JP4924435B2 - Separation device - Google Patents

Description

  The present invention relates to a simple separation apparatus for easily separating a condensed liquid into a solvent and an extract during the reaction.

  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.

  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.

  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.

  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.

  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.

  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.

  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.

Further, in the oil / water separator, an inverted U-shaped overflow pipe is provided to return the separated water to the oil / water separation tank in order to maintain the liquid level in the oil / water separation tank (Patent Documents 2 and 3). Etc.), and the structure is not such that oil can be easily taken out.
Japanese Unexamined Patent Publication No. 6-99005 JP-A-4-197403 Japanese Patent Laid-Open No. 2001-9204

  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.

  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.

  That is, the present invention provides the following simple separation apparatus.

(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) The simple separation apparatus according to (1), which is used for separation of essential oil extracted from solid biomass by solvent.

  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.

  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.

[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.

  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.

  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.

[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.

  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).

  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.

  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.

  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.

  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.

  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.

[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.

[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;

[Extraction container]
One-neck to four-neck cylindrical separable flasks and the like can be mentioned, but are not particularly limited.

[Cooling means]
Examples include Liebig tubes and Jim Roth, but are not particularly limited.

  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.

  Next, an extraction experiment example using various separation devices will be specifically described with reference to the drawings.

<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).

  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.

  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.

  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.

  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.

<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).

  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.

  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.

  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.

  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.

<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).

  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.

  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.

  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.

  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.

  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.

  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.

  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.

It is a figure explaining the extraction method of Experimental example 1,2. It is a figure explaining the extraction method of Experimental example 3. FIG. It is a schematic block diagram of the separation apparatus of the example of this invention. It is explanatory drawing of the three-way valve periphery of the separation apparatus of the example of this invention. It is explanatory drawing of the three-way valve periphery of the separation apparatus of the example of this invention. It is a schematic block diagram of the comparison separation apparatus.

Explanation of symbols

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)

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.   The simple separation device according to claim 1, which is used for separation of essential oil extracted from solid biomass by solvent.