JP2007098383A - Method for extracting oil from vegetable biomass using microwave, and apparatus therefor - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for extracting oil from vegetable biomass using a microwave that easily extracts at low cost and energy the oil that is easily handled and suited for transportation, and an apparatus to be used therefor. <P>SOLUTION: The method for extracting oil from vegetable biomass using a microwave comprises a step for generating or introducing vapor of an extracting solvent in a device for generating the microwave, a step for extracting oil by heating the above solvent and biomass by the microwave, a step for discharging the solvent vapor containing the oil out of the above device followed by cooling and a step for recovering the extracted oil and the solvent. The apparatus for extracting oil from vegetable biomass is equipped with a means of generating the microwave, a means of generating the solvent vapor, a means of extracting the oil from the vegetable biomass using the solvent vapor, a means of condensing the solvent vapor and a means of recovering the solvent. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method of extracting oil from plant biomass (hereinafter sometimes abbreviated as “biomass”) using microwaves, and an apparatus used therefor. In detail, it is related with the method and apparatus which extract useful substances, such as essential oil and fats and oils, from plant biomass using a microwave.

  As part of global warming countermeasures, there is power generation technology that uses biomass as fuel. Biomass includes industrial biomass such as municipal waste, food residues, and sewage sludge, as well as animal biomass such as livestock manure, plant biomass such as cultivated plants, felled trees, and crop residues. Plant-based biomass is generated by using a pulverized product or processed product (carbonized product, liquefied product, gasified product, etc.) as fuel.

  However, solid biomass is bulky and requires a large amount of energy for collection and transportation, and is not suitable when it is necessary to procure a large amount or when it is carried out far away. In order to solve this problem, there are technologies for biomass liquefaction and gasification (ethanolification, DME, hydrogenation), but currently all of them require large-scale equipment (such as culture equipment for ethanolization), Cost (DME, hydrogenation, etc.).

  In addition, various biomass contains various components, including high-value-added essential oil components, but the current method of using biomass consumes these high-value-added components as fuel. It has been.

  As a method for extracting oil from plant biomass, extraction by pressing, steam, hot water, organic solvent, lard, etc. has been conventionally performed. However, extraction efficiency is reduced by pressing, and extraction time is longer by steam distillation. In addition, the energy consumption is increased, and extraction with hot water or an organic solvent has a problem that the extraction time is long or complicated and the energy consumption is also large.

  In Patent Document 1, water vapor is injected into a pressurized sealed device containing plant material, heated to the core of the plant material by electromagnetic waves, natural fluid is extracted from the plant material, and then the extract is discharged outside the device. A method of collecting by gravity is disclosed. However, this method is an extraction method in which the inside of the apparatus is pressurized, and since an air compressor and a saturated water vapor generation apparatus are indispensable, it is difficult to say that the extraction method is simple.

Patent Document 2 discloses a method of obtaining a plant extract having good temporal stability and little coloration by putting a mixed solution of a raw material plant and an extraction solvent into a glass tube, irradiating with microwaves, and filtering. ing. In Patent Document 3, an electromagnetic wave is caused to act on water molecules as a solvent when oily components and the like are distilled and separated from natural materials such as plants, thereby creating an electron transfer state of the water molecules, which is easily deteriorated by heat and oxidized. A method for stably separating easily fragrant organic components is disclosed. However, these methods are not intended to obtain energy-saving, low-cost, high-value-added substances before burning biomass, but rather are methods devised to obtain high-quality plant extracts. It is.
Special Table 2002-54294 JP 2004-89786 A Japanese Patent Laid-Open No. 9-85001

  The present invention has been made to solve the above-described problems, and is a method for extracting oil from plant biomass using microwaves, which is easy to handle and suitable for transportation. It is an object of the present invention to provide a method for easily extracting at low cost and an apparatus used therefor.

  In order to solve the above-mentioned problems, the present inventors have intensively studied. As a result, the microwave can heat the extraction solvent and the biomass extract itself. By applying the principle of steam distillation using microwaves, we obtained the knowledge that oil such as high-value-added essential oils and fats and oils can be obtained from plant biomass with energy saving and low cost, The present invention has been reached.

That is, the present invention is as follows.
1) A method of extracting oil from plant biomass using microwaves,
In a microwave generator containing plant biomass, an extraction solvent vapor is generated or introduced, and the extraction solvent and plant biomass are heated by microwave to extract oil,
Exhausting the solvent vapor containing the oil out of the apparatus and condensing it to recover the extracted oil and solvent,
2) A method of extracting oil from plant biomass using microwaves,
In the microwave generator, the plant biomass contained in the extraction container is irradiated with microwaves, and the extraction solvent vapor introduced into the device is brought into contact with the plant biomass to extract oil,
Exhausting the solvent vapor containing the oil out of the apparatus and condensing it to recover the extracted oil and solvent,
3) A method of extracting oil from plant biomass using microwaves,
In the microwave generator, the plant biomass contained in the extraction solvent and the extraction container is irradiated with microwaves, the solvent vapor heated by the microwave and the plant biomass are contacted, and oil is extracted,
Exhausting the solvent vapor containing the oil out of the apparatus and condensing it to recover the extracted oil and solvent,
4) The method according to any one of 1) to 3), wherein the extraction solvent is microwave absorbing.
5) The method according to any one of 1) to 4), wherein the extraction solvent is water,
6) The method according to any one of 1) to 5), wherein the plant biomass is cultivation biomass or waste biomass.
7) The method according to any one of 1) to 6), wherein the microwave frequency is 0.5 GHz to 10 GHz.
8) An extraction device for extracting oil from plant biomass,
Microwave generation means, solvent vapor generation means, and extraction means for extracting oil from plant biomass by solvent vapor,
An extraction apparatus comprising heating means for heating the extraction solvent to make it vapor;
9) The extraction device according to 8), wherein the extraction means is an extraction container that contains plant biomass and extracts oil from the plant biomass by extraction solvent vapor,
10) The extraction device according to 8) or 9), which has a storage tank for storing the extraction solvent as the solvent vapor generation means,
11) The extraction device according to any one of 8) to 10), further comprising a solvent vapor condensing unit and a solvent recovery unit,
12) The extraction device according to any one of 8) to 11), wherein the extraction solvent is water,
13) The extraction device according to any one of 8) to 12), wherein the solvent vapor generated by the heating unit is supplied to the extraction unit via a solvent vapor supply path.
14) The extraction device according to any one of 8) to 13), wherein the solvent vapor generated by the heating unit is supplied to the extraction unit disposed above.
15) The extraction device according to any one of 8) to 14), wherein the heating means is a microwave generator or an electric heater.

  ADVANTAGE OF THE INVENTION According to this invention, it becomes possible to extract oils, such as essential oil and fats and oils, in a short time, energy saving, and low cost by heating biomass by microwave irradiation on normal-pressure conditions. The residue after extraction becomes a biomass fuel that has a high calorific value and is easy to handle.

  Hereinafter, preferred embodiments of a method for extracting oil from plant biomass using a microwave according to the present invention and an apparatus used therefor will be described in detail with reference to the drawings.

(Embodiment 1)
FIG. 1 is a diagram for explaining an outline of an extraction method and apparatus when an extraction solvent vapor generating means is outside a microwave generating means (microwave generator) according to an embodiment of the present invention. .

  In FIG. 1, 10 is a microwave generation means (microwave generation apparatus), 20 is a solvent vapor generation means (a storage tank for storing a solvent), and 30 is an extraction means (an extraction container such as a sealable container or tube). , 40 is a solvent vapor condensing means, and 50 is a solvent recovery means. In the solvent vapor generation means 20, the apparatus 20 is heated by the heating means 21, the solvent in the sealed apparatus 20 is heated to generate solvent vapor, and the generated solvent vapor is passed through the solvent vapor supply path 25. Then, it is introduced below the extraction means (extraction container) installed in the microwave generator.

  In the extraction means 30, for example, the raw or dried biomass 1 is placed on the perforated plate 2 provided with a large number of holes that are large enough to allow solvent vapor to pass through, and the oil content in the biomass is extracted. The biomass is not necessarily placed on the perforated plate, but by doing so, the steam can be brought into contact with the biomass more evenly.

  The introduced extraction solvent vapor is heated by the microwave irradiated in the microwave generator, and the heated solvent molecules come into contact with the biomass and pass between the biomasses 1 placed on the perforated plate 2. While rising. Since the placed raw biomass 1 has moisture close to the equilibrium moisture content, the retained moisture is activated by microwaves, and the oil contained in the biomass by the activated water is less than that of normal steam distillation. It becomes easy to be extracted. The extracted oil is discharged out of the apparatus through the solvent discharge path 35 together with the rising solvent vapor. Under the present circumstances, it is preferable that the inside of an apparatus is hold | maintained at 35 to 150 degreeC, More preferably, it is 90 to 140 degreeC. By maintaining the reaction temperature within this range, it is possible to prevent the extracted essential oil component from being decomposed and increase the extraction efficiency. Further, if necessary, the condensation of vapor can be prevented by heating the solvent vapor supply path 25 and the solvent discharge path 35.

  The discharged solvent vapor containing oil is cooled by the solvent vapor condensing means installed outside the microwave generator, and the cooled solvent vapor is recovered by the solvent recovery means. Extracted oil is also contained in the solvent vapor, so that the solvent and the oil component evaporated together can be liquefied by cooling the discharged solvent vapor. The temperature of the cooling section in the solvent vapor condensing means 40 is preferably in the range of −20 to 10 ° C., and preferably in the range of −10 to 5 ° C. when the solvent is water.

  The solvent recovery means 50 recovers the distillate condensed in the solvent vapor condensing means 40 and further liquefies the reaction product cooled in the cooling part of the solvent condensing means 40 at −86 ° C. to 5 ° C. It is also possible to recover the gaseous substances that were not. When the solvent is water, the oil component is separated into the upper layer, so that the oil component can be recovered by collecting it as it is. When the solvent is an organic solvent, only the oil can be recovered by vacuum distillation or the like.

  Further, when the solvent vapor for extraction is insufficient, for example, an operation such as installing a switching valve, a regulating valve or the like in the solvent vapor generating means 20 or the solvent vapor supply path 25 to temporarily open the solvent vapor generating means. By performing the above, it is possible to easily replenish the solvent during the reaction.

  Examples of the extraction solvent (same in the following embodiments) include water, alcohols such as ethers, methanol, and ethanol, and organic solvents such as ethyl acetate, pyridine, tetrahydrofuran, chloroform, and acetone. . All of these extraction solvents are microwave-absorbing, and water is preferable in consideration of cost, safety, and the like.

  In this embodiment, since the moisture originally contained in the biomass can be sufficiently heated, almost all of the microwave energy is used for heating the biomass (not for heating the solvent). Extraction becomes easy.

  In addition, according to the apparatus and method according to the present embodiment, it is possible to supply a large amount of solvent vapor, and to put biomass as much as possible into the space in the microwave generator so that a large amount of biomass can be charged. It is possible to sufficiently expose microwaves to biomass and solvent vapor, and to improve the efficiency of extraction. Moreover, since biomass can be put in the space in a microwave irradiation apparatus as much as possible, biomass can be processed in large quantities at a time. Although this method is suitable for the treatment of a large amount of biomass, it is particularly suitable for the treatment of soft biomass with a lot of moisture such as leaves. Moreover, it is suitable also when using the organic solvent with the low effect of the heating by a microwave.

(Embodiment 2)
FIG. 2 is a diagram for explaining an outline of the extraction method and apparatus when the extraction solvent vapor generation means is in the microwave generation means (microwave generation apparatus) according to an embodiment of the present invention. . In the present embodiment, the solvent vapor generation means is configured to generate vapor by microwave heating, and the generated vapor is configured to be supplied to the extraction means via the solvent vapor supply path 25. Yes.

  In FIG. 2, 10 is a microwave generation means, and the solvent vapor generation means 20 and the extraction means 30 are arranged in a microwave generation apparatus that is a microwave generation means. Reference numeral 40 denotes solvent vapor condensing means, and 50 denotes solvent recovery means. In the solvent vapor generation means 20, the solvent is heated by microwaves to generate solvent vapor, and the generated solvent vapor 25 is introduced into the lower part of the extraction means (extraction vessel) via the solvent vapor supply path 25.

  In the extraction means 30, the raw biomass 1 is placed on the perforated plate 2 provided with a large number of holes large enough to allow solvent vapor to pass through, and the oil content in the biomass is extracted.

  The introduced extraction solvent vapor comes into contact with the biomass placed on the perforated plate 2 while being heated by the microwave irradiated in the microwave generator, and rises while passing between the biomasses 1. Since the placed biomass 1 has moisture close to the equilibrium moisture content, the retained moisture is activated by microwaves, and the oil contained in the biomass is extracted by the activated water. The extracted oil is discharged out of the apparatus through the solvent discharge path 35 together with the rising solvent vapor. Under the present circumstances, it is preferable that the inside of an apparatus is hold | maintained at 35 to 150 degreeC, More preferably, it is 90 to 140 degreeC. By maintaining the reaction temperature within this range, it is possible to prevent the extracted essential oil component from being decomposed and increase the extraction efficiency. Further, if necessary, the condensation of vapor can be prevented by heating the solvent vapor supply path 25 and the solvent discharge path 35.

  The discharged solvent vapor containing oil is cooled by the solvent vapor condensing means installed outside the microwave generator, and the cooled solvent vapor is recovered by the solvent recovery means. Extracted oil is also contained in the solvent vapor, so that the solvent and the oil component evaporated together can be liquefied by cooling the discharged solvent vapor. The temperature of the cooling section in the solvent vapor condensing means 40 is preferably in the range of −20 to 10 ° C., and preferably in the range of −10 to 5 ° C. when the solvent is water.

  The solvent recovery means 50 recovers the distillate condensed in the solvent vapor condensing means 40 and further liquefies the reaction product cooled in the cooling part of the solvent condensing means 40 at −86 ° C. to 5 ° C. It is also possible to recover the gaseous substances that were not. When the solvent is water, the oil component is separated into the upper layer, so that the oil component can be recovered by collecting it as it is. When the solvent is an organic solvent, only the oil can be recovered by vacuum distillation or the like.

  According to the apparatus and method according to the present embodiment, since steam is also generated by microwaves, only one heating means is required, resulting in an energy saving apparatus. 2 shows an example in which the solvent vapor generating means 20 is installed only in the microwave generator 10, the solvent vapor generating means 20 is provided with a solvent supply path leading to the outside of the microwave generator 10, and the apparatus The solvent may be replenished from the outside, which makes it possible to supply a large amount of steam.

  Compared to the case where the steam generating means is provided outside the microwave generator, there is no concern that the steam will be condensed (condensation prevention energy is not required), and it is separate from the biomass extraction reactor. Therefore, both the solvent and the biomass can be irradiated with microwaves. By irradiating the solvent with microwaves, the solvent is easily made into a single molecule, and the property of the solvent vapor is constant as compared with external heating.

  In the present embodiment, since the solvent vapor generation means and the extraction means are separate, there is no possibility that biomass components are mixed into the solvent (vapor generation section), and the remaining solvent can be reused. It is easy to replenish the solvent during the reaction. It is suitable for oils that can be extracted with a small amount of steam compared to the amount of biomass (for example, biomass having a high water content). It is also suitable for oil extraction tests with small amounts.

(Embodiment 3)
FIG. 3 is a diagram for explaining an outline of the extraction method and apparatus when the extraction solvent vapor generation means is in the microwave generation means (microwave generation apparatus) according to an embodiment of the present invention. . In the present embodiment, the solvent vapor generation means is configured to generate vapor by microwave heating, and the generated vapor is supplied to the extraction means directly above without passing through the solvent vapor supply path 25. It is configured.

  In FIG. 3, 10 is a microwave generating means, and an apparatus in which the solvent vapor generating means 20 and the extracting means 30 are integrated is arranged in a microwave generating apparatus that is a microwave generating means. Reference numeral 40 denotes solvent vapor condensing means, and 50 denotes solvent recovery means. In the solvent vapor generating means 20, the solvent is heated by microwaves to generate solvent vapor, and the generated solvent vapor 25 is supplied to the biomass disposed immediately above.

  In the extraction means 30, the raw biomass 1 is placed on the perforated plate 2 provided with a large number of holes large enough to allow solvent vapor to pass through, and the oil content in the biomass is extracted.

  The supplied steam comes into contact with the biomass placed on the perforated plate 2 while being heated by the microwave irradiated in the microwave generator, and rises while passing between the biomasses 1. Since the placed biomass 1 has moisture close to the equilibrium moisture content, the retained moisture is activated by microwaves, and the oil contained in the biomass is extracted by the activated water. The extracted oil is discharged out of the apparatus through the solvent discharge path 35 together with the rising solvent vapor. Under the present circumstances, it is preferable that the inside of an apparatus is hold | maintained at 35 to 150 degreeC, More preferably, it is 90 to 140 degreeC. By maintaining the reaction temperature within this range, it is possible to prevent the extracted essential oil component from being decomposed and increase the extraction efficiency. Further, if necessary, the condensation of vapor can be prevented by heating the solvent vapor supply path 25 and the solvent discharge path 35.

  The discharged solvent vapor containing oil is cooled by the solvent vapor condensing means installed outside the microwave generator, and the cooled solvent vapor is recovered by the solvent recovery means. Since the solvent oil contains extracted oil, the solvent and the oil that has evaporated together can be liquefied by cooling the discharged solvent vapor. The temperature of the cooling section in the solvent vapor condensing means 40 is preferably in the range of −20 to 10 ° C., and preferably in the range of −10 to 5 ° C. when the solvent is water.

  The solvent recovery means 50 recovers the distillate condensed in the solvent vapor condensing means 40 and further liquefies the reaction product cooled in the cooling part of the solvent condensing means 40 at −86 ° C. to 5 ° C. It is also possible to recover the gaseous substances that were not. When the solvent is water, the oil component is separated into the upper layer, so that the oil component can be recovered by collecting it as it is. When the solvent is an organic solvent, the oil can be recovered by vacuum distillation or the like.

  According to the apparatus and method according to the present embodiment, since steam is generated by microwaves, only one heating means is required, and the apparatus is the most energy-saving. FIG. 3 shows an example in which the solvent vapor generating means 20 is installed only in the microwave generator 10, but the solvent vapor generating means 20 is provided with a solvent supply path leading to the outside of the microwave generator 10, and the apparatus The solvent may be replenished from the outside, which makes it possible to supply a large amount of steam.

  Compared to the case where the steam generating means is provided outside the microwave generator, there is no concern that the steam will be condensed (condensation prevention energy is not required), and it is separate from the biomass extraction reactor. Therefore, both the solvent and the biomass can be irradiated with microwaves. By irradiating the solvent with microwaves, the solvent is easily made into a single molecule, and the property of the solvent vapor is constant as compared with external heating.

  In the present embodiment, the generated steam can be immediately applied to the biomass, and the steam pressure applied to the biomass can be slightly increased in the three types of apparatuses shown in FIGS. It is suitable for extracting oil components with boiling points, extracting oil from slightly crushed biomass, and hard (trunk, fruit shell, etc.) biomass. By increasing the vapor pressure, the oil inside the biomass is attracted by the surrounding moisture and is easily extracted. The shape of the extraction container is preferably one having a shape that spreads as much as possible in the interior of the microwave generator, since the area to be irradiated with microwaves can be increased.

  In the apparatus and method according to the present invention, cultivation biomass and waste biomass are mainly used as plant biomass. Examples of cultivated biomass include trees, grass leaves, fruits, branches, and roots. Waste biomass includes timber, thinned wood, felled trees, pruned branches, sawdust, bark, chips, wood chips, driftwood, bamboo, firewood, wood construction waste wood, etc .; fir shell, rice straw, wheat straw, Agricultural biomass such as bagasse and oil palm (raw material of palm oil); food biomass such as food residues from food factories and the restaurant industry. Among these, from the viewpoint of oil content, cultivated biomass and food-based biomass are good, and cultivated biomass is suitable in terms of component stability. Moreover, fruit and leaves are preferable among cultivated biomass, and conifers are generally preferable to hardwoods.

  In the present invention, microwaves are irradiated to the biomass separated from the extraction solvent, so that moisture contained in the biomass can be directly heated, and oil components in the biomass are extracted more than ordinary steam distillation. It becomes easy.

  The output, frequency, and irradiation method of the microwave irradiated from the microwave generator are not particularly limited, and may be electrically controlled so that the reaction temperature can be maintained within a predetermined range. If the output is too low, the amount of solvent vapor generated will be small. If the output is too high, biomass will ignite, bumping of the solvent and rapid evaporation will occur. desirable. The microwave frequency is preferably 0.5 to 10 GHz. If the frequency is less than 0.5 GHz, the solvent molecules can follow the direction of the electric field and the heating efficiency is poor, and if the frequency exceeds 10 GHz, the container such as glass is heated, which is not efficient. Microwave irradiation may be either continuous irradiation or intermittent irradiation, but it is preferable to perform continuous irradiation while being electrically controlled. As the microwave oscillator, a microwave oscillator such as a magnetron, a microwave oscillator using a solid element, or the like can be used as appropriate.

  Moreover, the material of the apparatus used for the solvent vapor generation means and extraction means installed in the microwave generator is a material that transmits microwaves, such as polyethylene, Teflon (registered trademark) plastic, earthenware, quartz glass, etc. Is preferred.

  Hereinafter, the present invention will be described more specifically with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples.

<Example 1 (Steam introduction type of Embodiment 1)>
A Teflon eye plate (2) was installed in a separable three-necked cylindrical flask (30) having an inner diameter of 100 mm and a height of 100 mm installed in the microwave generator (10) shown in FIG. A 5 mm hole was used for the eye plate, and a Teflon punching sheet having a mesh size of 0.75φ was installed on the top so that the biomass would not spill down. On top of this, 53.92 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).

  In addition to the microwave generator (10), a 500 ml eggplant type flask (20) containing 161.09 g of pure water and zeolite was placed in the mantle heater (21) and connected to the cylindrical flask (30). did. Further, a Liebig condenser (40) having a length of 300 mm was installed so as to be connected to the cylindrical flask, and a 100 ml separatory funnel (50) was connected thereto. In addition to the Liebig cooling pipe, an auxiliary cooling Dimroth may be further 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.

  The eggplant-shaped flask (20) is heated with a mantle heater at 120 ° C., and when the generated steam reaches the cylindrical flask (30), the cylindrical flask is irradiated with microwaves having a frequency of 2.45 GHz, and biomass While controlling the microwave output so as to keep the sample temperature at 120 to 150 ° C., the reaction was performed for 60 minutes, and steam distillation was performed. The total reaction time at this time was 80 minutes. When appropriate during the reaction, an appropriate amount of the aqueous layer (lower layer) of the liquid collected in the separating funnel was transferred to another container (distilled water container) so that oil-water separation was always possible in the separating funnel.

  The amount of essential oil recovered every 10 minutes from the initial distillation of steam distillation was measured. The total oil yield after the reaction was 779.4 mg. Moreover, it was 3583.23 mg when this was converted into the essential oil yield per biomass 100g-dry.

  The calorific value of the obtained essential oil was 42463 J / g as measured with a calorimeter-J from Yoshida Seisakusho.

<Example 2 (steam generation, tandem type of embodiment 3)>
To a separable three-necked cylindrical flask (30) having an inner diameter of 100 mm and a height of 100 mm installed in the microwave generator (10) shown in FIG. Was installed. The same thing as Example 1 was used for the eye plate and the biomass fall prevention sheet. On top of this, 53.92 g of Todomatsu leaf pulverized material pulverized to 8 mm under as biomass was added. A Liebig condenser tube (40) having a length of 300 mm was connected to the outside of the microwave generator (10) so as to be connected to the cylindrical flask (30), 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.

  The reaction apparatus was irradiated with microwaves having a frequency of 2.45 GHz, and the reaction was performed for 60 minutes while controlling the microwave output so as to keep the biomass sample temperature at 120 to 150 ° C., and steam distillation was performed. In addition, of the liquid collected in the separating funnel at an appropriate time during the reaction, an appropriate amount of the aqueous layer (lower layer) was transferred to a distilled water container so that oil-water separation was always possible in the separating funnel.

  The amount of essential oil recovered every 10 minutes from the initial distillation of steam distillation was measured. The total oil yield after the reaction was 549.7 mg. Moreover, when this was converted into the essential oil yield per 100 g-dry of biomass, it was 2527.20 mg.

<Comparative example (conventional steam distillation)>
Except not performing microwave irradiation, the steam distillation of the conventional method was performed by the same apparatus structure as Example 1. FIG. Ribbon heaters were installed as auxiliary heating means at the steam introduction connecting portion between the eggplant-shaped flask (20) for generating steam and the reaction vessel (30) and at the connecting portion between the reaction vessel outlet and the Liebig condenser. To a 500 ml eggplant type flask (20) installed in the mantle heater (21), 499.99 g of pure water and zeolite were added. In the reaction vessel (30), 60.08 g of pulverized Todomatsu leaf was added to the eye plate and the biomass falling prevention sheet.

  The eggplant-shaped flask (20) was heated with a 120 ° C. mantle heater, and the ribbon heater installed at the steam inlet connection portion and the connection portion between the reaction vessel outlet and the Liebig condenser was also heated at 120 ° C. The reaction was performed for 60 minutes from the time when the generated steam reached the reaction vessel (30), and steam distillation was performed. Further, the total reaction time at this time was 133 minutes. In addition, of the liquid collected in the separating funnel at an appropriate time during the reaction, an appropriate amount of the aqueous layer (lower layer) was transferred to a distilled water container so that oil-water separation was always possible in the separating funnel.

  The oil yield after the reaction was 525.1 mg. Moreover, it was 2166.59 mg when this was converted into the essential oil yield per 100 g-dry of biomass.

  Table 1 shows the results of values obtained by converting the amount of recovered essential oil every 10 minutes from the first distillation in Examples 1 and 2 and Comparative Examples into the yield of essential oil per 100 g-dry of the sample. As is apparent from Table 1, this example was able to recover a large amount of essential oil in a shorter time than steam distillation.

<Example 3 (comparison of power consumption)>
The power consumption in the reactions of Examples 1 and 2 and Comparative Example was measured. The power consumption of the microwave irradiation device was calculated from the integrated value obtained from the data logger obtained from the power supply value from the microwave irradiation control device. The power consumption of the mantle heater was obtained by measuring the power consumption with a WT130 digital power meter manufactured by YOKOGAWA. Table 2 shows the results of comparing the energy consumption per unit essential oil yield of each Example, based on the value in the comparative example (conventional method). From the results in Table 2, it can be seen that the method and apparatus of the present invention are energy saving compared to the conventional method.

  By the method of the present invention, various natural substances can be extracted from plant biomass, and the extract can be used in various industrial fields such as pharmaceuticals, cosmetics, foods, fragrances, and dyes. Moreover, the plant biomass after extraction can be utilized as a fuel. Furthermore, the method and apparatus of the present invention can be applied to small scale extraction tests.

It is a block diagram which shows the outline of the extraction apparatus which concerns on Embodiment 1. FIG. It is a block diagram which shows the outline of the extraction apparatus which concerns on Embodiment 2. FIG. It is a block diagram which shows the outline of the extraction apparatus which concerns on Embodiment 3.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Biomass 2 Porous board 10 Microwave generation means 20 Solvent vapor generation means 21 Heating means 25 Solvent vapor supply path 30 Extraction means 35 Solvent discharge path 40 Solvent vapor condensation means 50 Solvent recovery means

Claims (15)

A method for extracting oil from plant biomass using microwaves,
In a microwave generator containing plant biomass, an extraction solvent vapor is generated or introduced, and the extraction solvent and plant biomass are heated by microwave to extract oil,
A method comprising exhausting the solvent vapor containing the oil out of the apparatus and condensing it to recover the extracted oil and the solvent. A method for extracting oil from plant biomass using microwaves,
In the microwave generator, the plant biomass contained in the extraction container is irradiated with microwaves, and the extraction solvent vapor introduced into the device is brought into contact with the plant biomass to extract oil,
A method comprising exhausting the solvent vapor containing the oil out of the apparatus and condensing it to recover the extracted oil and the solvent. A method for extracting oil from plant biomass using microwaves,
In the microwave generator, the plant biomass contained in the extraction solvent and the extraction container is irradiated with microwaves, the solvent vapor heated by the microwave and the plant biomass are contacted, and oil is extracted,
A method comprising exhausting the solvent vapor containing the oil out of the apparatus and condensing it to recover the extracted oil and the solvent.   The method according to claim 1, wherein the extraction solvent is microwave-absorbing.   The method according to claim 1, wherein the extraction solvent is water.   The method according to any one of claims 1 to 5, wherein the plant biomass is cultivated biomass or waste biomass.   The method according to any one of claims 1 to 6, wherein a frequency of the microwave is 0.5 GHz to 10 GHz. An extraction device for extracting oil from plant biomass,
Microwave generation means, solvent vapor generation means, and extraction means for extracting oil from plant biomass by solvent vapor,
An extraction apparatus comprising heating means for heating the extraction solvent to make it vapor.   The extraction device according to claim 8, wherein the extraction means is an extraction container that contains plant biomass and extracts oil from the plant biomass by extraction solvent vapor.   The extraction device according to claim 8 or 9, further comprising a storage tank for storing the extraction solvent as the solvent vapor generation means.   The extraction device according to any one of claims 8 to 10, further comprising a solvent vapor condensing unit and a solvent recovery unit.   The extraction device according to any one of claims 8 to 11, wherein the extraction solvent is water.   The extraction apparatus according to any one of claims 8 to 12, wherein the solvent vapor generated by the heating means is supplied to the extraction means via a solvent vapor supply path.   The extraction apparatus according to any one of claims 8 to 13, wherein the solvent vapor generated by the heating unit is supplied to the extraction unit disposed above. The extraction device according to any one of claims 8 to 14, wherein the heating means is a microwave generator or an electric heater.

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