JP6236350B2 - Oily component extraction method - Google Patents

Description

  The present invention relates to a method for extracting an oily component from a predetermined material, and more particularly, to a method for extracting an oily component from a material containing a large amount of water in addition to algae containing the oily component.

  For example, algae such as squid are capable of producing many oily components and can be cultured in water. Therefore, it is proposed to extract oily components from such algae and use them as materials for biofuels. Has been.

  For the purpose of extracting an oil component from such an oil component-containing material, an extraction method for extracting an oil component from an oil component-containing material using an extraction solvent is known. As such an extraction method, for example, a hexane extraction method using hexane as an extraction solvent is known (see Patent Document 1).

JP 2011-68741 A

  However, since algae cultured in water contain a large amount of water even in a state where they are taken out from water and collected, it is very difficult to extract oily components from materials containing algae. Furthermore, in the hexane extraction method using such algae as a material, the algae culture step, the obtained algae concentration step, the concentrated algae dehydration step, the dehydrated algae drying step, and the dried algae crushing Complicated processes such as a process, an extraction process using hexane, and a thermal separation process between hexane and an oil component are necessary.

  Therefore, the subject of this invention is providing the extraction method of the oil component which can perform the extraction of the oil component from the material containing a lot of water | moisture content in addition to an oil component in a simple process efficiently. .

As a result of diligent research, the present inventors have found that the above-described problems can be solved by performing treatment with dimethyl ether (hereinafter sometimes referred to as DME) and treatment with a separation solvent such as hexane, The present invention has been completed.
That is, the present invention provides the following [1] to [6].
[1] A method for extracting an oily component from a material containing moisture and an oily component,
Step (A) A step of contacting the material with dimethyl ether in a liquid state in a container to obtain a treated product,
Step (B) removing dimethyl ether in the treated product as dimethyl ether in a gaseous state;
Step (C) adding a separation solvent to the treated product from which dimethyl ether has been removed, and dissolving the oil component in the separation solvent;
Step (D) selectively obtaining the separation solvent in which the oil component is dissolved;
A step (E) of extracting the oily component from the separation solvent in which the oily component is dissolved.
[2] The step (A) is a step of obtaining a mixed liquid of the material and dimethyl ether in a liquid state as the treated product.
The step (B) is a step of obtaining a mixed liquid from which dimethyl ether has been removed by introducing dimethyl ether in the mixed liquid out of the container as dimethyl ether in a gaseous state,
The method for extracting an oily component according to [1], wherein the step (C) is a step of further adding a separation solvent to the mixed solution from which dimethyl ether has been removed and dissolving the oily component in the separation solvent.
[3] The oil component extraction method according to [2], wherein the step (A) is a step of mixing the material and dimethyl ether in a liquid state and stirring in the container.
[4] In the step (B), the dimethyl ether led out of the container is recovered, and the recovered dimethyl ether is supplied as liquid dimethyl ether to the mixed liquid from which the dimethyl ether has been removed. And extracting the oily component according to [2] or [3], further including a step of repeating the step of obtaining the mixed solution one or more times by inducing gas as dimethyl ether outside the container.
[5] The method for extracting an oily component according to any one of [1] to [4], wherein the separation solvent is selected from the group consisting of pentane, hexane, and heptane.
[6] The method for extracting an oil component according to [5], wherein the separation solvent is hexane.

  ADVANTAGE OF THE INVENTION According to this invention, in addition to an oil-based component, extraction of the oil-based component from the material derived from the algae obtained by culture | cultivation containing a lot of water | moisture content can be performed efficiently by a simple process.

FIG. 1 is a diagram schematically showing the configuration of an apparatus used for the extraction method.

1. Extraction Method First, the extraction method will be described.
The method for extracting an oil component according to an embodiment of the present invention is a method for extracting an oil component from a material containing a large amount of moisture in addition to the oil component.

  The extraction method according to the embodiment of the present invention is a flow-through mode in which dimethyl ether is brought into contact with the material while circulating (circulating) the inside and outside of the container, and a stirring type in which dimethyl ether and the material are mixed (stirred) in a closed system ( It can be applied to any of the batch type embodiments. Hereinafter, both aspects will be described.

(material)
As a material to which the extraction method according to the embodiment of the present invention is applied, any material containing an oily component and moisture can be used. Here, the “oil component” refers to a substance containing one or more components extracted by the extraction method according to the embodiment of the present invention. The oily component to be extracted may be a useful component or an unnecessary component to be removed, for example, harmful to the environment or the human body. Components that can be used are preferred.

  Examples of extracting useful oily components include coal containing subbituminous coal, lignite, lignite, peat, etc., water-containing substances such as sewage sludge, biomaterials containing oily components, and a mixture containing a large amount of moisture. An example in which an oily component is extracted from the material to produce a useful oily material such as a raw material for biofuel can be given.

  Specific examples of the biomaterial include seeds such as algae, sunflower, sesame, and corn that can produce and contain oily components such as Euglena and Ikadamo, and the bone marrow of sugarcane stems. From the viewpoint of efficiently obtaining a useful oily material such as a raw material for biofuel, it is preferable to use Euglena as the biomaterial.

  Moreover, as a mixture containing the said biomaterial, the mixture containing various substances used for these biomaterials and the culture | cultivation as needed can be mentioned. For example, when using an organism that can be cultivated in the aquatic environment such as algae that can produce and contain oily components as the biomaterial, the organism and water collected (concentrated) by any suitable treatment such as filtration and centrifugation are used. The containing mixture can be subjected to the extraction method of the present invention. In addition, from the viewpoint of stable supply and storage of materials, processed materials obtained by subjecting biological materials to treatments such as freezing, drying, and crushing may be used.

  It is preferable from the viewpoint of energy efficiency that the moisture content in the material is smaller. However, in the extraction method of the present invention, the content ratio of moisture in the material (the ratio of moisture to the total amount of the material immediately before being subjected to the step (A)) may be 50% by mass or more, and further 90% by mass. % Or more. In particular, when a stirring method is used, the content of water in the material may be about 95% by mass. Even in such a material containing a large amount of moisture, the extraction method according to the embodiment of the present invention can efficiently extract the oil component. Therefore, extraction of oily components can be carried out even when a material that has been subjected to preliminary dehydration treatment only before being subjected to the extraction method of the present invention, or a material that has not been subjected to preliminary dehydration treatment, can be used. It can be carried out efficiently with a simple process.

  In the extraction method according to the embodiment of the present invention, the oil component contained in the material is a substance other than water, and can be dissolved in liquid dimethyl ether and / or a separation solvent at a concentration equal to or higher than the saturation solubility of water. It is a substance. Preferably, the solubility of the oily component in dimethyl ether is at least 10 times that of water in dimethyl ether and / or a separation solvent, and more preferably, the oily component is compatible with dimethyl ether and / or the separation solvent in any proportion. . Many oily components are compatible with dimethyl ether in liquid state and / or separation solvent in any proportion, and any of these can be applied to the extraction method of the present invention.

  Preferable examples of oily components that can be extracted by the extraction method according to the embodiment of the present invention include useful oily components contained in the biomaterial as described above, particularly oily components produced and contained by algae. . Examples of such algae include Euglena, Scenedesmus, Chlorella, Arthrospira, Botryococcus, Pseidischic. Algae to which it belongs.

  The algae that can be used may be artificially cultured algae or algae collected in a natural environment.

  For example, when Euglena is cultured as such algae and used as a material, it can be cultured by a conventionally known method described in, for example, “Euglena Physiology and Biochemistry”, Academic Publishing Center (1989).

  The oily component that is produced by algae and that can be extracted by the extraction method according to the embodiment of the present invention is not particularly limited. Examples of components that can be contained in oily components produced by algae include aliphatic ester compounds in which aliphatic carboxylic acids and aliphatic alcohols are ester-bonded, solid at room temperature in the range of about 15 to 40 carbon atoms Or the aliphatic hydrocarbon which is a liquid form is mentioned. Examples of aliphatic hydrocarbons include linear aliphatic hydrocarbons. Specific examples of such aliphatic hydrocarbons include heptadecene and eicosadiene.

(Process (A))
The extraction method according to the embodiment of the present invention includes a step (A) of obtaining a processed product by bringing a material into contact with dimethyl ether in a liquid state in a container.
Step (A) is a step of extracting the oil component contained in the material by dissolving it in dimethyl ether.

  The dimethyl ether in the liquid state can contain 7.2% by mass of water at 20 ° C. and 7.8% by mass of water at 30 ° C. Further, dimethyl ether can dissolve a larger amount of oily components even in a state containing moisture as already described. Furthermore, since dimethyl ether in a liquid state has a weaker polarity than water, it dissolves an oily component and is easily separated from water in a gas state.

  If dimethyl ether having such characteristics is used, even if algae containing a large amount of water is used as a material, for example, the process of destroying the cell walls of algae, that is, the drying and crushing processes of algae, and the removal of water Even without carrying out the step, the oily component can be extracted directly from algae containing a large amount of water very easily.

  When the step (A) is performed by a stirring method, the step (A) is a step of obtaining a mixed liquid as a processed product by bringing the material and liquid dimethyl ether into contact with each other in a container.

  The mode of contact between the material and liquid dimethyl ether in step (A) is not particularly limited, and is a stirring type mode in which the material and liquid dimethyl ether are brought into contact with each other and mixed in a container. It is possible to adopt any mode adopted in the extraction method using dimethyl ether, such as a flow mode that circulates in a circulating manner and passes the flow of dimethyl ether through the material, and appropriately selects according to the properties of the material. Can do.

  More specifically, when step (A) is carried out in a flow-through manner, step (A) is a step of obtaining a mixed liquid as a processed product by bringing a material and liquid dimethyl ether into contact with each other in a container. Alternatively, the process may be a step of obtaining an extract and a residue obtained by solid-liquid separation of a mixture obtained by bringing the material and liquid dimethyl ether into contact with each other using a filter or the like. .

  When the step (A) is carried out by a flow-through method, the step of reintroducing the extract obtained by solid-liquid separation into the container may be further performed once or twice or more. Since dimethyl ether can contain a large amount of oily components, the recovery rate of the oily components can be further increased in this way.

  Examples of the production method and production apparatus of dimethyl ether that can be used in the step (A) include JP-A-11-130714, JP-A-10-195009, JP-A-10-195008, and JP-A-10-182527. No. 10-182535, No. 09-309850, No. 09-309852, No. 09-286754, No. 09-173863, No. 09-173848, Special No. 09-173845 is cited.

  From the viewpoint of making the process simpler and simplifying the configuration of the apparatus to be used, there is a stirring type embodiment in which the material and liquid dimethyl ether are stirred in a container, and the material and liquid dimethyl ether are brought into contact with each other and mixed. preferable.

  If the stirring type mode in which the material and dimethyl ether in a liquid state are brought into contact with each other is mixed, there is no need to perform a centrifugal separation step and a filtering step, so that a simpler process and a simpler device configuration are used. Can do. Further, since the recovery rate of dimethyl ether can be increased, the cost can be further reduced.

  The amount of dimethyl ether used in the step (A) can be any suitable amount provided that the object of the present invention is not impaired.

  When the step (A) is carried out by the stirring method already described, the amount of dimethyl ether used is such that the mass of the dimethyl ether is from the viewpoint of the extraction rate of the oil component, and the material contains 95% by mass of water. In such a case, the amount may be about 1000 with respect to the mass of components (solid content) other than water. The ratio of the mass of dimethyl ether to the mass of components other than water is preferably about 200, more preferably about 160.

  When the material is algae or the like that has been dried and crushed, the amount of DME in the liquid state is the weight of the DME (DME weight) and the weight of the completely dried material (absolutely dry weight). The ratio “DME weight / absolute dry weight” may be set to an amount of about 1000 from the viewpoint of the extraction ratio of the oil component. The value of “DME weight / absolute dry weight” is preferably about 200, more preferably about 160, from the viewpoint of the extraction rate of the oil component.

  When step (A) is carried out in a stirring manner, the stirring is performed by shaking (shaking) the container itself, or the mixture in the container is stirred using a conventionally known stirring means such as a stirring blade or a stirring bar. It can be carried out by stirring.

  In the step (A), other materials other than these may be mixed in the system in which the material and dimethyl ether are brought into contact with each other. As another substance, for example, an auxiliary extraction solvent may be mixed. Such other substance is preferably a substance which is a gas at 25 ° C. (normal temperature) and 1 atm, like dimethyl ether. Moreover, it is preferable that it is a substance provided with 1 or more of a characteristic with low toxicity, an oily component being easy to melt | dissolve, and being easily available. Examples of other substances include ethyl methyl ether, formaldehyde, acetaldehyde, butane and propane. Among these, butane and propane can be preferably used from the viewpoints of easy availability (low cost), low toxicity, and low risk of handling.

  Dimethyl ether is in a gaseous state at normal temperature and normal pressure, but is usually in a liquid state at a normal temperature in a range of about 3.5 atm (0.35 MPa) to 5 atm (0.51 MPa). Therefore, since the process (A) is performed under a pressurized condition at room temperature, the configuration of the container used in the process (A) and the pipes, valves, etc. connected to the container can handle dimethyl ether in a liquid state. Is done. Here, “normal temperature” means a temperature at which temperature adjustment is not particularly performed, and is generally a temperature in the range of about 0 ° C. to 50 ° C. The “normal pressure” means a pressure (atmospheric pressure) in which pressure is not particularly adjusted.

  In carrying out the step (A), from the viewpoint of the saturated vapor pressure of dimethyl ether, when the temperature is −10 ° C. to 50 ° C., the pressure in the container may be in the range of 0.18 MPa to 1.14 MPa. When the temperature is 0 ° C. to 40 ° C., the pressure is more preferably in the range of 0.26 MPa to 0.89 MPa.

  The time required for the step (A) to be carried out by stirring, that is, the upper limit of the time during which the material and the liquid dimethyl ether are kept in contact with each other is not particularly limited on the condition that the oily component is reliably extracted. . Even if the time required when the step (A) is performed by a stirring method is within 5 minutes, for example, it is considered sufficient for extraction of the oil component. The time required for the step (A) can be set to, for example, about 5 minutes to 30 minutes from the viewpoint of achieving both reliable extraction of the oil component and simplicity of the step.

  Thus, when a process (A) is performed by a stirring type, the time required for a process (A) and by extension, the time required for implementation of the extraction method of the oily component of this invention can be shortened.

(Process (B))
The method for extracting an oil component according to the embodiment of the present invention includes a step (B) of removing dimethyl ether in the treated product as dimethyl ether in a gaseous state.

  Step (B) is a step of separating the oily component compatible with methyl ether from dimethyl ether by removing dimethyl ether by vaporizing it. By this step, the oily component extracted from the material in step (A) is separated from dimethyl ether and is present in the mixed solution in a state isolated from the material and dimethyl ether.

  Step (B) is performed after sufficiently contacting (mixing) the material and liquid dimethyl ether in step (A).

  In the case of the stirring type, step (B) is a step of obtaining a mixed liquid from which dimethyl ether has been removed by deriving dimethyl ether in the mixed liquid out of the container as gaseous dimethyl ether.

  In the case of a flow-through type, step (B) is a step of obtaining a mixed liquid from which dimethyl ether has been removed by deriving dimethyl ether in the mixed liquid out of the container as dimethyl ether in a gaseous state, or a processed product The step of obtaining an extract from which dimethyl ether has been removed by placing the extract obtained by solid-liquid separation under reduced pressure conditions.

  In the step (B), the pressure is reduced to a pressure at which at least a part or all of dimethyl ether is in a gaseous state, so that dimethyl ether in a gaseous state is guided out of the system through piping, valves, etc. as much as possible. This is done by removing. The step (B) is preferably a step of gradually reducing the pressure over time from the viewpoint of preventing bumping.

  In carrying out the step (B), from the viewpoint of efficiently removing dimethyl ether, the pressure after depressurization is, for example, a temperature of about −10 ° C. to 50 ° C. and a pressure of about 0.18 MPa to 1.14 MPa. The temperature is preferably about 0 ° C. to 40 ° C., and the pressure is more preferably about 0.26 MPa to 0.89 MPa.

  In order to remove dimethyl ether more efficiently, the pressure may be reduced to a pressure lower than the atmospheric pressure, or the container itself may be swung.

  Step (B) may further include a further step such as further heating the mixed solution or the extract from which dimethyl ether has been removed to a temperature equal to or higher than the boiling point of dimethyl ether corresponding to the pressure. By carrying out such further steps, it is possible to further reduce the residual proportion of dimethyl ether that inevitably remains after the step (B).

  As described above, dimethyl ether is in a liquid state at normal temperature and at a relatively low pressure, and is in a gaseous state at normal temperature and normal pressure. Therefore, dimethyl ether in a liquid state is only decompressed to the predetermined pressure or normal pressure at normal temperature. It is easy to separate and remove as dimethyl ether in the gaseous state. Therefore, the extraction method according to the embodiment of the present invention can be implemented in a simpler process, and the configuration of equipment and apparatus necessary for the implementation can be further simplified.

  In step (B), dimethyl ether derived outside the container is recovered, and the recovered dimethyl ether is supplied as liquid dimethyl ether to the mixed liquid from which dimethyl ether has been removed, and then step (A) is performed. As described above, the method may further include a step of repeating the step of obtaining the liquid mixture one or more times (hereinafter referred to as a recovery and a repetition step) by being led out of the container.

  In the step (B), the recovered gaseous dimethyl ether is converted into a liquid dimethyl ether, and any suitable method known to those skilled in the art, such as a compression (pressurization) step, a cooling step, or a combination thereof, is conventionally known. Any suitable apparatus can be used.

  If the “recovery and repetition step” already described is performed, the oily component can be extracted more effectively from the mixed solution, that is, the material, and the oily component recovery rate can be further improved.

(Process (C))
The method for extracting an oily component according to an embodiment of the present invention includes a step (C) of further adding a separation solvent to the treated product from which dimethyl ether has been removed and dissolving the oily component in the separation solvent.
Step (C) is a step of separating the oily component extracted from the material in steps (A) and (B) from the mixture or the extract by dissolving it in a separation solvent.

  The amount of the separation solvent used in the step (C) can be any suitable amount provided that the object of the present invention is not impaired.

  In carrying out the step (C), the amount of the separation solvent is such that the ratio of the mass of the separation solvent to the mass of the treated product from which dimethyl ether has been removed is about 10 from the viewpoint of efficient separation of the oil component. Good. Regarding the amount of the separation solvent, the ratio of the mass of the separation solvent to the mass of the treated product from which dimethyl ether has been removed is preferably about 3, and more preferably about 1.

  Step (C) can be carried out by adding the separation solvent to the mixture or the extract at normal temperature and pressure and shaking the container, or stirring with a stirring blade, a stirring bar, or the like.

  Step (C) may be repeated two or more times. By performing the step (C) a plurality of times, the oil component recovery rate can be further improved.

  As a separation solvent that can be used in the step (C), for example, pentane, hexane, heptane, dichloromethane, chloroform, acetone, ethyl acetate, benzene, ethers, and toluene can be used. The separation solvent is preferably selected from the group consisting of pentane, hexane, and heptane, and more preferably hexane, from the viewpoint of ease of handling.

  When the extraction method according to the embodiment of the present invention is performed in a flow-through manner, an oil component that has inevitably remained is separated by adding a separation solvent to the solid component that has been solid-liquid separated. You may perform a process further. By carrying out such a step, the oil component recovery rate can be further improved.

(Process (D))
The method for extracting an oil component according to an embodiment of the present invention includes a step (D) of selectively obtaining a separation solvent in which the oil component is dissolved.
Step (D) is a step of fractionating the separation solvent in which the oil component is dissolved.

  First, the container in which the step (C) has been performed is allowed to stand at room temperature for a predetermined time. The time for standing the container is preferably 1 minute to 3 minutes from the viewpoint of stabilizing the layer (phase) formed by the separation solvent and the mixed solution or the extract (residue), and is within 1 minute. It is more preferable.

  By this standing, the separation solvent in which the oil component is dissolved and the mixed solution or the extract (residue) are separated into layers (phases).

  Subsequently, only the separation solvent in which the oil component is dissolved is separated. This sorting step can be performed by any conventionally known and suitable sorting method and apparatus.

(Process (E))
The method for extracting an oil component according to an embodiment of the present invention includes a step (E) of extracting the oil component from a separation solvent in which the oil component is dissolved.

  By performing the step (E) after the step (D), the oily component is obtained by extracting the oily component from the separated “separated solvent in which the oily component is dissolved”.

  Step (E) can be performed by removing the separated solvent in a gaseous state under conditions such as temperature and pressure at which only the selected separation solvent is in a gaseous state and the oil component is in a liquid state.

  In the step (E), for example, when the separation solvent is hexane, the separation solvent hexane can be removed by setting the temperature to about 40 ° C. under vacuum (reduced pressure) conditions.

  By carrying out the steps (A) to (E), the oil component can be extracted from the material.

(Other processes)
The extracted oily component may be subjected to any conventionally known suitable purification step in order to extract only a specific component, for example.
When the extracted oily component is used as a fuel (biofuel), any conventionally known suitable process such as hydrodeoxygenation process, hydrocracking process, hydroisomerization process, methyl esterification A reforming process such as a process may be performed.

(Residue)
The residue after the oil component is extracted may be disposed of by a predetermined method suitable for the selected material, or may be reused.
For example, when algae is used as a material, the residue can be used for uses such as pharmaceuticals, cosmetics, foods, health foods, foods for specified health use, chemicals (industrial materials), feeds, fertilizers, fuels and the like.

2. Apparatus Hereinafter, an apparatus for carrying out an extraction method according to an embodiment of the present invention will be described with reference to the drawings.

  The drawings only schematically illustrate the shape, size and arrangement of the components to the extent that the invention can be understood. The present invention is not limited by the description based on the following drawings, and each component can be appropriately changed without departing from the gist of the present invention.

FIG. 1 is a diagram showing a configuration of an apparatus used in an extraction method according to an embodiment of the present invention.
The apparatus used for the extraction method according to the embodiment of the present invention has a function of extracting an oil component from a material containing moisture and an oil component.

  As shown in FIG. 1, the apparatus 10 includes a container 20 in which the material can be contacted (mixed) with dimethyl ether or a separation solvent. In addition, the apparatus 10 connects the storage tank 30 in which dimethyl ether and / or a separation solvent are stored, the container 20 and the storage tank 30, and introduces piping for introducing the dimethyl ether and / or the separation solvent into the container 20. 42.

  The apparatus 10 is further connected at one end to the container 20, and a lead-out pipe 44 for leading the gaseous dimethyl ether to the outside of the container 20, and a valve 50 provided in the lead-out pipe 44 for adjusting the pressure inside the container 20. And a liquefier 60 that is connected to the other end of the outlet pipe 44 and liquefies gaseous dimethyl ether to make it liquid.

  The apparatus 10 is further connected at one end to the container 20 and has a separation pipe 48 for leading the separation solvent containing the oil component to the outside of the container 20, and is connected to the other end of the separation pipe 48 and contains the oil component. And a separation tank 70 for storing a separation solvent. The separation tank 70 may be configured to separate the separation solvent and the oil component by heat treatment or the like and extract the oil component.

  The apparatus 10 includes a liquefier 60 and a reintroduction pipe 46 that is connected to the container 20 and the storage tank 30 and reintroduces the dimethyl ether that has been changed from a gas state into a liquid state into the container 20 and / or the storage tank 30. It is out. The reintroduction pipe 46 may be a pipe for reintroducing liquid dimethyl ether (oil component, dimethyl ether containing water) directly into the storage tank 30 without using the liquefier 60.

  The apparatus 10 may further include components (not shown) such as piping and valves other than the components described with reference to FIG. 1 on the condition that the object of the present invention is not impaired. For example, the container 20 includes a pipe for introducing the material, a pipe for flowing dimethyl ether to the material when the step (A) is a flow type, a valve for controlling these flow rates, a pump, a heat exchanger, You may further provide the control apparatus etc. for controlling the operation | movement of each component contained in a compressor and the apparatus 10. FIG.

  The container 20, the storage tank 30, the pipe 40 including the introduction pipe 42, the lead-out pipe 44, the re-lead pipe 46, and the separation pipe 48, the valve 50, the liquefier 60, and any other suitable configurations not shown are The liquid state dimethyl ether can be used.

  Conventionally, the shape, size, capacity, flow rate, material (material), etc. of the container 20, the storage tank 30, the pipe 40, the valve 50, the liquefier 60, the separation tank 70, etc. can be adapted to the assumed implementation scale. Any known suitable structure can be employed.

  Hereinafter, the present invention will be described more specifically with reference to examples. The present invention is not limited to the following examples.

<Example 1>
In this example, an algae concentrate of Euglena (Euglena Gracilis Z strain) was used as a material.

(Preparation of algae concentrate)
Euglena was cultured according to the method described in the appendix of “Euglena Physiology and Biochemistry”, Academic Publishing Center (1989). Euglena was cultured outdoors by sunlight for 7 days using a Cramer-Myers medium using a pool with an area of 1.2 m ² . Thereafter, an anaerobic treatment was carried out for a whole day according to the description on page 114 of the same book, and this was further centrifuged at 3000 G for 30 minutes to remove only the liquid layer substantially free of Euglena to obtain a concentrated solution. By repeating the same operation, 15 L of the anaerobic concentrated solution was collected (hereinafter, the obtained concentrated solution is referred to as an algal concentrate).

The water content of the algae concentrate used in this example was 91.4% by mass as an average value when measured three times.
The water content was measured by subjecting the algae concentrate to a vacuum drying treatment. This vacuum drying treatment was performed at a drying temperature of 35 ° C. and a drying time of 7 hours. The results are shown in Table 1 below.

(Treatment of algae concentrate with DME)
Algae concentrates containing three amounts of Euglena corresponding to (1) 1.0 g, (2) 0.5 g, and (3) 0.25 g in terms of absolute dry algae weight were poured into a pressure vessel. Distilled water was added to the pressure vessel, and the water content of the algal concentrate was adjusted to 95% by mass.

  Next, DME in a liquid state was supplied while the inside of the pressure vessel was kept airtight, and the algae concentrate and DME were brought into contact with each other. The amount of DME in the liquid state is such that the value of “DME weight / absolute dry weight”, which is a ratio of the weight of DME (DME weight) to the weight of the completely dried Euglena (absolute dry weight), is (1) 40 2) 80 and (3) 160. Note that when the DME in the liquid state is supplied, the pressure in the pressure vessel rises and enters a pressurized state.

  Next, the pressure vessel was stirred by overturning with a stirrer to mix the algae concentrate and DME. Inversion stirring was carried out for 30 minutes at a rotation speed of 50 rpm.

  Next, the pressure vessel is fixed at a normal position, and the airtight state of the pressure vessel is released and the pressure in the pressure vessel is reduced to change the liquid state DME into a gaseous state, and the gaseous state DME is led out of the pressure vessel. . At this time, the pressure in the pressure vessel becomes atmospheric pressure.

(Treatment with separation solvent)
The algae concentrate that had been treated with DME was poured into a separatory funnel having a capacity of 100 mL. Next, after adding 40 mL of hexane as a separation solvent to the separatory funnel, a process of overturning stirring using a stirrer was performed three times.
Next, after leaving the separating funnel for 3 minutes to separate the mixture, the lower layer (aqueous layer) is collected in a beaker, and the upper layer (organic layer) is collected in an eggplant-shaped flask to contain an oil component. A separation solvent was obtained selectively.

  Further, the aqueous layer collected in the beaker is added to the separatory funnel, 40 mL of hexane is added to the separatory funnel as a separation solvent, and the mixture and the separatory funnel are left to stand for 3 minutes by using a stirrer and stirring. After separation, the lower layer was collected in a beaker, and the upper layer was collected in an eggplant-shaped flask, and the process of selectively obtaining a separation solvent containing an oily component was repeated three times.

  The separation solvent containing the oily component collected in the eggplant-shaped flask was dried under reduced pressure using an evaporator at a temperature of 40 ° C. with a pressure of −0.1 MPa, then the temperature was set to 50 ° C. and the pressure was set to −0.1 MPa for 5 hours. The extraction process which extracts an oily component from a isolation | separation solvent was performed by vacuum-drying.

(Recovery rate)
From the change in the weight of the eggplant type flask containing the organic layer before and after the extraction treatment, the recovery rate of the extracted (recovered) oily component was calculated by the following formula.
Formula: Recovery rate (%) = weight of extracted oily component (g) / absolute dry weight (g)
The results are shown in Table 2 below.

  As is apparent from Table 2, when the value of “DME weight / absolute dry weight” is (1) 40, the recovery rate exceeds 10%, and (2) when it is 80, 15%. In the case of (3) 160, it was close to 20%.

<Comparative Example 1>
(Preparation of algae concentrate and treatment of algae concentrate with DME)
The process for preparing the algae concentrate and the process for treating the algae concentrate with DME were carried out in the same manner as in Example 1 described above.

(Centrifugation)
The total amount of the algae concentrate that had been treated with DME was transferred to a centrifuge tube and centrifuged at 2800 G for 60 minutes to separate it into a liquid layer containing an oil component and a solid containing algae and water.

(Treatment with separation solvent)
Only the liquid layer was separated and poured into a separating funnel having a capacity of 100 mL. Next, 40 mL of hexane was added to the separatory funnel as a separation solvent, and the process of overturning stirring using a stirrer was repeated three times.

  Next, after leaving the separating funnel for 3 minutes to separate the mixture, the lower layer (aqueous layer) is collected in a beaker, and the upper layer (organic layer) is collected in an eggplant-shaped flask to contain an oil component. A separation solvent was obtained selectively. Further, the aqueous layer collected in the beaker is added to the separatory funnel, 40 mL of hexane is added to the separatory funnel as a separation solvent, and the mixture and the separatory funnel are left to stand for 3 minutes by using a stirrer and stirring. After separation, the lower layer was collected in a beaker, and the upper layer was collected in an eggplant-shaped flask, and the process of selectively obtaining a separation solvent containing an oily component was repeated three times.

  The separation solvent containing the oily component collected in the eggplant-shaped flask was dried under reduced pressure using an evaporator at a temperature of 40 ° C. with a pressure of −0.1 MPa, then the temperature was set to 50 ° C. and the pressure was set to −0.1 MPa for 5 hours. The extraction process which extracts an oily component from a isolation | separation solvent was performed by vacuum-drying.

(Recovery rate)
The recovery rate was calculated in the same manner as in Example 1 already described. The results are shown in Table 3.

  As is apparent from Tables 2 and 3, according to the method for extracting oily components of the present invention, an oily component equal to or more than that in Comparative Example 1 in which the centrifugation step was performed could be obtained. That is, according to the extraction method of the present invention, the oil component can be efficiently obtained in a simpler process without performing a complicated process such as a centrifugal separation process.

<Comparative example 2>
(Preparation of algae concentrate)
An algae concentrate containing Euglena equivalent to 1.0 g in absolute dry algae weight was weighed and poured into a separatory funnel having a capacity of 100 mL. Distilled water was further added to the algae concentrate in the separating funnel to adjust the water content of the algae concentrate to 95% by mass.

(Treatment with separation solvent)
The process of adding 40 mL of hexane as a separation solvent to the extracted algae concentrate in the separatory funnel and stirring by overturning using a stirrer was repeated three times.

  Next, after leaving the separating funnel for 3 minutes to separate the mixture, the lower layer (aqueous layer) is collected in a beaker, and the upper layer (organic layer) is collected in an eggplant-shaped flask to contain an oil component. A separation solvent was obtained selectively. Further, the aqueous layer collected in the beaker is added to the separatory funnel, 40 mL of hexane is added to the separatory funnel as a separation solvent, and the mixture and the separatory funnel are left to stand for 3 minutes by using a stirrer and stirring. After separation, the lower layer was collected in a beaker, and the upper layer was collected in an eggplant-shaped flask, and the process of selectively obtaining a separation solvent containing an oily component was repeated three times.

  The separation solvent containing the oily component collected in the eggplant-shaped flask was dried under reduced pressure using an evaporator at a temperature of 40 ° C. with a pressure of −0.1 MPa, then the temperature was set to 50 ° C. and the pressure was set to −0.1 MPa for 5 hours. The extraction process which extracts an oily component from a isolation | separation solvent was performed by vacuum-drying.

(Recovery rate)
The recovery rate was calculated in the same manner as in Example 1 already described. The results are shown in Table 4.

  As is clear from Tables 2 and 4, according to the method for extracting an oily component of the present invention using both DME and a separation solvent, the recovery rate of the oily component is further improved as compared with Comparative Example 2 using only the separation solvent. I was able to improve.

  According to the method for extracting an oily component of the present invention, the oily component can be extracted efficiently by a simple process without performing a complicated process such as a centrifugal separation process. Further, according to the method for extracting an oily component of the present invention, since the oily component is extracted using not only dimethyl ether but also a separation solvent, the recovery rate of the oily component can be further increased.

DESCRIPTION OF SYMBOLS 10 apparatus 20 container 30 storage tank 40 piping 42 introduction piping 44 outlet piping 46 reintroduction piping 48 separation piping 50 valve 60 liquefier 70 separation tank

Claims (6)

A method for extracting an oily component from a material containing moisture and an oily component,
Step (A) A step of contacting the material with dimethyl ether in a liquid state in a container to obtain a treated product,
Step (B) removing dimethyl ether in the treated product as dimethyl ether in a gaseous state;
Step (C) adding a separation solvent (however, dimethyl ether is removed from the separation solvent) to the treated product from which dimethyl ether has been removed, and dissolving the oily component in the separation solvent;
Step (D) selectively obtaining the separation solvent in which the oil component is dissolved;
A step (E) of extracting the oily component from the separation solvent in which the oily component is dissolved. The step (A) is a step of obtaining a mixed liquid of the material and dimethyl ether in a liquid state as the treated product,
The step (B) is a step of obtaining a mixed liquid from which dimethyl ether has been removed by introducing dimethyl ether in the mixed liquid out of the container as dimethyl ether in a gaseous state,
The method for extracting an oily component according to claim 1, wherein the step (C) is a step of further adding a separation solvent to the mixed solution from which dimethyl ether has been removed and dissolving the oily component in the separation solvent.   The method for extracting an oily component according to claim 2, wherein the step (A) is a step of mixing the material and dimethyl ether in a liquid state and stirring in the container.   The step (B) collects dimethyl ether led out of the container, and supplies the recovered dimethyl ether to the mixed liquid from which dimethyl ether has been removed as liquid dimethyl ether to perform the step (A), The method for extracting an oily component according to claim 2 or 3, further comprising a step of repeating the step of obtaining the mixed solution one or more times by inducing the dimethyl ether in a gaseous state outside the container.   The method for extracting an oily component according to any one of claims 1 to 4, wherein the separation solvent is selected from the group consisting of pentane, hexane, and heptane.   The method for extracting an oily component according to claim 5, wherein the separation solvent is hexane.

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