JP2009226357A - Subcritical extraction apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a subcritical extraction apparatus which can produce an extraction solution of a high effective component concentration by carrying out batch-type subcritical extraction treatment continuously while keeping energy efficiency and work efficiency even when the separation of a residue from an extract is not easy. <P>SOLUTION: The subcritical extraction apparatus includes a plurality of batch-type extractors 10A-10D for extracting a fragment-shaped object to be treated in subcritical conditions, a filter 12 used commonly with the extractors, and a filtrate circulation line 48 which filters the extract from one extractor and supplies the obtained filtrate selectively to the other extractors as an extracting liquid. Multistage extraction treatment is carried out by the extractors 10A-10D, to increase the concentration of the extracted component of the extract. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a subcritical extraction apparatus that extracts a high-concentrated extract by treating extraction raw materials such as mushrooms and mushroom waste fungus beds under subcritical conditions.

  In recent years, the mushroom industry has been developed along with the increase in consumer demand and the improvement of cultivation technology, and many kinds of mushrooms that have never been seen have been produced in large quantities. These mushrooms are cultivated by inoculating so-called fungus bed kits with hardened oga and proper nutrition. However, the waste microbial bed discharged in large quantities is a big environmental problem. As a method of disposing of this mushroom cultivation waste fungus bed, a method of incineration disposal can be considered, but usually a large amount of water (usually 50-70% moisture) is contained in the mushroom cultivation waste fungus bed. Incineration requires a lot of energy and is not a good idea.

  Accordingly, various studies have been made to reuse the discharged fungus cultivation waste bed, and various attempts have been made. For example, Patent Document 1 proposes a method of using active ingredients such as carbohydrates, nitrogen, and minerals remaining in a mushroom cultivation waste fungus bed in order to use the mushroom cultivation waste fungus bed for re-cultivation of mushrooms. ing.

  In addition, attempts have been made to use mushroom cultivation waste fungus beds as compost. For example, Patent Document 2 proposes a production method for efficiently composting a mushroom cultivation waste fungus bed by adding oligosaccharides to the mushroom cultivation waste fungus bed to promote microbial fermentation. Alternatively, as a raw material for methane fermentation by microorganisms, attempts have been made to use it for the production of alcohol and methane gas, and further attempts have been made to use it as livestock feed.

  However, the method of using the active ingredient remaining in the mushroom cultivation waste fungus bed described in Patent Document 1 only uses the ingredients of the cultivation bed remaining in the mushroom cultivation waste fungus bed, Effective mushroom components such as glucan-derived sugar components and chitin components possessed by mushroom hyphae remaining in the floor sawdust and part of fruiting bodies are discarded without being used. Furthermore, the wood component of sawdust used in the mushroom cultivation waste fungus bed contains a large amount of cellulose, hemicellulose, lignin, etc., and is difficult to be decomposed, which hinders microbial fermentation and adversely affects the efficiency of microbial fermentation. There was a problem of giving.

  Moreover, about the manufacturing method made into compost described in the said patent document 2, the raw material of methane fermentation by microorganisms, and the feed of livestock, undegraded cellulose, hemicellulose, lignin, etc. still remain in a mushroom cultivation waste microbial bed. Since a large amount of wood components remain, it is often harmful to use microbial fermentation for composting, raw materials for various microbial fermentation, livestock feed, and the like. Furthermore, the mushroom cultivation waste fungus bed contains mushroom mycelium and mushroom scraps that are part of the fruiting body intertwined with the lump of sawdust, and the above composting process, the raw material for microbial fermentation and the feed for livestock In the process of doing this, this mushroom scrap may rot and give off a foul odor, which may lead to environmental pollution.

  Therefore, in Patent Document 3, focusing on the mushroom components remaining in the mushroom cultivation waste fungus bed, mushroom components can be efficiently extracted from a part of mushroom hyphae and fruit bodies, and malodor caused by mushroom waste There has been proposed a new hot water treatment method for mushroom cultivation waste fungus beds, which can also prevent the occurrence of water. This is a pressurized hydrothermal treatment method for a mushroom cultivation waste fungus bed characterized by extracting mushroom components by bringing pressurized hot water (subcritical water) into contact with the mushroom cultivation waste fungus bed. According to the present invention, mushroom components can be efficiently extracted from a part of mushroom hyphae and fruit bodies remaining in the mushroom cultivated waste bed, and the generation of malodor caused by mushroom waste can be prevented.

  With subcritical water, when the water temperature is 374 ° C and the pressure is 218atm (647K, 22.1MPa), the density of water and water vapor is equal and water (liquid) or water vapor (gas) cannot be distinguished. It is water at a temperature and pressure below the so-called critical point of water. Therefore, the treatment with subcritical water is carried out as a batch type treatment in which the waste microbial bed of raw material and extraction water are enclosed in an autoclave (pressure kettle) and kept in a subcritical state for a predetermined time.

  By the way, since the mushroom component in the solution obtained by extraction is finally commercialized as a solid component, it is necessary to remove moisture from the extraction solution. In order to obtain solid components by removing water from the solution, there are a distillation (fractional distillation) method in which the solution is heated to a predetermined temperature, and a method using a spray dryer that sprays the heated space. The more processing, the longer the processing time and energy, and the higher the processing cost and the lower the quality.

  Therefore, it is considered efficient to increase the concentration of the extraction solution as much as possible at the stage of the extraction process. That is, it is a method in which the same treated water is batch-treated a plurality of times for different waste bed materials. For example, Patent Document 4 proposes a batch continuous extraction apparatus that is used in an extract extraction and recovery process from coffee, tea, bonito, crude drugs, and other natural materials in the beverage / food processing industry and the Chinese medicine industry. According to this, at least three or more extraction kettles are used, and the extract is flowed in series through a plurality of extraction kettles, whereby the concentration is gradually increased to obtain a high concentration extract. Such a method is possible because the extraction residue and the extract are easily separated in the pressure cooker.

Japanese Patent No. 2638399 JP-A-11-171777 JP 2006-176765 A Japanese Patent No. 2798902

  However, in the subcritical extraction treatment of the mushroom waste fungus bed, as described above, the mushroom waste that is part of the mushroom hyphae and part of the fruit body remains intertwined with the lump of sawdust, as described above, In order to improve the extraction efficiency, this is subdivided and further extracted with stirring inside the pressure cooker. Therefore, the solid component in the extract is considerably refined and is often dispersed in the solution to form a sludge. Therefore, it is not easy to separate the residue from the extract. Therefore, it is difficult to apply the treatment method as described in Patent Document 4 to subcritical extraction of mushroom waste fungus beds.

  Therefore, even if separation of the residue from the extract is not easy, the present invention continuously performs batch-type subcritical extraction treatment while maintaining energy efficiency and work efficiency, so that an extract solution having a high active ingredient concentration is obtained. It is an object of the present invention to provide a subcritical extraction apparatus capable of producing

  The present invention has been made to solve the above-mentioned problems, and the subcritical extraction device according to claim 1 is a plurality of batch-type extractions for performing extraction processing of a strip-like workpiece under subcritical conditions. , A filter shared by the plurality of extractors, and a filtrate circulation line that selectively supplies the filtrate obtained by filtering the extract from one extractor to the other extractors as the extract liquid And a plurality of extraction processes are performed by the plurality of extractors to sequentially increase the concentration of extracted components in the extract.

  In the first aspect of the invention, the filtrate obtained by filtering the extract from one extractor is selectively supplied as the extract liquid to the other extractor via the filtrate circulation line. Even if it is not easy to separate the residue from the extract, it is possible to cause a plurality of batch type extractors to perform a multistage continuous extraction process by installing a small number of filters. As a result, it is possible to produce an extraction solution having a high active ingredient concentration at low equipment cost without installing a filter for each extractor, and the temperature of the filter can be maintained by improving the operating efficiency of the filter. The energy for reheating the filtrate can be reduced.

  According to a second aspect of the present invention, there is provided the subcritical extraction apparatus according to the first aspect of the invention, wherein the filter pressurizes and filters the extract. Thereby, since the processing time of a filter reduces, many extractors can be made to respond | correspond to one filter.

  According to a third aspect of the present invention, there is provided the subcritical extraction apparatus according to the first or second aspect of the present invention, wherein a storage tank for temporarily storing the liquid is provided at a front stage or a rear stage of the filter. Thereby, since these storage tanks act as a buffer, it is possible to reduce downtime due to timing shift.

  According to the first to third aspects of the invention, even if it is not easy to separate the residue from the extract, batch-type subcritical extraction is continuously performed by installing a small number of filters. Thus, it is possible to provide a subcritical extraction apparatus that produces an extraction solution having a high active ingredient concentration. Therefore, it is possible to reduce energy and labor when purifying the active ingredient in the subsequent process, and to greatly reduce the overall cost.

Hereinafter, a subcritical extraction apparatus according to an embodiment of the present invention will be described with reference to the drawings.
FIG. 1 shows the overall configuration of a subcritical extraction apparatus for waste mushroom bed processing according to an embodiment of the present invention. Four batch type extractors (autoclaves) 10A to 10D and, as will be described later, It is mainly comprised by the one pressurization type filter (filter press) 12 shared by these extractors 10A-10D.

  Each of the extractors 10A to 10D has a known structure in which a heat or cooling jacket 14 is provided in a sealable pressure vessel, and a raw material inlet 16 is provided in an upper portion so as to be openable and closable, and an extract liquid is provided in a lower portion. A discharge port 18 for discharging is provided. In addition, a stirrer 20 for improving the processing efficiency is provided inside the container. A steam supply line 22 for heating having a once-through boiler 21 and a cooling water supply line 24 for cooling are connected to the jacket 14, and supply or discharge of these can be controlled by on-off valves 26 and 27. .

  New liquid supply lines 30 extending from a supply source (not shown) via a preheating heat exchanger 28 are connected to the upper portions of the extractors 10A to 10D via open / close valves 32, respectively. The liquid is appropriately supplied as an extraction liquid. The discharge ports 18 of the respective extractors 10A to 10D are connected to a discharge line 34 provided in common, and the discharge line 34 is connected to an extract storage tank 36 that temporarily stores the extract. The extract storage tank 36 is provided with an extract solution pipe 42 for sending the extract to the filter 12 by the extract pump 40. The filter 12 uses a so-called filter press that can perform solid-liquid separation relatively quickly by pressurizing the liquid to be treated and forcibly passing the filter, and the separated solid matter (residue ) And a storage container 46 are provided.

  Between the filter 12 and each of the extractors 10A to 10D, there is a filtrate circulation line 48 that selectively supplies the filtrate obtained by solid-liquid separation in the filter 12 as an extraction liquid to each of the extractors 10A to 10D. Is provided. In the filtrate circulation line 48, a filtrate storage tank 50 for temporarily storing the filtrate, a filtrate pump 52, a heat exchanger 54 for reheating the filtrate, and supply to each of the extractors 10A to 10D are selectively controlled. An opening / closing valve 56 is provided. Further, the filtrate circulation line 48 is provided with a recovery line 58 for sending the filtrate obtained by filtering the extracted liquid after the final stage processing to, for example, a recovery tank (not shown).

  The operations of the extractors 10A to 10D, the filter 12 and the heat exchanger 54 and other associated devices shown in this figure are automatically controlled using known sensing or computer technology as necessary. . In addition, the flow of the extraction liquid, the extraction liquid, the filtrate, or the fluid such as steam or cooling water can be controlled by various valves provided in these lines, and these valves can be operated manually or Automatic operation by a computer or the like is possible.

  In the following, the processing steps by the subcritical extraction apparatus configured as described above will be described with reference to FIGS. 2 and 3 in addition to FIG. 2 shows a simplified flow of the extraction liquid (new liquid supply line 30), the extraction liquid (discharge line 34), and the filtrate (filtrate circulation line 48) in the apparatus of FIG. The on-off valve and other details are omitted. FIG. 3 shows the operation schedule of each of the extractors 10 </ b> A to 10 </ b> D and the filter 12 very schematically, and corresponding steps are shown in the drawing in the following description.

  Moreover, in the following embodiment, the order of processing of each of the extractors 10A to 10D is determined in advance, but of course is not limited to this. In the embodiment, four extraction processes are performed by the four extractors 10 </ b> A to 10 </ b> D (A → B → C → D), but an arbitrary number of processes of five or more stages can be performed. In addition, it is assumed that the efficiency of the extraction process at each stage decreases as it goes to the subsequent stage. Here, the same processing time is set in each case.

  First, an extraction liquid (warm water) is press-fitted into the extractor 10A from the new liquid supply line 30 (1), and a strip-shaped raw material is charged from the inlet 16 from a raw material supply device (not shown). The steam generated in the once-through boiler 21 is supplied from the steam supply line 22 to the jacket 14, and the temperatures of the extractors 10 </ b> A to 10 </ b> D are gradually increased, and the predetermined time is maintained under a predetermined subcritical condition (120 ° C. to 220 ° C.). An extraction process is performed (2).

  Next, steam is discharged from the jacket 14 and cooling water is injected into the jacket 14 from the cooling water supply line 24 to lower the temperature of the extract. After the inside of the container of the extractor 10A reaches a predetermined temperature, the lower extract outlet 18 is opened, the extract is sent to the discharge line 34, further sent from the extract reservoir 36 to the filter 12, and filtered (3 ). The separated residue is stored in a container by a belt conveyor. On the other hand, after the filtrate is stored in the filtrate storage tank 50, the filtrate pump 52 is operated at a predetermined timing, reheated by the heat exchanger 54, and supplied to the extractor 10B from the filtrate circulation line 48 (4). The shortage corresponding to the residue and evaporation is supplied from the new liquid supply line 30. Then, extraction processing and subsequent filtration and circulation steps are performed in the same manner as in the case of the extractor 10A. The same process is performed by the extractor 10C and the extractor 10D, and the filtrate in the final stage is recovered from the recovery line (L). On the other hand, the extractor 10A, after performing operations such as internal cleaning, is charged again with a new raw material and a new extraction liquid (1 ′), and performs the first stage extraction process of a new cycle ( 2 ′), the above steps are sequentially repeated.

  In this embodiment, a four-stage extraction process is repeated to recover a solution having a more concentrated extraction component. When a thin solution component is solidified, for example, by distillation, energy is required to evaporate a large amount of water, so processing a concentrated solution saves a lot of energy and labor. Needless to say.

  In order to filter the extract which is difficult to separate into solid and liquid as in the case of the waste bacteria bed, the pressure type filter 12 is used, but the processing time for one time is compared with the processing time of the extractors 10A to 10D. Since the extractors 10A to 10D are processed once and cleaned once, the filter 12 performs the process 5 times without any problem because it is much shorter. If a failure occurs in any of the processes, there is a possibility that the timing will be shifted and there will be a situation where the processing of the filter 12 must be waited. Further, the extract storage tank 36 or the filtrate storage tank 50 can serve as a buffer that absorbs a slight shift in timing.

  Thus, by setting the number of the filter 12 according to the processing time of the filter 12 and the extractors 10A to 10D, the filter 12 can be used more than when the filter 12 is provided for each of the extractors 10A to 10D. The number of installations can be reduced, the equipment cost can be reduced, and the operating efficiency of the filter 12 is improved, so that the temperature of the filter 12 is prevented from lowering, and the temperature of the extract liquid when passing through the filter 12 is prevented. Can be removed. Therefore, the amount of heating by the heat exchanger for reheating in the filtrate circulation line 48 can be reduced, which is advantageous in terms of energy efficiency.

(Example)
Experiments were conducted using small extractors 10A to 10D in order to confirm a decrease in the extraction amount per raw material when extraction processing was performed by circulating the extract.
As the extractors 10A to 10D, a 500 cc stirring autoclave was used, and the waste maitake mushroom bed was crushed to about 2 mm and stirred as a material to be treated, and 300 cc, 91.7 g was used as a batch. Using. In the first stage treatment, 252.9 g of ion-exchanged water was used as the extraction liquid, and the total amount of the second and subsequent stages was the same as that of the previous stage filtrate. Since the filter 12 is experimental equipment, the Nuccie type was used.

The extraction process at each stage is performed after charging the raw materials and the extraction liquid, raising the autoclave to 150 degrees in about 1 hour with stirring, holding it at 150 degrees for 1 hour, and then cooling to 80 degrees or less. At that time, the autoclave lid was opened and filtered with a filter 12. A part of the filtrate was collected, and the amount of extract contained in the test sample was measured. The results are shown below.
Extract concentration from the first stage extractor 3.0wt%
Concentration of extract from the second stage extractor 5.5 wt%
Extract concentration from the third stage extractor 7.9wt%
Extract concentration from the 4th stage extractor 10.0wt%

  As a result, the extraction efficiency of the subsequent processing is slightly reduced, but a large amount of raw material exists at a low cost, so that a slight decrease in the recovery rate does not cause a problem. According to this, when the drying process is completed after the first stage, 97 wt% of water is removed to obtain 3 wt% of mushroom components, whereas when the process up to the fourth stage is performed, 90 wt% of water is obtained. 10% by weight of mushroom components can be obtained by removing water.

It is a figure which shows the whole structure of the subcritical extraction apparatus of embodiment of this invention. It is a figure which simplifies and shows the flow of the extract of the subcritical extraction apparatus of FIG. It is a figure which shows the timing of operation | movement of each apparatus at the time of operation of the apparatus of FIG.

Explanation of symbols

10A to 10D Extractor 12 Filter 30 New liquid supply line 34 Discharge line 36 Extract liquid storage tank 48 Filtrate circulation line 50 Filtrate storage tank 54 Heat exchanger

Claims (3)

  It is obtained by filtering a plurality of batch type extractors that perform extraction processing of a strip-like workpiece under subcritical conditions, a filter shared by the plurality of extractors, and an extract from one extractor. A filtrate circulation line for selectively supplying the obtained filtrate to another extractor as an extraction liquid, and performing a multi-stage extraction process with the plurality of extractors so as to sequentially increase the concentration of the extracted components in the extract. A subcritical extraction device characterized in that   The subcritical extraction apparatus according to claim 1, wherein the filter pressurizes and filters the extract.   The subcritical extraction device according to claim 1 or 2, wherein a storage tank for temporarily storing the liquid is provided in a front stage or a rear stage of the filter.

Images