing the pulp (vl) of the inert gas introduction pipe (ld) provided on the side wall of this dryer (1), open the pulp (V2) and turn on the vacuum pump ( VP) to reduce the degree of vacuum in the dryer (1) to 5 x 1O-2.
A vacuum was drawn to about Torr to freeze the moisture in the residue. While maintaining this vacuum state, this dryer (1
) The heater (1e) installed at the bottom of the container
C. By heating for 20 hours, the basket (1
b) After drying the moisture in the residue stored in the chamber from the 43rd section to the 5th section, the vacuum pump is stopped and the pulp (v2) is closed, and the pulp ( (1) Inject an inert gas (e.g. carbon dioxide gas) into the dryer under pressure to bring the inside of the dryer to normal pressure. 500 ml of the dried residue in the high-pressure extraction container (2)
Transfer the water and add 300ml of ethanol! The top cover (2) is equipped with a blow valve (BV) and a pressure gauge (P).
After a) is applied to the container (2), the liquefied carbon dioxide is compressed into a liquid by a pump (PO) installed on the system connected to the high-pressure cylinder (3) filled with liquefied carbon dioxide, and then heated using a hot water heating method. The supercritical carbon dioxide gas heated to 40U using the vaporizer (3a) is passed through the pulp (■3), and then transferred to the jacket (2b) provided on the outer periphery of this container (2).
C hot water is circulated and press-fitted into the container while being kept warm;
After the pressure inside the container (2) reached 200 kyt77G, the pump (Po) was stopped. After leaving it for 3 hours under these conditions, the pump (Po) is driven for 4 hours to inject supercritical carbon dioxide gas into the container (2), and when the pressure inside the container exceeds 200 kg/mG. , a pressure regulating valve (CV) installed in the outlet pipe (2C) of the container (2).
The carbon dioxide gas containing the extract and the extraction promoter is discharged from I) via the conduit (2d) and is further discharged from said valve (C).
VI) Separation vessel (4) via K-connected conduit (2e)
10C water is passed through a jacket (4b) provided on the outer periphery of the container and transferred to the container (4), and in the container, the extraction accelerator containing the extract and carbon dioxide gas are separated, and the carbon dioxide gas is When the pressure of carbon gas exceeds 30 kp/CIflG, carbon dioxide gas is discharged from the conduit (4d) of the pressure regulating valve (CV2) provided in the outlet pipe (4C) provided in the container (4), and the valve (CV2) is discharged outside the system through the outlet pipe (4c).
使用された二酸化炭素量は、秤１）（Ａ）で計量した結
果、２７ｋｐであった。The amount of carbon dioxide used was measured using scale 1) (A) and was 27 kp.
分離された抽出物を含んだエタノールは分離容器（４）
の底部に設けた流出管（４ａ）のパルプ（Ｖ４）を通し
て抜き出した。得られたエタノール溶液は２７０ ｍｌ
で常法の蒸留法を用いてエタノールを除去した後の残分
け３４ｇであった。その残分を分析した結果、脂肪酸エ
ステル、高級アルコール、トリグリセライド、油脂類、
ビタミン類及び芳香物質等の混合有機物で、その中には
アントシアニン系色素が認められなかった。Ethanol containing the separated extract is stored in a separation container (4)
The pulp was extracted through the pulp (V4) of the outflow pipe (4a) provided at the bottom of the. The resulting ethanol solution is 270 ml
After removing ethanol using a conventional distillation method, the remaining amount was 34 g. Analysis of the residue revealed fatty acid esters, higher alcohols, triglycerides, oils and fats,
It is a mixed organic substance such as vitamins and aromatic substances, and no anthocyanin pigments were observed in it.
なお、抽出促進助剤であるエタノールをエチルエーテル
及びｎ−ブタンの各々に替える他は実施例１に準じる抽
出分離をした結果、同様の混合有機物を得た。The same mixed organic matter was obtained as a result of extraction and separation in accordance with Example 1, except that ethanol, which was an extraction accelerator, was replaced with ethyl ether and n-butane, respectively.
実施例２
第１図に示す真空凍結乾燥器（１）内に含水葡萄醸造残
渣物１．Ｏｋ、ｐを入れ、この乾燥器（１）に蓋体（ｌ
ｃ）を施して、不活性ガス導入管（１ｄ）のパルプ（Ｖ
ｌ）から窒素ガスを供給しながらパルプ（Ｖ２）を開き
、除湿器（１ａ）を介して真空ポンプ（ＶＰ）にてこの
乾燥器内を５Ｔｏｒｒ程度に真空引きしつつ該乾燥器内
に装備される加熱器（Ｉｅ）でその乾燥器内の温度を４
０Ｃに加温することの操作を３２時間行うことによって
残渣物中の水分を４３係から５係まで乾燥させた後、真
空ポンプ（ｖｐ）、加熱器（１ｅ）を止めて、容器（１
）内を常圧にした。かくして得られた乾燥残渣物を実施
例１に準じて抽出分離を行なった。得られた結果は実施
例１のものと同様であった。Example 2 Water-containing grape brewing residue 1. Ok, put the p, and put the lid (l) into this dryer (1).
c) to remove the pulp (V
The pulp (V2) is opened while supplying nitrogen gas from 1), and the inside of this dryer is evacuated to about 5 Torr with a vacuum pump (VP) via a dehumidifier (1a). The temperature inside the dryer is set to 4.
After heating the residue to 0C for 32 hours to dry the moisture content from 43 to 5, the vacuum pump (vp) and heater (1e) are stopped, and the container (1e) is heated to 0C.
) was brought to normal pressure. The thus obtained dried residue was subjected to extraction and separation according to Example 1. The results obtained were similar to those of Example 1.
なお、上記実施例１で実施した抽出溶媒のエタノールと
二酸化炭素の超臨界混合ガス供給方法以外の実施態様に
ついて、次に付言する。The following is an additional comment regarding embodiments other than the method of supplying a supercritical mixed gas of ethanol as an extraction solvent and carbon dioxide, which was carried out in Example 1 above.
エタノール０．８１ を溶存する液化二酸化炭素を充填
したボンベ（３）から第１図に示すポンプ（Ｐｏ）およ
び気化器（３ａ）により、抽出用高圧容器（２）内の圧
力を２００ｋｐ／ｄＧに昇圧、保持したのち、実施例１
に準じて抽出分離した結果、得られた抽出物（有機質成
分）は実施例１で得られたものと同等であった・
第２図は、抽出溶媒供給装置の一例を示すものにして、
液化二酸化炭素を充填した高圧ボンベ（３）からポンプ
（Ｐｏ）によ！７２００ ｋｊＩ／ｃｒＩｔＧに液圧縮
したのち、気化器（３ａ）でガス化する。一方抽出促進
助剤としてのエタノール槽（３′）からポンプ（Ｐｌ）
により２００ｋｙ／ｍＧに液圧縮して、それぞれの導管
（３ｂ）、（３’ａ）の連結部で混合して０．７４％の
超臨界混合ガス１４ｍ”をパルプ（Ｖ３） ヲ経て抽出
用高圧容器に供給し、第１図に図示の抽出容器（２）及
び分離容器（４）を用いて実施例１に準じて抽出・分離
した結果、得られた抽出物は実施例１で得られたものと
同等であった。The pressure inside the high-pressure extraction container (2) is raised to 200 kp/dG from a cylinder (3) filled with liquefied carbon dioxide in which 0.81% of ethanol is dissolved, using the pump (Po) and vaporizer (3a) shown in Figure 1. After increasing and holding the pressure, Example 1
As a result of extraction and separation in accordance with
By pump (Po) from high pressure cylinder (3) filled with liquefied carbon dioxide! After compressing the liquid to 7200 kjI/crItG, it is gasified in a vaporizer (3a). On the other hand, the pump (Pl) is pumped from the ethanol tank (3') as an extraction accelerator.
The liquid is compressed to 200 ky/mG and mixed at the connecting part of each conduit (3b) and (3'a) to produce 14 m of 0.74% supercritical mixed gas to pulp (V3) and then to high pressure for extraction. As a result of extraction and separation according to Example 1 using the extraction container (2) and separation container (4) shown in FIG. 1, the obtained extract was the same as that obtained in Example 1. It was equivalent to that.
なお、同図中の符号（Ａ）、（Ｂ）は秤りを示すIn addition, the symbols (A) and (B) in the same figure indicate scales.
第１図は本発明を実施する装置の一例を示す説明図、第
２図は抽出溶媒供給装置の一実施態様を示す説明図であ
る。
図中の１は乾燥器、２は抽出用高圧容器、３は高圧ボン
ベ、４は分離容器である。
第 ２ 図FIG. 1 is an explanatory diagram showing an example of an apparatus for carrying out the present invention, and FIG. 2 is an explanatory diagram showing an embodiment of an extraction solvent supply apparatus. In the figure, 1 is a dryer, 2 is a high-pressure container for extraction, 3 is a high-pressure cylinder, and 4 is a separation container. Figure 2
Claims (2)
不活性ガス雰囲気下で乾燥処理してから抽出用高圧容器
に入れ、次いで、抽出促進助剤である低沸点溶媒と、該
容器を加温しながら超臨界点以上の二酸化炭素を添加し
て、超臨界二酸化炭素混合ガス状態を保持し、抽出促進
助剤を含んだ超臨界二酸化炭素混合ガス相に前記残渣物
中の有機質成分を選択抽出させることを特徴とする葡萄
果房醸造残渣物から有機質成分を抽出する方法。(1) Grape bunch brewing residue is subjected to vacuum freeze-drying treatment or drying treatment under an inert gas atmosphere, and then placed in a high-pressure container for extraction, and then a low boiling point solvent, which is an extraction accelerator, is added to the container. Add carbon dioxide above the supercritical point while heating to maintain a supercritical carbon dioxide mixed gas state, and select organic components in the residue into the supercritical carbon dioxide mixed gas phase containing an extraction promotion aid. A method for extracting organic components from grape bunch brewing residue.
不活性ガス雰囲気下で乾燥処理してから抽出用高圧容器
に入れ、次いで、抽出促進助剤である低沸点溶媒と、該
容器を加温しながら超臨界点以上の二酸化炭素を添加し
て、超臨界二酸化炭素混合ガス状態を保持し、抽出促進
助剤を含んだ超臨界二酸化炭素混合ガス相に前記残渣物
中の有機質成分を移行させる抽出工程と、前記抽出高圧
容器の一側に接続される導管から超臨界二酸化炭素もし
くは前記抽出促進助剤を含む超臨界二酸化炭素混合ガス
を圧入し、上記抽出条件を保持しながら該容器に接続さ
れる導出管よりその抽出条件で得られた有機質成分を含
んだ超臨界二酸化炭素混合ガス相を取り出し、前記導出
管に設けた減圧装置を介して二酸化炭素の臨界点近傍か
ら三重点近傍のガス状態まで減圧して密閉分離容器内に
連続移送して該容器内で二酸化炭素ガスと有機質成分を
含む抽出促進助剤を分離し、二酸化炭素ガスは該容器か
ら放出して有機質成分を含んだ抽出促進助剤を分離する
工程とからなることを特徴とする葡萄果房醸造残渣物か
ら有機質成分を抽出・分離する方法。(2) Grape bunch brewing residue is subjected to vacuum freeze-drying treatment or drying treatment under an inert gas atmosphere, then placed in a high-pressure container for extraction, and then a low boiling point solvent, which is an extraction accelerator, is added to the container. Carbon dioxide above the supercritical point is added while heating to maintain a supercritical carbon dioxide mixed gas state, and the organic components in the residue are transferred to a supercritical carbon dioxide mixed gas phase containing an extraction promoting agent. and injecting supercritical carbon dioxide or a supercritical carbon dioxide mixed gas containing the extraction accelerator from a conduit connected to one side of the high-pressure extraction container, and while maintaining the above-mentioned extraction conditions, into the container. The supercritical carbon dioxide mixed gas phase containing organic components obtained under the extraction conditions is extracted from the connected outlet pipe, and the supercritical carbon dioxide mixed gas phase containing organic components obtained under the extraction conditions is extracted from the vicinity of the critical point of carbon dioxide to the vicinity of the triple point through a pressure reducing device installed in the outlet pipe. The pressure is reduced to a gas state and the mixture is continuously transferred into a sealed separation container to separate the carbon dioxide gas and the extraction promoting aid containing organic components in the container, and the carbon dioxide gas is released from the container to remove the organic components. A method for extracting and separating organic components from grape bunch brewing residue, the method comprising the step of separating an extraction promoting aid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60172492A JPS6236178A (en) | 1985-08-07 | 1985-08-07 | Extraction and separation of organic component from grape cluster brewing residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60172492A JPS6236178A (en) | 1985-08-07 | 1985-08-07 | Extraction and separation of organic component from grape cluster brewing residue |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6236178A true JPS6236178A (en) | 1987-02-17 |
Family
ID=15942978
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60172492A Pending JPS6236178A (en) | 1985-08-07 | 1985-08-07 | Extraction and separation of organic component from grape cluster brewing residue |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6236178A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6434254A (en) * | 1987-07-28 | 1989-02-03 | Shonan Koryo Corp | Method for processing and treating food |
| ES2103238A1 (en) * | 1996-02-22 | 1997-09-01 | Invest De La Ind Agroalimentar | Process for extracting natural products by means of supercritical fluids |
| JP2001157567A (en) * | 1999-09-24 | 2001-06-12 | Asahi Soft Drinks Co Ltd | Malic polyphenol-containing beverage |
| JP2007002119A (en) * | 2005-06-24 | 2007-01-11 | Nkk Kk | Method for producing carbon dioxide-dme mixed gas |
-
1985
- 1985-08-07 JP JP60172492A patent/JPS6236178A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6434254A (en) * | 1987-07-28 | 1989-02-03 | Shonan Koryo Corp | Method for processing and treating food |
| ES2103238A1 (en) * | 1996-02-22 | 1997-09-01 | Invest De La Ind Agroalimentar | Process for extracting natural products by means of supercritical fluids |
| JP2001157567A (en) * | 1999-09-24 | 2001-06-12 | Asahi Soft Drinks Co Ltd | Malic polyphenol-containing beverage |
| JP2007002119A (en) * | 2005-06-24 | 2007-01-11 | Nkk Kk | Method for producing carbon dioxide-dme mixed gas |
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