JP4924435B2 - Separation device - Google Patents
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- JP4924435B2 JP4924435B2 JP2008001106A JP2008001106A JP4924435B2 JP 4924435 B2 JP4924435 B2 JP 4924435B2 JP 2008001106 A JP2008001106 A JP 2008001106A JP 2008001106 A JP2008001106 A JP 2008001106A JP 4924435 B2 JP4924435 B2 JP 4924435B2
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Description
本発明は、反応中に、簡便に、凝縮された液体を溶媒と抽出物とに分離する簡易分離装置に関する。 The present invention relates to a simple separation apparatus for easily separating a condensed liquid into a solvent and an extract during the reaction.
従来より精油等の有用物質を取得するために、水や有機溶媒を用いて植物原料または動物原料から該有用物質を抽出することが行われている。近年は、精油等のバイオマス抽出物を得るため、水蒸気蒸留を応用した簡便な抽出装置も市販されている。 Conventionally, in order to obtain useful substances such as essential oils, extraction of the useful substances from plant raw materials or animal raw materials using water or organic solvents has been performed. In recent years, in order to obtain biomass extracts such as essential oils, a simple extraction device applying steam distillation is also commercially available.
精油等の抽出は、木の葉、実などの植物材料または動物材料から水や有機溶媒を用いて行うことが多いが、従来の2層もしくは複数溶媒系の抽出では、ある程度の時間、加熱還流した後、溶媒と抽出物とを分液漏斗を用いて液分離していた。そのため、水蒸気蒸留では、水蒸気あるいは水を大量に反応系に導入する必要があった。 Extraction of essential oils is often performed from plant materials such as leaves and fruits or animal materials using water or organic solvents, but in conventional two-layer or multi-solvent extraction, after heating and refluxing for a certain period of time, The solvent and the extract were separated using a separatory funnel. Therefore, in the steam distillation, it is necessary to introduce a large amount of steam or water into the reaction system.
また、目的物を抽出しきるまで加熱を行うため、反応初期に抽出されたものまで無駄に加熱されており、そのため折角抽出した目的物が熱劣化してしまうなどの問題があり、熱劣化を避けるためには抽出しきる前に加熱を停止する必要があった。 In addition, since heating is performed until the target product is completely extracted, even the one extracted at the initial stage of the reaction is heated wastefully. Therefore, it was necessary to stop the heating before the extraction was completed.
さらに、抽出物の溶媒への溶解度を増すためには、ある程度大量の溶媒を必要としていたため、加熱にエネルギーを要していた。 Furthermore, in order to increase the solubility of the extract in a solvent, a certain amount of solvent is required, and thus heating requires energy.
また、抽出操作後、溶媒と抽出物を分液漏斗へ移して分液する必要があるため、操作が煩雑な上、ロスが発生していた。あるいは、ロスをカバーするために、容器を溶媒で洗浄した洗浄液を回収する必要があった。 In addition, after the extraction operation, it is necessary to transfer the solvent and the extract to a separatory funnel to separate the liquid, so that the operation is complicated and loss occurs. Or in order to cover loss, it was necessary to collect | recover the washing | cleaning liquid which wash | cleaned the container with the solvent.
さらに、水蒸気蒸留では水蒸気もしくは水を大量に反応系に加える必要があるため、加熱にエネルギーがかかり、且つ、必要に応じて水を追添加する必要があった。 Furthermore, since steam distillation requires a large amount of steam or water to be added to the reaction system, it takes energy for heating, and it is necessary to add water as necessary.
抽出に使用する溶媒を減少させるため、オレンジ油からオレンジ油酸素付加物を水で抽出するにあたり、逆浸透膜等の膜分離プロセスを使用して連続的に水を分離、再循環させる方法が提案されている(特許文献1参照)。しかしながら、膜分離プロセスを利用して溶媒を再循環させることは有効な手段の一つではあるが、簡便な方法とは言い難い。 In order to reduce the solvent used for extraction, a method of continuously separating and recirculating water using a membrane separation process such as reverse osmosis membrane is proposed for extracting orange oil oxygen adduct from orange oil with water. (See Patent Document 1). However, recycling the solvent using a membrane separation process is an effective means, but is not a simple method.
また、油水分離装置では、油水分離タンク内の液位を保持するために逆U字型の溢流管を設け分離水を油水分離タンクに戻すことが行われているが(特許文献2,3等を参照)、油を簡易に取り出せる構造にはなっていない。
本発明は、抽出物を、熱劣化させることなく、少ない溶媒量で、省エネルギー、高効率で、簡便に取り出すことができる簡易分離装置を提供することを目的とする。 It is an object of the present invention to provide a simple separation device that can easily extract an extract with a small amount of solvent, energy saving, high efficiency, and without causing thermal degradation.
前記課題を解決するため、本発明者らは鋭意検討した結果、下記の構成からなる簡易分離装置を、抽出容器と冷却管との間に設けることにより、上層に抽出物を速やか、かつ効率よく分離して熱劣化を防ぐと共に、下層の溶媒を戻り管を通じて抽出容器に戻すことで、溶媒量を最小、かつ追添加することなく抽出、蒸留できることを見出し、本発明に到達した。 In order to solve the above-mentioned problems, the present inventors have intensively studied. As a result, by providing a simple separation device having the following configuration between the extraction vessel and the cooling pipe, the extract can be quickly and efficiently added to the upper layer. The present inventors have found that it is possible to separate and prevent thermal degradation and return the lower layer solvent to the extraction vessel through the return pipe, thereby extracting and distilling the solvent with minimum amount and without additional addition.
すなわち、本発明は、以下の簡易分離装置を提供するものである。 That is, the present invention provides the following simple separation apparatus.
(1)凝縮された液体を溶媒と抽出物とに分離するための簡易分離装置であって、
抽出容器に連通する主管(31)と、
冷却手段に連通する受け管(32)と、
該受け管から前記主管に連通する戻り管(33)と、を備え、
前記受け管は、その下端が三方向弁(34)に連結されると共に、該三方向弁を介して前記戻り管に連通し、該戻り管は、一定の液位を保持しうる垂直高さを有し、その他端が主管に連結されており、
前記主管の上部(35)は、連結端が受け管に対して鈍角を形成するように受け管上部に連結されてなり、
前記主管はその下端に抽出容器との連結部(36a)を有し、かつ、前記受け管はその上端に冷却手段との連結部(36b)を有する簡易分離装置。
(1) A simple separation device for separating a condensed liquid into a solvent and an extract,
A main pipe (31) communicating with the extraction container;
A receiving pipe (32) communicating with the cooling means;
A return pipe (33) communicating from the receiving pipe to the main pipe,
The receiving pipe has a lower end connected to the three-way valve (34) and communicates with the return pipe via the three-way valve, and the return pipe has a vertical height that can maintain a constant liquid level. The other end is connected to the main pipe,
The upper part (35) of the main pipe is connected to the upper part of the receiving pipe so that the connecting end forms an obtuse angle with respect to the receiving pipe,
The main pipe has a connecting portion (36a) with an extraction container at its lower end, and the receiving pipe has a connecting portion (36b) with a cooling means at its upper end.
(2)固体バイオマスから溶媒抽出した精油の分離に用いる、前記(1)に記載の簡易分離装置。 (2) The simple separation apparatus according to (1), which is used for separation of essential oil extracted from solid biomass by solvent.
本発明に係る簡易分離装置を、抽出容器と冷却管との間に設けることにより、反応中に、分離装置の受け管の上層に抽出物を分離することができるので、抽出物の熱劣化を防げると共に、下層の溶媒が戻り管を通じて抽出容器に戻されるので、溶媒量を最小かつ追添加することなく抽出することができる。しかも、主管の連結端が受け管に対して鈍角に形成されているため、凝縮した液体が逆流すること無く、確実に受け管に溜められるので、回収効率が高い。反応後は、三方向弁の操作により、簡便に抽出物あるいは抽出物を含有する液層を分取することができる。省溶媒の抽出なので、省エネルギーである。 By providing the simple separation apparatus according to the present invention between the extraction container and the cooling pipe, the extract can be separated into the upper layer of the receiving pipe of the separation apparatus during the reaction, so that the thermal degradation of the extract is prevented. In addition, the lower layer solvent is returned to the extraction container through the return pipe, so that the extraction can be performed without adding a minimum amount of solvent. In addition, since the connecting end of the main pipe is formed at an obtuse angle with respect to the receiving pipe, the condensed liquid is surely stored in the receiving pipe without flowing back, so that the recovery efficiency is high. After the reaction, the extract or the liquid layer containing the extract can be easily separated by operating the three-way valve. Since it is a solvent-saving extraction, it is energy-saving.
以下、本発明に係る簡易分離装置を図面を参照しながら詳細に説明する。図3は、本発明の分離装置の概略構成を示す図(図4と5は部分拡大図)であり、図6は比較の分離装置を示す図である。 Hereinafter, a simple separation device according to the present invention will be described in detail with reference to the drawings. FIG. 3 is a diagram showing a schematic configuration of the separation device of the present invention (FIGS. 4 and 5 are partially enlarged views), and FIG. 6 is a diagram showing a comparative separation device.
[作用]
本発明の分離装置は、抽出容器から蒸発した後、冷却手段により凝縮された液体を、反応中に、溶媒と抽出物とに分離する簡易分離装置である。図3に示すように、分離装置(30)は、抽出容器に連通する主管(31)と、冷却手段に連通する受け管(32)と、該受け管から前記主管に連通する戻り管(33)と、を備えている。前記受け管は、その下端が三方向弁(34)に連結されると共に、該三方向弁(34)を介して前記戻り管に連通し、該戻り管(33)は、一定の液位を保持しうる垂直高さを有し、その他端が主管の上方部分に連結されている。主管の上部(35)は、受け管(32)の上部で受け管に連結し、主管上部の連結端の角度(α)は受け管に対して鈍角に形成されている。主管(31)は、下端に抽出容器との連結部(36a)を有し、受け管(32)は、上端に冷却手段との連結部(36b)を有しており、それぞれ、抽出容器および冷却手段に連結させて用いることができる。
[Action]
The separation device of the present invention is a simple separation device that separates the liquid condensed by the cooling means into a solvent and an extract during the reaction after evaporating from the extraction container. As shown in FIG. 3, the separation device (30) includes a main pipe (31) communicating with the extraction container, a receiving pipe (32) communicating with the cooling means, and a return pipe (33) communicating from the receiving pipe to the main pipe. ) And. The receiving pipe has a lower end connected to the three-way valve (34) and communicates with the return pipe via the three-way valve (34), and the return pipe (33) has a certain liquid level. It has a vertical height that can be held, and its other end is connected to the upper part of the main pipe. The upper part (35) of the main pipe is connected to the receiving pipe at the upper part of the receiving pipe (32), and the angle (α) of the connecting end of the upper part of the main pipe is formed at an obtuse angle with respect to the receiving pipe. The main pipe (31) has a connection part (36a) to the extraction container at the lower end, and the receiving pipe (32) has a connection part (36b) to the cooling means at the upper end. It can be used by being connected to a cooling means.
本発明の分離装置において、主管(31)は蒸気を冷却手段に導く機能と、凝縮された溶媒を抽出容器に戻す機能を有している。受け管(32)は凝縮された液体、すなわち、抽出溶媒と抽出物を溜めて分離する機能を有しており、更に該受け管に連結された三方向弁を用いれば抽出物を簡易に取り出すことが可能となる。戻り管(33)は、受け管に溜めた液体を主管を通じて抽出容器に戻す機能を有している。 In the separation apparatus of the present invention, the main pipe (31) has a function of guiding the vapor to the cooling means and a function of returning the condensed solvent to the extraction container. The receiving pipe (32) has a function of accumulating and separating the condensed liquid, that is, the extraction solvent and the extract, and if the three-way valve connected to the receiving pipe is used, the extract can be easily taken out. It becomes possible. The return pipe (33) has a function of returning the liquid accumulated in the receiving pipe to the extraction container through the main pipe.
一方、図6に示す分離装置(30´)は、主管の連結端の角度(β)が受け管に対して鋭角に形成されていること以外は、本発明の分離装置と同じである。 On the other hand, the separator (30 ′) shown in FIG. 6 is the same as the separator of the present invention except that the angle (β) of the connecting end of the main pipe is formed at an acute angle with respect to the receiving pipe.
[分離方法]
本発明の分離装置を用いて溶媒と抽出物の分離操作を行う場合、反応開始前および反応中は、三方向弁(34)を図3に示す方向に保持し、受け管と戻り管を開放する。三方向弁には手前側に図示しない三方コックが備えられている。反応開始前には、抽出容器の空焚き防止の目的で、受け管に呼び水(溶媒)を添加してもよい。反応の進行にともない、受け管(32)には凝縮された溶媒と抽出物が溜まる。溶媒には、抽出物の比重よりも、比重の大きい溶媒を選定すれば、抽出物と溶媒の比重差を利用して抽出物と溶媒を二層に分離することができる。この際、受け管は分離管の役割をする。
[Separation method]
When performing the separation operation of the solvent and the extract using the separation apparatus of the present invention, the three-way valve (34) is held in the direction shown in FIG. 3 before starting the reaction and during the reaction, and the receiving tube and the return tube are opened. To do. The three-way valve is provided with a three-way cock (not shown) on the front side. Before starting the reaction, priming water (solvent) may be added to the receiving tube for the purpose of preventing emptying of the extraction container. As the reaction proceeds, the condensed solvent and extract accumulate in the receiving tube (32). If a solvent having a specific gravity greater than the specific gravity of the extract is selected as the solvent, the extract and the solvent can be separated into two layers by utilizing the specific gravity difference between the extract and the solvent. At this time, the receiving tube serves as a separation tube.
下層に溜まった溶媒量が、戻り管(33)の最高点に到達すると、戻り管(33)に溜まっていた溶媒と受け管(32)に溜まっていた溶媒は、図3の点線で示す高さ、すなわち主管と戻り管の連結部位の高さになるまで、主管(31)を経由して抽出容器に戻される。その結果、受け管(32)には抽出物と溶媒が残る。さらに反応が進行すると、点線の水位を維持しながら下層の溶媒だけが順次抽出容器に戻されていくので、受け管(32)には抽出物が徐々に増えていく。 When the amount of the solvent accumulated in the lower layer reaches the highest point of the return pipe (33), the solvent accumulated in the return pipe (33) and the solvent accumulated in the receiving pipe (32) That is, it is returned to the extraction container via the main pipe (31) until the height of the connecting portion of the main pipe and the return pipe is reached. As a result, the extract and solvent remain in the receiving tube (32). As the reaction proceeds further, only the lower layer solvent is sequentially returned to the extraction vessel while maintaining the dotted water level, so that the extract gradually increases in the receiving tube (32).
図6に示すように、主管の連結端と受け管との成す角度(β)が鋭角であると、凝縮した溶媒の一部が主管を介して抽出容器に戻る現象(逆流)が起こるが、本発明では、図3に示すように、主管の連結端と受け管との成す角度(α)が鈍角であるので、逆流防止効果がある。そのため、短時間で効率よく抽出することができる、 As shown in FIG. 6, when the angle (β) formed between the connecting end of the main pipe and the receiving pipe is an acute angle, a phenomenon (back flow) occurs in which a part of the condensed solvent returns to the extraction container through the main pipe. In the present invention, as shown in FIG. 3, since the angle (α) formed between the connecting end of the main pipe and the receiving pipe is an obtuse angle, there is a backflow prevention effect. Therefore, it can be extracted efficiently in a short time.
反応終了後は、三方向弁(34)を図4に示す方向に保持し、戻り管(33)の出口を開放することにより、戻り管(33)に溜まっていた溶媒を捨てることができる。 After completion of the reaction, the three-way valve (34) is held in the direction shown in FIG. 4 and the outlet of the return pipe (33) is opened, so that the solvent accumulated in the return pipe (33) can be discarded.
次に、三方向弁(34)を図5に示す方向に保持し、受け管(32)を開放して、戻り管(33)を閉鎖し、受け管に溜まっていた溶媒を捨てれば、その後に、上層の抽出物のみを分離することができる。 Next, hold the three-way valve (34) in the direction shown in FIG. 5, open the receiving pipe (32), close the return pipe (33), and discard the solvent accumulated in the receiving pipe. In addition, only the upper layer extract can be separated.
したがって、本発明の分離装置を用いることにより、抽出および分離が可能で、かつ、溶媒が逆流せずに循環されるので、溶媒量を最小で、かつ追添加することなく抽出、蒸留できる。 Therefore, by using the separation apparatus of the present invention, extraction and separation are possible, and the solvent is circulated without backflow, so that extraction and distillation can be performed with a minimum amount of solvent and without additional addition.
なお、本発明の分離装置において、抽出溶媒に抽出物が溶解する場合は、抽出溶媒よりもさらに抽出物の溶解度が高く比重が軽く、かつ、抽出溶媒とは混和しない溶媒(例えばエーテル等)を、予め分離装置の受け管に仕込んでおくことにより、抽出物を速やかに移層させ、抽出物が溶け込んでいない状態の溶媒を抽出容器に戻すことができる。 In the separation apparatus of the present invention, when the extract is dissolved in the extraction solvent, a solvent (for example, ether) having a higher solubility and a lower specific gravity than the extraction solvent and immiscible with the extraction solvent is used. The extract can be quickly transferred to the extraction vessel by preliminarily charging the separator in the separator, and the solvent in which the extract is not dissolved can be returned to the extraction container.
[溶媒]
本発明の分離装置を用いた抽出において、抽出溶媒としては、水の他、エーテル類、メタノール、エタノールなどのアルコール類、酢酸エチル、ピリジン、テトラヒドロフラン、クロロホルム、アセトンなどの有機溶媒を、それぞれ単独でまたは組合わせて用いることができる。その中でもコスト、安全性等を考慮すると水が好ましい。
[solvent]
In the extraction using the separation apparatus of the present invention, as the extraction solvent, water, alcohols such as ethers, methanol, and ethanol, and organic solvents such as ethyl acetate, pyridine, tetrahydrofuran, chloroform, and acetone are used alone. Or they can be used in combination. Among these, water is preferable in consideration of cost, safety and the like.
[被抽出物]
本発明の分離装置を用いて有用物質の抽出、分離を行う場合、適用する被抽出物としては、植物原料または動物原料からなる固体バイオマスが好適である。植物原料としては、木や草の葉、実、枝、根など栽培系バイオマス;木材、間伐材、伐採木、剪定枝、おがくず、樹皮、チップ、端材、流木、竹、笹、木質建築廃材などの木質系バイオマス;モミ殻、稲藁、麦藁、バガス、アブラヤシ(パーム油の原料)のヤシ殻などの農作物系バイオマス;食品工場や外食産業から出る食品残渣;等を挙げることができる。
[To be extracted]
When extracting and separating useful substances using the separation apparatus of the present invention, solid biomass composed of plant raw materials or animal raw materials is suitable as an extract to be applied. Plant raw materials include tree and grass leaves, berries, branches, roots, and other cultivated biomass; Wood biomass such as fir husk, rice straw, wheat straw, bagasse, oil palm (raw material of palm oil) and other agricultural crop biomass; food residue from food factories and restaurant industry;
[抽出容器]
一つ口〜四つ口の円筒形セパラブルフラスコ等が挙げられるが、特に限定されない。
[Extraction container]
One-neck to four-neck cylindrical separable flasks and the like can be mentioned, but are not particularly limited.
[冷却手段]
リービッヒ管、ジムロート等が挙げられるが、特に限定されない。
[Cooling means]
Examples include Liebig tubes and Jim Roth, but are not particularly limited.
以上、本発明に係る簡易分離装置の実施形態について説明したが、本発明はこれら実施形態に限定されるものではなく、本発明の範囲を逸脱することなく種々の変形が可能であることは言うまでもない。 Although the embodiments of the simple separation device according to the present invention have been described above, the present invention is not limited to these embodiments, and it goes without saying that various modifications can be made without departing from the scope of the present invention. Yes.
次に、各種分離装置を用いた抽出実験例を図面を参照しながら具体的に説明する。 Next, an extraction experiment example using various separation devices will be specifically described with reference to the drawings.
<実験例1>
図1に示したマイクロ波発生装置(10)内に設置された内径200mmのセパラブル三ツ口円筒フラスコ(20)に、純水50.08gと沸石を加え、テフロン(登録商標)製の目皿(2)を設置した。目皿の穴は5mmのものを使用し、その上に、バイオマスが下にこぼれ落ちないようにメッシュサイズ0.75φのテフロン(登録商標)パンチングシートを設置した。この上に、バイオマスとしてトドマツ葉粉砕物300.06gを加えた。トドマツ葉粉砕物は分析ミル(IKA Works Guangzhou社製 型式:A11 basic)にて8mmアンダーに破砕して得た。
<Experimental example 1>
To a separable three-necked cylindrical flask (20) having an inner diameter of 200 mm installed in the microwave generator (10) shown in FIG. ) Was installed. A hole with a diameter of 5 mm was used, and a Teflon (registered trademark) punching sheet having a mesh size of 0.75φ was placed thereon so that the biomass would not spill down. On top of this, 300.06 g of Todomatsu leaf pulverized product was added as biomass. Todomatsu leaf pulverized product was obtained by crushing under 8 mm using an analysis mill (model: A11 basic, manufactured by IKA Works Guangzhou).
マイクロ波発生装置(10)外に、円筒フラスコ(20)と連結するように、図6に示す構成の分離装置(30´)の連結部(36a´)を連結管(25)を介して連結し、受け管部に呼び水として純水12.89gを加えた。分離装置の上部に連結部(36b´)を介して長さ300mmのジムロート冷却管(40)を連結した。また、ジムロート冷却管の上部に、余分な排ガスをドラフトへ送気する管を設けた。 The connecting portion (36a ') of the separation device (30') having the configuration shown in FIG. 6 is connected to the outside of the microwave generator (10) via the connecting pipe (25) so as to be connected to the cylindrical flask (20). Then, 12.89 g of pure water was added to the receiving tube as priming water. A Dimroth cooling pipe (40) having a length of 300 mm was connected to the upper part of the separator through a connecting part (36b ′). In addition, a pipe for supplying excess exhaust gas to the draft was provided at the upper part of the Dimroth cooling pipe.
周波数2.45GHz、最大出力700Wのマイクロ波を出力一定にて上記反応装置に照射し、水蒸気蒸留を行った。反応時間は初留発生後20分を基本とした。 The reactor was irradiated with microwaves having a frequency of 2.45 GHz and a maximum output of 700 W, and steam distillation was performed. The reaction time was basically 20 minutes after the first distillation occurred.
初留までの所要時間、初留から反応終了までの時間、及び精油回収量を計測した。初留までの所要時間は5分、反応終了までの時間は20分であり、終了時に円筒フラスコ内には十分な水があり、さらに蒸留を続けることが可能であった。反応後の全油分収量は3416mgであった。また、これをバイオマス100g-dryあたりの精油収量に換算すると2103mgであった。 The time required for the first distillation, the time from the first distillation to the end of the reaction, and the amount of recovered essential oil were measured. The time required for the first distillation was 5 minutes, and the time required for completion of the reaction was 20 minutes. At the end of the reaction, there was sufficient water in the cylindrical flask, and distillation could be continued. The total oil yield after the reaction was 3416 mg. Moreover, it was 2103 mg when this was converted into the essential oil yield per 100 g-dry of biomass.
反応を通して、バイオマスが過加熱になったり、焦げたりすることはなかったが、凝縮水のうち10%程度が抽出容器に戻ってしまう現象が見られた。 Throughout the reaction, the biomass was not overheated or burned, but a phenomenon was observed in which about 10% of the condensed water returned to the extraction vessel.
<実験例2>
図1に示したマイクロ波発生装置(10)内に設置された内径200mmのセパラブル三ツ口円筒フラスコ(20)に、純水50.04gと沸石を加え、テフロン(登録商標)製の目皿(2)を設置した。目皿の穴は5mmのものを使用し、その上に、バイオマスが下にこぼれ落ちないようにメッシュサイズ0.75φのテフロン(登録商標)パンチングシートを設置した。この上に、バイオマスとしてトドマツ葉粉砕物300.06gを加えた。トドマツ葉粉砕物は分析ミル(IKA Works Guangzhou社製 型式:A11 basic)にて8mmアンダーに破砕して得た。
<Experimental example 2>
50.04 g of pure water and zeolite are added to a separable three-necked cylindrical flask (20) having an inner diameter of 200 mm installed in the microwave generator (10) shown in FIG. ) Was installed. A hole with a diameter of 5 mm was used, and a Teflon (registered trademark) punching sheet having a mesh size of 0.75φ was placed thereon so that the biomass would not spill down. On top of this, 300.06 g of Todomatsu leaf pulverized product was added as biomass. Todomatsu leaf pulverized product was obtained by crushing under 8 mm using an analysis mill (model: A11 basic, manufactured by IKA Works Guangzhou).
マイクロ波発生装置(10)外に、円筒フラスコ(20)と連結するように、図6に示す構成の分離装置(30´)の連結部(36a´)を連結管(25)を介して連結し、受け管部に呼び水として純水14.22gを加えた。分離装置の上部に連結部(36b´)を介して長さ300mmのジムロート冷却管(40)を連結した。また、ジムロート冷却管の上部に、余分な排ガスをドラフトへ送気する管を設けた。さらに、分離装置の受け管(32´)を図面左方向に1.3度傾くように設置し、ジムロート冷却管からの戻り凝縮水が主管(31´)を通して抽出容器に戻り難いようにした。このようにすることにより、主管の上部(35´)の傾きは逆傾斜となり、実質的に図3に示す装置と同じ機能を有する装置を実験的に作製した。 The connecting portion (36a ') of the separation device (30') having the configuration shown in FIG. 6 is connected to the outside of the microwave generator (10) via the connecting pipe (25) so as to be connected to the cylindrical flask (20). Then, 14.22 g of pure water was added as priming water to the receiving tube. A Dimroth cooling pipe (40) having a length of 300 mm was connected to the upper part of the separator through a connecting part (36b ′). In addition, a pipe for supplying excess exhaust gas to the draft was provided at the upper part of the Dimroth cooling pipe. Further, the receiving pipe (32 ') of the separation device was installed so as to incline 1.3 degrees in the left direction of the drawing so that the return condensed water from the Dimroth cooling pipe hardly returned to the extraction container through the main pipe (31'). By doing in this way, the inclination of the upper part (35 ') of the main pipe was reversed, and an apparatus having substantially the same function as the apparatus shown in FIG. 3 was experimentally produced.
その後、実験例1と同様に反応を行い、蒸気発生が終了した時点で反応を終了することとした。 Thereafter, the reaction was carried out in the same manner as in Experimental Example 1, and the reaction was terminated when the generation of steam was completed.
その結果、初留までの所要時間は5分、反応終了までの時間は20分であり、終了時に円筒フラスコ内には十分な水があり、さらに蒸留を続けることが可能であった。反応後の全油分収量は3045mgであった。また、これをバイオマス100g-dryあたりの精油収量に換算すると1874mgであった。 As a result, the time required for the first distillation was 5 minutes, and the time required for completion of the reaction was 20 minutes. At the end of the reaction, there was sufficient water in the cylindrical flask, and distillation could be continued. The total oil yield after the reaction was 3045 mg. Moreover, this was 1874 mg when converted into the essential oil yield per 100 g-dry of biomass.
反応を通して、バイオマスが過加熱になったり、焦げたりすることはなかった。また、凝縮水が抽出容器に戻ってしまう現象も目視では確認されなかった。 Throughout the reaction, the biomass was not overheated or burnt. Moreover, the phenomenon that condensed water returns to an extraction container was not confirmed visually.
<実験例3>
図2に示したマイクロ波発生装置(10)内に設置された内径200mmのセパラブル三ツ口円筒フラスコ(20)に、純水50.04gと沸石を加え、テフロン(登録商標)製の目皿(2)を設置した。目皿の穴は5mmのものを使用し、その上に、バイオマスが下にこぼれ落ちないようにメッシュサイズ0.75φのテフロン(登録商標)パンチングシートを設置した。この上に、バイオマスとしてトドマツ葉粉砕物300.03gを加えた。トドマツ葉粉砕物は分析ミル(IKA Works Guangzhou社製 型式:A11 basic)にて8mmアンダーに破砕して得た。
<Experimental example 3>
To a separable three-necked cylindrical flask (20) with an inner diameter of 200 mm installed in the microwave generator (10) shown in FIG. ) Was installed. A hole with a diameter of 5 mm was used, and a Teflon (registered trademark) punching sheet having a mesh size of 0.75φ was placed thereon so that the biomass would not spill down. On top of this, 300.03 g of ground Todomatsu leaves was added as biomass. Todomatsu leaf pulverized product was obtained by crushing under 8 mm using an analysis mill (model: A11 basic, manufactured by IKA Works Guangzhou).
マイクロ波発生装置(10)外に、円筒フラスコ(20)と連結するように長さ300mmのリービッヒ冷却管(40)を連結し、さらに100ml容の分液ロート(50)を連結した。なお、冷却部(40)にはリービッヒ冷却管に加えて分岐管にて補助冷却用のジムロートを連結してもよい。また、分液ロートとリービッヒ冷却管との連結部を分岐し、余分な排ガスをドラフトへ送気する管を設けた。 A 300 mm long Liebig condenser (40) was connected to the outside of the microwave generator (10) so as to be connected to the cylindrical flask (20), and a 100 ml separatory funnel (50) was further connected. In addition to the Liebig cooling pipe, an auxiliary cooling Dimroth may be connected to the cooling section (40) by a branch pipe. Further, a connecting portion between the separatory funnel and the Liebig cooling pipe was branched, and a pipe for supplying excess exhaust gas to the draft was provided.
その後、実験例1と同様に反応を行い、蒸気発生が終了したり、焦げなどの異臭が発生した時点で反応を終了することとした。 Thereafter, the reaction was carried out in the same manner as in Experimental Example 1, and the reaction was terminated when the generation of steam was completed or when a strange odor such as scorching occurred.
その結果、初留までの所要時間は5分で、反応終了までの時間は15分であった。これは、反応後15分でバイオマスがわずかに焦げる臭いが発生し、危険防止のため反応を終了したためである。反応後の全油分収量は3266.7mg(2011mg/100g-dry)であったが、得られた油分は褐色に着色しており、油成分が熱分解したことが示唆された。また、反応後、円筒フラスコ内のバイオマスの一部がやや焦げていた。 As a result, the time required for the first distillation was 5 minutes, and the time required for completion of the reaction was 15 minutes. This is because 15 minutes after the reaction, a odor that slightly burns the biomass was generated, and the reaction was terminated to prevent danger. The total oil yield after the reaction was 3266.7 mg (2011 mg / 100 g-dry), but the obtained oil was colored brown, suggesting that the oil component was thermally decomposed. In addition, after the reaction, a part of the biomass in the cylindrical flask was slightly burnt.
以上の実験例における精油回収量を試料100g-dryあたりの精油収量に換算した値、および、得られた精油の性状を表1に示した。 Table 1 shows values obtained by converting the essential oil recovery amount in the above experimental examples into the essential oil yield per 100 g-dry of the sample, and the properties of the obtained essential oil.
回収した精油をガスクロマトグラフィー(GC)で分析し、検出された主要成分(ピネン)及び熱劣化成分のピーク面積比(主要成分/劣化成分)を求めた結果、表1に示すように、凝縮水が抽出容器に戻り難くした分離装置では劣化成分が減少することが確認できた。 The recovered essential oil was analyzed by gas chromatography (GC), and the peak area ratio (main component / deteriorated component) of the detected main component (pinene) and heat-degraded component was determined. It was confirmed that the degradation component decreased in the separation device in which the water did not easily return to the extraction container.
上記の結果から明らかなように、本発明の簡易分離装置を用いることにより、他の分離装置と比べて、短時間で熱劣化のない精油をほぼ同量回収することができた。 As is clear from the above results, by using the simple separation device of the present invention, it was possible to recover substantially the same amount of essential oil without thermal degradation in a short time compared to other separation devices.
本発明の分離装置は、各種の溶媒抽出操作に適用することができる。その場合、必要に応じ連結手段を介して、抽出容器および冷却手段に連通させて用いれば良い。これにより、省溶媒、省エネルギー、高効率で有用物質を抽出することが可能になる。各種バイオマスから抽出した各種天然物質は、製薬、化粧品、食品、芳香剤、染色剤、溶剤などの様々な産業分野で利用することができる。 The separation apparatus of the present invention can be applied to various solvent extraction operations. In that case, it may be used in communication with the extraction container and the cooling means via the connecting means as required. Thereby, it becomes possible to extract a useful substance with solvent saving, energy saving, and high efficiency. Various natural substances extracted from various biomasses can be used in various industrial fields such as pharmaceuticals, cosmetics, foods, fragrances, dyes and solvents.
1 バイオマス
2 目皿
3 溶媒
10 マイクロ波発生装置
20 反応容器
21 温度計
25 連結管
30,30´ 分離装置
31,31´ 主管
32,32´ 受け管
33,33´ 戻り管
34,34´ 三方向弁
35,35´ 主管上部
36a,36b,36a´,36b´ 連結部
40 冷却管
50 分液漏斗
DESCRIPTION OF SYMBOLS 1 Biomass 2 Eye plate 3 Solvent 10 Microwave generator 20 Reaction container 21 Thermometer 25 Connecting pipe 30, 30 'Separating device 31, 31' Main pipe 32, 32 'Receptacle 33, 33' Return pipe 34, 34 'Three directions Valves 35, 35 'Main pipe upper parts 36a, 36b, 36a', 36b 'Connection part 40 Cooling pipe 50 Separating funnel
Claims (2)
抽出容器に連通する主管と、
冷却手段に連通する受け管と、
該受け管から前記主管に連通する戻り管と、を備え、
前記受け管は、その下端が三方向弁に連結されると共に、該三方向弁を介して前記戻り管に連通し、該戻り管は、一定の液位を保持しうる垂直高さを有し、その他端が主管に連結されており、
前記主管の上部は、連結端が受け管に対して鈍角を形成するように受け管上部に連結されてなり、
前記主管はその下端に抽出容器との連結部を有し、かつ、前記受け管はその上端に冷却手段との連結部を有する簡易分離装置。 A simple separation device for separating a condensed liquid into a solvent and an extract,
A main pipe communicating with the extraction container;
A receiving pipe communicating with the cooling means;
A return pipe communicating from the receiving pipe to the main pipe,
The receiving pipe has a lower end connected to a three-way valve and communicates with the return pipe via the three-way valve, and the return pipe has a vertical height capable of holding a constant liquid level. The other end is connected to the main pipe,
The upper part of the main pipe is connected to the upper part of the receiving pipe so that the connecting end forms an obtuse angle with respect to the receiving pipe,
The main pipe has a connecting part with an extraction container at the lower end, and the receiving pipe has a connecting part with a cooling means at the upper end.
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