Method and apparatus for producing useful substances

Abstract

To provide a method and an apparatus for producing useful substances for producing two or more useful substances using wood as a raw material.SOLUTION: A method and an apparatus for producing useful substances comprises: a raw material introduction step of introducing wood chips into a processing space S1 of a closed container 12; a first subcritical water treatment step of introducing steam at 4-15 atm at 120-200°C to subcritical water reaction treat raw materials, and obtaining a first mixed solution containing fulvic acid, humic acid, wood chips and / or solids thereof; an intermediate pressure reduction step of discharging high-pressure steam from the processing space to reduce pressure; a liquid recovery step of recovering only liquid that will be the raw material of fulvic acid / humic acid from the processing space; a second subcritical water treatment step of introducing steam at 15-30 atm at 200-250°C to obtain a second mixed solution containing a carbonized solid formed by carbonizing the raw material by a subcritical water reaction and pyroligneous acid produced along with carbonization; a liquid recovery step of recovering only the raw material liquid of pyroligneous acid from the processing space; and a solid carbide recovery step.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present invention relates to a method and an apparatus for producing useful substances, and more particularly to a method and an apparatus for producing useful substances, particularly fulvic acid / humic acid and wood acetic acid, using wood as a raw material. [Background technology]

[0002] Humic substances such as fulvic acid and humic acid are said to be a general term for "organic matter with an unspecified chemical structure (non-living organic matter)" that is broken down by microbial and chemical action after the death of an organism. It is empirically known that some humic substances are functional and some are not, and this is thought to be largely influenced by whether or not they contain intermediate products that are produced when the organic matter of living organisms, which is organic matter in the natural world, returns to the soil. Humic substances that contain these intermediate products, i.e. that are functional, are sometimes called humus precursors. (Non-Patent Document 1)

[0003] Substances equivalent to this humus (or humus precursors) exist in nature, and even if it is unclear whether humus has been recognized since ancient times, it has been used in various ways for its effects on crop growth and medicinal properties against illness and injury. Meanwhile, in recent years, modern agriculture and raw material processing methods that actively utilize developed chemical substances have been widely used. However, apart from such modern agriculture and raw material processing, the use of this humus, which has been utilized since ancient times, is beginning to be reconsidered, and some solutions containing artificially produced fulvic acid at selectively high concentrations are being sold.

[0004] For example, Patent Document 1 is a technology relating to a wastewater treatment method that utilizes a bacterial group consisting of soil-dwelling facultative anaerobic bacteria that have been cultivated to produce metabolic products containing phenol and / or compounds with phenol exposure groups. This "metabolic product containing phenol and / or compounds with phenol exposure groups" induces a polycondensation reaction for humification by reacting with silicic acid and the like, and the technology aims to disclose an excellent wastewater treatment method that utilizes humic plants.

[0005] As seen in Patent Document 1 and Non-Patent Document 1, technologies that utilize humus precursors and humic substances (humic plants) are being studied. Here, it is known that humic plants contain humin, fulvic acid, humic acid, etc., as the degree of humification (degree of polycondensation reaction) of their components. In general humic substances, the ratio of fulvic acid to humic acid is about 2:8 by weight.

[0006] As shown in Patent Document 1, there are some processes for treating wastewater containing organic substances that use substances equivalent to this humic substance, but the fulvic acid and humic acid in humic substances are not simple substances, and are considered to be groups of multiple organic compounds, and because they are difficult to separate, the specific effects of each substance have not been fully studied. However, commercially available solutions containing fulvic acid are expected to be effective as (micro)biologically active liquids, and products that selectively contain fulvic acid at high concentrations are required for use in applications such as agriculture, where the provision of products as cheap as possible in large quantities is required.

[0007] Therefore, in JP 2017-112947 A (Patent Document 2), with regard to fulvic acid, which is a humic substance that is expected to be used as a (micro)biologically active liquid, the following manufacturing method was proposed for the purpose of providing a method for manufacturing a high-ratio fulvic acid-containing liquid that contains a high ratio of fulvic acid to humic acid compared to the ratio of general humic substances.

[0008] The method for producing a fulvic acid-containing liquid proposed in the above Patent Document 2 is characterized by an anaerobic culture step in which an organic substance mixed liquid obtained by mixing organic substances and fulvic acid-acclimated sludge is cultured for 4 hours or more at a dissolved oxygen concentration of 0.1 mg-O / L or less to reduce the organic substances in the organic substance mixed liquid by anaerobic culture to obtain an anaerobic culture liquid; an aerobic culture step in which the anaerobic culture liquid is cultured for 6 hours or more at a dissolved oxygen concentration of 0.2 mg-O / L or more to increase the fulvic acid in the anaerobic culture liquid to obtain a fulvic acid-containing culture liquid; an aerobic culture liquid return step in which the culture liquid cultured in the aerobic culture step before the completion of the culture is returned to the anaerobic culture step; and a fulvic acid-containing liquid is obtained from the fulvic acid-containing culture liquid obtained from the aerobic culture step.

[0009] The applicant of the present invention previously proposed in Japanese Patent No. 6286605 a method for producing a fulvic acid solution that is completely different from those described in the above-mentioned publications.

[0010] The method for producing fulvic acid proposed in this patent publication is as follows: an apparatus preparation step of preparing a treatment apparatus including a sealed container having a closable treatment space therein, steam ejection means for ejecting high-temperature and high-pressure steam into the sealed container, a supply section having an opening / closing mechanism for supplying raw material into the sealed container, and a discharge section having an opening / closing mechanism for discharging a treatment liquid produced by the treatment of the raw material with the steam to the outside; a raw material input step of inputting a raw material containing wood chips as a main raw material from the supply unit into a treatment space of the sealed container of the treatment device; a processing step of subjecting the raw material to a subcritical water reaction processing while introducing steam having a temperature of 120 to 250°C and a pressure of 12 to 35 atm into the processing space containing the raw material and stirring the raw material to obtain a mixed solution containing fulvic acid, humic acid, and a suspension of wood chips and / or fragments thereof; A fulvic acid solution obtaining process for obtaining a fulvic acid solution by separating fulvic acid from the obtained mixed solution. The present invention relates to a method for producing a fulvic acid solution, the method comprising the steps of: [Prior art documents] [Patent documents]

[0011] [Patent Document 1] Special Publication No. 5-66199

[0012] [Patent Document 2] JP 2017-112947 A

[0013] [Patent Document 3] Patent No. 6286605 [Non-patent literature]

[0014] [Non-Patent Document 1] Mamoru Uchimizu, "Nature and Reincarnation: Earth, Nature, Humans, and Society: Basic Civilization Theory," pp. 18-28, Mangasha, 1986 Summary of the Invention [Problem to be solved by the invention]

[0015] According to the method for producing fulvic acid described in the above patent publication, it is possible to efficiently produce fulvic acid with high purity. However, wood contains a number of other useful substances (including useful substances derived from wood), and in the past, the solid matter obtained after fulvic acid extraction was not effectively utilized except for being used as animal feed.

[0016] Therefore, an object of the present invention is to provide a method and apparatus for producing two or more useful substances using wood as a raw material. [Means for solving the problem]

[0017] The above object can be achieved by the method and apparatus for producing a useful substance according to the present invention having the following configurations (1) to (18). (1) A method for producing useful substances by treating wood chips as a raw material to produce at least two or more useful substances, comprising the steps of: an apparatus preparation step of preparing a treatment apparatus including a sealed container having a closable treatment space therein, a supply unit for supplying raw material into the sealed container, a steam ejection means for ejecting high-temperature, high-pressure steam into the sealed container, an outlet unit having an open / close valve for ejecting only liquid from the sealed container and an open / close mechanism for ejecting solid matter, and a steam outlet having a steam exhaust valve for ejecting high-pressure steam from the sealed container; a raw material input step of inputting a raw material containing wood chips as a main raw material from the supply unit into a treatment space of the sealed container of the treatment device; a first subcritical water treatment step in which the raw material is subjected to a subcritical water reaction treatment while introducing steam having a temperature of 120 to 200°C and a pressure of 4 to 15 atm into the treatment space into which the raw material has been charged, and stirring the raw material to obtain a first mixed solution containing fulvic acid, humic acid, and solid matter of wood chips and / or fragments thereof; an intermediate pressure reduction step of opening the steam exhaust valve to exhaust high-pressure steam from the treatment space to reduce the pressure in the treatment space from high pressure; A first liquid recovery process in which the on-off valve is opened to recover only the liquid that is the raw material for fulvic acid / humic acid from the treatment space; a closing step of closing the steam exhaust valve and the on-off valve; a second subcritical water treatment step in which the raw material is carbonized by a subcritical water reaction while stirring the raw material and introducing steam having a temperature of 200 to 250°C and a pressure of 15 to 30 atm into the treatment space in which the solid is present, to obtain a second mixed solution containing a carbonized solid formed by the carbonization and wood acetic acid produced by the carbonization; a final depressurization step of opening the steam exhaust valve to exhaust high pressure steam from the treatment space to reduce the pressure in the treatment space from high pressure to atmospheric pressure; a second liquid recovery step of opening the on-off valve to recover only the liquid serving as a raw material for wood acetic acid from the treatment space; and a solid recovery step of opening the opening / closing mechanism and recovering solid carbide from the treatment space; A method for producing a useful substance, comprising: (2) The method for producing a useful substance according to (1) above, wherein in the first subcritical water treatment step, the maximum temperature is held for 15 to 20 minutes. (3) The method for producing a useful substance according to (1) or (2) above, wherein in the second subcritical water treatment step, the maximum temperature is held for 15 to 20 minutes. (4) The method for producing a useful substance according to (1) above, wherein the wood is felled wood or waste wood. (5) The method for producing a useful substance according to (4) above, wherein the felled wood is from broadleaf or coniferous trees. (6) The method for producing a useful substance according to (5) above, wherein the broad-leaved tree is birch, willow, chestnut, oak or beech. (7) The method for producing a useful substance according to (5) above, wherein the coniferous tree is pine, cedar, cypress or Asunaro. (8) The method for producing a useful substance according to (4) above, wherein the waste material is solid wood or plywood. (9) The method for producing a useful substance according to any one of (1) to (8), wherein the treatment step is carried out for 1 to 8 hours. (10) The method for producing a useful substance according to (5) above, wherein the main raw material is broad-leaved wood, and the pressure of the steam introduced in the treatment step is 12 to 25 atm. (11) The method for producing a useful substance according to (5) above, wherein the main raw material is coniferous wood, and the pressure of the steam introduced in the treatment step is 20 to 35 atm. (12) The method for producing a useful substance according to any one of (1) to (11), wherein the raw material is introduced into the treatment space in a volumetric ratio of 90% or less. (13) The method for producing a useful substance according to any one of (1) to (11), wherein the raw material is introduced into the treatment space in an amount of 50 to 80% by volume. (14) The method for producing a useful substance according to any one of (1) to (13), wherein the stirring in the treatment step is performed by a rotating stirring member disposed within the treatment space. (15) The method for producing a useful substance according to any one of (1) to (14), wherein an alkaline solution is added as an additive in the raw material charging step. (16) A method for producing a useful substance according to any one of (1) to (15) above, which comprises, as a raw material, leaves of a woody plant. (17) The method for producing a useful substance according to any one of (1) to (16), wherein the treatment device is provided with a condensation means connected to the steam exhaust port, and volatile organic compounds derived from wood are condensed and recovered from the high-pressure steam ejected from the steam exhaust port by the condensation means. (18) An apparatus for producing useful substances that processes wood chips as raw material to produce at least two or more useful substances, the apparatus comprising: a sealed container having a closable processing space therein; a supply section for supplying raw material into the sealed container; steam ejection means for ejecting high-temperature, high-pressure steam into the sealed container; an outlet section having an opening / closing valve for ejecting only liquid from within the sealed container and an opening / closing mechanism for ejecting solids; a steam exhaust port having a steam exhaust valve for ejecting high-pressure steam from the sealed container; and condensation means connected to the steam exhaust port for condensing and recovering volatile organic compounds derived from wood from the high-pressure steam ejected from the steam exhaust port. Effect of the Invention

[0018] As described above, according to the present invention, at least two useful substances can be produced in a series of steps using mainly wood chips as raw materials, which has the advantage of being extremely efficient and economical. Furthermore, according to the present invention, it is possible to obtain a fulvic acid solution with high purity. [Brief description of the drawings]

[0019] [Figure 1] 1 is a cross-sectional view showing an example of an apparatus for producing a useful substance according to an embodiment of the present invention. [Diagram 2] 1 shows the transition of the treatment pressure and the treatment temperature in the treatment step in the method for producing a useful substance of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0020] An apparatus 10 for producing a useful substance according to an embodiment of the present invention will now be described. The manufacturing apparatus 10 includes a sealed container 12 having a closed space S1 as a processing space for accommodating wood chips as raw material, a steam ejection means 14 for ejecting high-temperature, high-pressure steam as subcritical water into the sealed container 12, an outlet 16 provided on the bottom side of the sealed container 12 and having an opening / closing mechanism 26, and a separation and recovery means 18 for separating and recovering the processed raw material and liquid only by direct discharge from the outlet 16. The shape of the sealed container 12 may be, for example, a rectangular box shape, a three-dimensional polygonal tube shape, a cylindrical shape, a barrel shape, a drum shape, or any other shape, but a shape that allows the material to be discharged by utilizing gravity from the outlet 16 provided on the bottom side is preferable. It is preferable that the bottom of the sealed container is provided with a downward slope toward the outlet.

[0021] The separation and recovery means 18 may have a liquid recovery section 50 communicating with the inside of the sealed container 12 via the discharge port 16, and a gravity flow recovery mechanism 52 for recovering only the liquid in the sealed container 12 to the recovery section 50 by gravity flow via the discharge port 16. The raw material as a solid content processed near the discharge port 16 remains in the sealed container 12 as it is, and only the liquid flows naturally downward to the recovery section 50 by utilizing gravity, so that the raw material and the liquid can be separated and recovered. The recovery section 50 may be configured in any manner as long as it has a closed space S2 for recovering the liquid, such as a metal tank, a box body having a three-dimensional polygonal shape, or a tubular body. A plurality of storage sections may be formed.

[0022] In the above example, the separation means is incorporated in the processing apparatus. However, the processing apparatus itself does not need to be provided with the separation means, and the separation means may be provided separately. In addition, the gravity flow recovery mechanism 52 includes a liquid recovery flow path 54 that connects the discharge outlet 16 of the sealed container 12 to the recovery section 50, and the liquid recovery flow path 54 may be arranged horizontally or downwardly sloping from the side communicating with the discharge outlet 16 toward the recovery section 50.

[0023] An opening / closing mechanism 26 is provided midway along a discharge path R1 from the discharge port 16 for the treated raw material, and a liquid inlet 58 of a liquid recovery passage 54 is connected in communication with the opening / closing mechanism 26 upstream of the discharge path.

[0024] In addition, the liquid recovery flow path 54 is provided with an opening / closing valve 60 that selectively switches the connection state to block the flow path while the raw material is being processed in the sealed container 12 and to open the flow path when only the liquid is being recovered after processing.

[0025] The bottom surface of the closed space S2 of the recovery section 50 may be set lower than the position of the discharge port 16 of the sealed container 12.

[0026] The sealed container 12 is preferably formed in a sideways barrel shape with a discharge outlet 16 provided at the bottom of the left-right center and a diameter gradually decreasing from the left-right center toward both left and right ends, and a stirring member 30 is provided inside the sealed container 12. The stirring means 30 is provided laterally coaxially with the horizontal center axis of the sealed container 12 and has a rotating shaft 49 rotatably supported at both ends, and a stirring blade 48 attached to the rotating shaft 49 and extending in the circumferential direction of the rotating shaft 49, and the length from the rotating shaft 49 to the blade tip of the stirring blade 48 is preferably formed so as to be large at the center position in the longitudinal direction of the rotating shaft 49 and gradually decrease toward both ends, in accordance with the sideways barrel shape of the sealed container 12, as shown in the figure.

[0027] In addition, the steam ejection means 14 may include a rotating shaft / steam ejection pipe 28 configured by forming a rotating shaft 49 as a hollow tube and forming a plurality of steam ejection holes 44 on the circumferential surface of the hollow tube.

[0028] Although not shown, it is preferable that the sealed container 12 is supported by support legs so that it is placed at a certain height from the ground. The sealed container 12 is formed, for example, by processing a metal plate so as to have heat and pressure resistance, and the closed space inside is about 2 m 3It is preferable that the container is provided with a size of 100 mm or more. The sealed container 12 has an inlet 20 at the top center and an outlet 22 at the bottom center, and opening / closing mechanisms 24, 26 are provided to open and close the inlet and outlet. The sealed container 12 is provided with a safety valve (not shown), for example, a pressure-adjustable safety valve, which releases internal steam when the internal pressure exceeds a set value. A sound-absorbing and deodorizing device is provided in the middle of the exhaust pipe connected to the safety valve, and the steam exhausted through the safety valve is deodorized and deodorized before being exhausted to the outside air.

[0029] The diameter of the discharge outlet 16 is set to, for example, about 300 mm. A discharge tube 36 protruding downward is connected to the discharge outlet 16 to form the discharge path R1 for the treated raw material. The opening / closing mechanism 26 for opening and closing the discharge outlet 16 is provided in the middle of the discharge path R1 of the discharge tube 36. That is, the discharge section 22 includes the discharge outlet 16, the discharge tube 36, and the opening / closing mechanism 26. Since the sealed container 12 is formed in a barrel shape lying on its side, the raw material inside tends to gather from the left and right due to gravity toward the center where the discharge outlet 16 is provided, and the treated raw material can be easily discharged from the discharge outlet 16 by simply opening the opening / closing mechanism 26.

[0030] The charging section 20 has a charging port 42 opened at the center of the upper side of the sealed container 12, and a charging tube 43 protruding upward is attached to the charging port 42, and the opening and closing mechanism 24 is provided to open and close the inside of the charging tube 43. The charging port 42 can be opened via the opening and closing mechanism 24 to charge raw materials into the sealed container, and is closed during processing to maintain the closed state of the closed space S1 within the sealed container 12.

[0031] The steam ejection means 14 ejects high-temperature, high-pressure steam into the sealed container 12, and creates a high-temperature, high-pressure state inside the sealed container 12 to process the raw material using the steam. As shown in FIG. 1, the steam ejection means 14 includes a steam ejection pipe 28 arranged inside the sealed container 12 and consisting of a hollow pipe with a number of steam ejection holes 44 formed on the circumferential side, a steam generator 46 such as a boiler, and a steam delivery pipe 47 for supplying steam from the steam generator 46 into the steam ejection pipe 28. The steam generator 46 includes a steam supply control valve 46a for controlling the supply state and the supply stop state of the generated steam, and the supply of steam can be temporarily stopped by closing the steam supply control valve 46a. The steam supply control valve 46a may be provided in the steam delivery pipe 47. The steam ejected from the steam ejection means 14 into the sealed vessel 12 is set to a high temperature and high pressure that meets the conditions of subcritical water in order to properly treat the raw material. For example, the steam ejected from the steam ejection pipe 28 is set to a temperature of 120 to 250°C and a pressure of about 4 to 30 atm. The inside of the sealed vessel 12 is set to a temperature of 120 to 250°C and a pressure of about 4 to 30 atm. The steam ejection pipe 28 is arranged horizontally at a substantially central position in the vertical direction of the sealed vessel 12, and is rotatably supported by bearings 45 provided on both end walls 12a and 12b of the sealed vessel. That is, the steam ejection pipe 28 is adapted to eject steam radially while rotating around a horizontal axis and directly hit the raw material with the steam. The steam ejection pipe 28 is adapted to rotate by obtaining a rotational driving force from a rotary drive device (not shown) such as a motor via a chain 70 or the like. Furthermore, an agitating blade 48 constituting the agitating means is attached to the steam ejection pipe 28, and the steam ejection pipe 28 also serves as the rotating shaft 49 of the agitating means. That is, in this embodiment, the steam ejection means 14 includes the rotating shaft / steam ejection pipe 28 configured by making the rotating shaft 49 of the agitating means a hollow tube and forming a plurality of steam ejection holes on the circumferential surface of the hollow tube. Note that the steam ejection means is not limited to this configuration, and may have any other configuration, such as a configuration in which steam is ejected from the tip of a tube inserted into a sealed container, or a configuration in which a plurality of steam ejection pipes are arranged.

[0032] The stirring means 30 is a means for stirring the raw material to be processed in the sealed container, and can process the raw material evenly and quickly. The stirring means 30 includes a rotating shaft 49 consisting of the steam ejection pipe 28, and a stirring blade 48 attached to the rotating shaft 49 and having a portion that expands in the circumferential direction of the rotating shaft. In this embodiment, the stirring blade 48 is formed of a right-handed spiral blade 48a and a left-handed spiral blade 48b, which are wound in opposite directions and are provided at approximately the center position in the axial direction of the rotating shaft 49. As described above, the stirring blade 48 is provided so that the length from the rotating shaft to the blade tip gradually decreases from the left-right center portion toward both ends. This allows the raw material to be reliably stirred in accordance with the sideways barrel shape of the sealed container 12. Furthermore, it is provided so that a certain amount of gap H is formed between the blade tip and the inner wall of the sealed container 12. The spiral blades 48a and 48b stir the raw material while crushing the solid raw material as they transport the raw material from the center toward both end walls. The raw material conveyed to the both end walls 12a, 12b by the stirring blades 48 is pushed forward by the raw material conveyed later at the end walls 12a, 12b, and is conveyed so as to return to the center after passing through the gap H along the inner wall of the sealed container 12. The stirring means 30 is not limited to the above configuration, and may have any other configuration.

[0033] The separation and recovery means 18 is a means for separating and recovering the treated raw material and the liquid in the sealed container 12 after steam treatment, simply by direct operation from the discharge port. As shown in Fig. 1, the separation and recovery means 18 has a liquid recovery section 50 communicating with the inside of the sealed container 12 via the discharge port 16, and a gravity flow recovery mechanism 52 for recovering the liquid via the discharge port 16 into the recovery section 50 by gravity flow.

[0034] The liquid recovery flow passage 54 has its liquid inlet 58 connected to the outlet 16 to form a liquid recovery path R2 branched off from the discharge path R1 of the treated raw material. In this embodiment, the liquid recovery flow passage 54 is made of a metal tube with an inner diameter of about 6 mm, for example. As described above, the liquid recovery flow passage 54 is provided with an on-off valve 60 that selectively switches the communication state of the flow passage. The on-off valve 60 is switched to block the flow passage during the processing of the raw material in the sealed container, and to communicate the flow passage when only the liquid is separated and recovered after the processing. As a result, the liquid in a state in which the moisture and steam contained in the raw material are liquefied at the same time as the raw material and the bacteria and malodorous components in the raw material are liquefied can be treated with high-temperature and high-pressure steam. The liquid separated and recovered after the processing can be recovered in a state in which it has been sterilized and the malodorous and harmful components have been decomposed, and there is no need to perform secondary processing on the separated and recovered liquid, which saves labor and time.

[0035] A volatile useful substance recovery mechanism 30 for recovering volatile useful substances such as terpene oil is provided at the top of the sealed container 12. This volatile useful substance recovery mechanism 30 includes a high-temperature, high-pressure steam exhaust pipe 31 connected to the sealed space S1 via a high-pressure, high-temperature steam exhaust port 19 provided in the sealed container 12, a steam exhaust valve 32 provided upstream of this high-temperature, high-pressure steam exhaust pipe 31, a condensation means 34 that receives high-temperature, high-pressure steam from the steam exhaust valve 32, cools it, condenses the high-pressure, high-temperature steam, and recovers a liquid containing volatile organic compounds derived from wood, and a storage container 38 to which the liquid from the condensation means 34 is transported via a pipeline 35.

[0036] The liquid stored in the storage container 38 is a liquid containing volatile organic compounds derived from wood as described above, and if necessary, the volatile organic compounds are extracted from the liquid and made into a product.

[0037] The manufacturing apparatus 10 is composed of a central processing circuit and the like, and is equipped with a control circuit 100 that controls the operation of the opening / closing mechanism 26, the steam exhaust valve 32, the steam generator 46, the steam supply control valve 46a, the opening / closing valve 60, etc., in accordance with a predetermined program stored in advance.

[0038] Next, a method for producing a useful substance according to an embodiment of the present invention using the above-described production apparatus 10 will be described. The method for producing a useful substance according to an embodiment of the present invention includes the steps of: preparing a treatment device as described above; a raw material input step of inputting a raw material containing wood chips as a main raw material from the supply unit into a treatment space of the sealed container of the treatment device; a first subcritical water treatment step in which the raw material is subjected to a subcritical water reaction treatment while introducing steam having a temperature of 120 to 200°C and a pressure of 4 to 15 atm into the treatment space into which the raw material has been charged, and stirring the raw material to obtain a first mixed solution containing fulvic acid, humic acid, and solid matter of wood chips and / or fragments thereof; an intermediate pressure reduction step of opening the steam exhaust valve to exhaust high-pressure steam from the treatment space to reduce the pressure in the treatment space from high pressure; A liquid recovery process in which the on-off valve is opened to recover only the liquid that is the raw material for fulvic acid / humic acid from the treatment space; a closing step of closing the steam exhaust valve and the on-off valve; a second subcritical water treatment step in which the raw material is carbonized by a subcritical water reaction while stirring the raw material and introducing steam having a temperature of 200 to 250°C and a pressure of 15 to 30 atm into the treatment space in which the solid is present, to obtain a second mixed solution containing a carbonized solid formed by the carbonization and wood acetic acid produced by the carbonization; a final depressurization step of opening the steam exhaust valve to exhaust high pressure steam from the treatment space to reduce the pressure in the treatment space from high pressure to atmospheric pressure; a liquid recovery step of opening the on-off valve to recover only the liquid serving as a raw material for wood acetic acid from the treatment space; and a solid recovery step of opening the opening / closing mechanism and recovering solid carbide from the treatment space; It is equipped with: In the above, it is preferable that the raw material supplying step and subsequent steps are automatically performed by the control circuit 100 in accordance with a predetermined program.

[0039] Each of the above steps will now be described in detail. 《Equipment preparation process》 With reference to the drawing, a manufacturing apparatus (processing apparatus) as described above is prepared.

[0040] 《Raw material input process》 The main raw material is wood chips. The size of the chips is preferably about 50 to 150 cm in long side and about 5 cm in short side. As a sub-material or additive, an alkaline solution can be added to efficiently generate more fulvic acid. The steam pressure and temperature when an alkaline solution is added may be the same as when it is not added.

[0041] Generally, felled wood or waste wood can be used as the wood. The felled wood may be either broadleaf or coniferous. The broad-leaved tree may be any broad-leaved tree, but currently, for example, birch, willow, chestnut, oak, beech, etc. are preferably used. At present, for example, pine, cedar, cypress, and asparagus tree are preferably used as the coniferous tree. When using felled timber, it is not necessary to remove the bark, etc. Also, leaves, roots, and fruit shells such as coconut shells may be included as is or in chip form.

[0042] Examples of waste materials include wood waste (lumber, planks: solid wood, laminated wood, plywood (plywood)) generated during the demolition of wooden houses. Such wood waste is usually made into chips, so it can be used as it is as a raw material. The above-mentioned raw materials may be mixed for use. For example, in a normal household, when cutting down trees, various kinds of cut trees are discharged, and these may be mixed together as they are, without sorting, and made into chips to be used as raw material. Of course, waste wood chips may be mixed into them.

[0043] The raw material, which is the chips as described above, is fed into the treatment space, and the amount of the raw material is preferably 90% or less, particularly 50-80%, of the closed space S1 of the sealed container 12, i.e., the treatment space. If the amount of raw material fed is less than this range, the treatment efficiency is poor, and if it exceeds this range, the steam cannot act effectively on the raw material, and there is a risk that the production of fulvic acid will be insufficient.

[0044] <First subcritical water treatment process> In this process, the raw material is subjected to a subcritical water reaction treatment while introducing high-pressure high-temperature steam into the treatment space into which the raw material is charged, and the raw material is stirred to obtain a first mixed solution containing fulvic acid, humic acid, and solid matter of wood chips and / or fragments thereof. The steam, which varies depending on the type and state of the raw material used, is set at a temperature of 120 to 200°C and a pressure of 4 to 15 atm so that the raw material is not carbonized. Therefore, the treatment space is set at a treatment temperature and pressure of 120 to 200°C and 4 to 15 atm. The amount of steam introduced depends on the volume of the treatment space and the amount of raw material to be treated, but is preferably an amount that completely fills the surplus space (the space obtained by subtracting the volume of the raw material charged from the treatment space).

[0045] When broadleaf trees are used as the felled materials, the high-pressure, high-temperature steam supplied in the treatment step preferably has a temperature of 120 to 200° C. and a pressure of 4 to 15 atm. On the other hand, when using coniferous trees as the felled materials, the high-pressure, high-temperature steam supplied in the treatment step preferably has a temperature of 140 to 200° C. and a pressure of 5 to 15 atm. In this treatment step, as described above, while steam is introduced into the treatment space into which the raw materials have been charged, the raw materials are stirred and treated by a subcritical water reaction. The treatment time is preferably 15 to 20 minutes at the maximum temperature and maximum pressure holding time, i.e., the set treatment temperature and pressure. If the treatment time is shorter than the above range, the reaction time will be insufficient, i.e., the production of fulvic acid and humic acid will be insufficient, and a considerable amount of fulvic acid and humic acid will remain in the raw material. If the treatment time exceeds the above range, the raw material will be carbonized, and unintended substances will be mixed into the solution. In this treatment process, the raw material is treated with a subcritical water reaction, and fulvic acid and humic acid are contained in a solution. This solution also contains a suspension of wood chips and / or its fragments. That is, a mixed solution containing fulvic acid, humic acid, and a suspension of wood chips and / or its fragments is obtained. In the mixed solution obtained in this process, fulvic acid accounts for 3 to 12% of the total amount (of the solid content) of fulvic acid and humic acid.

[0046] <<Intermediate pressure reduction process>> After the first subcritical water treatment step is completed, the steam exhaust valve 32 is opened to discharge a portion of the high-pressure steam from the treatment space, thereby lowering the pressure in the treatment space from the high pressure. This pressure reduction is for the purpose of enabling the subsequent first liquid recovery step to be performed safely and efficiently, and it is sufficient to reduce the pressure in the treatment space to about 2 to 4 atm. It is not necessary to reduce it to atmospheric pressure. The temperature also decreases with this pressure reduction, but it is extremely small, and the decrease is only about several degrees Celsius, including the temperature decrease in the subsequent first liquid recovery step. The decrease in temperature is due to natural cooling. In order to efficiently perform the subsequent second subcritical water treatment step, it is desirable for the temperature decrease to be as small as possible. The steam discharged in this process is led to the condensation means 34, where it is condensed into a liquid containing useful components such as volatile components, and the condensed liquid is collected in a storage container 38 via a pipeline 35.

[0047] <<First liquid recovery process>> In this process, the opening / closing mechanism 26 is kept closed, and the opening / closing valve 60 is opened, and the liquid (fulvic acid / humic acid mixed solution) that is the raw material for fulvic acid / humic acid is recovered from the treatment space to the recovery section 50 via the liquid recovery flow path 54. The mixed solution may be used as it is, but the humic acid and fulvic acid are separated from the mixed solution to obtain a fulvic acid solution and a humic acid solution. The separation of the humic acid and the fulvic acid in the obtaining process is performed by making the solution acidic and separating the humic acid by precipitation or filtration. The pH of the solution is preferably 2 to 3. At this time, the solid content remains in the sealed container 12 and awaits the next process. The pressure reducing step and the first liquid recovering step are preferably performed by closing the steam supply control valve 46a and temporarily stopping the supply of steam to the sealed container 12.

[0048] 《Closing process》 Next, the steam exhaust valve 32 and the on-off valve 60 are closed.

[0049] <Second subcritical water treatment process> In the second subcritical water treatment process, the solid matter remaining in the treatment space is treated with subcritical water using steam having a higher temperature and pressure than the steam used in the first subcritical water treatment process. That is, while introducing steam having a temperature of 200 to 250°C and a pressure of 15 to 30 atm into the treatment space, the raw material is stirred, and a carbonized solid formed by carbonizing the raw material using a subcritical water reaction and a second mixed solution containing wood acetic acid produced as a result of the carbonization are obtained. When coconut shells are used as the material, the well-known coconut shell activated carbon is obtained, which is a particularly preferred useful substance.

[0050] Final pressure reduction process After the second subcritical water treatment process, which is the previous process, is completed, the steam exhaust valve 32 is opened to exhaust the high-pressure steam from the treatment space, thereby reducing the pressure in the treatment space from high pressure to atmospheric pressure. At this time, if useful substances are expected to be present in the discharged pressurized steam, the discharged high-pressure steam may be liquefied by condensation means 34 and collected in storage vessel 38, similar to the case after the intermediate pressure reduction step. The useful substances in this case include terpene oil, etc. Incidentally, the temperature also drops along with this pressure drop, but this drop in temperature is due to natural cooling.

[0051] <<Second liquid recovery process>> The on-off valve 60 is opened to recover only the liquid from the treatment space. This liquid is wood vinegar rich in wood acetic acid, and can be used as a disinfectant, crop growth inhibitor, crop growth promoter, deodorizer, etc. by simply diluting it to a predetermined dilution concentration without purification.

[0052] <Solid recovery process> Thereafter, the opening and closing mechanism 26 is opened, and the solid carbide is collected from the treatment space. This completes the method for producing two or more useful substances according to the embodiment of the present invention. The changes in the treatment pressure and treatment temperature during the above treatment steps are shown in FIG. [Explanation of symbols]

[0053] 10. Organic waste treatment equipment 12. Airtight containers 14 Steam ejection means 16 Outlet 18 Separation and Recovery Methods 26 Opening and closing mechanism 30 Stirring means 32 Steam exhaust valve 50 Collection Department 52 Gravity recovery mechanism 54 Liquid recovery flow path 58 Liquid inlet 60 Opening and closing valve 100 Control circuit

Claims

1. A method for producing useful substances by treating wood chips as a raw material to produce at least two or more useful substances, comprising the steps of: an apparatus preparation step of preparing a treatment apparatus including a sealed container having a closable treatment space therein, a supply unit for supplying raw material into the sealed container, a steam ejection means for ejecting high-temperature, high-pressure steam into the sealed container, an outlet unit having an open / close valve for ejecting only liquid from the sealed container and an open / close mechanism for ejecting solid matter, and a steam outlet having a steam exhaust valve for ejecting high-pressure steam from the sealed container; a raw material input step of inputting a raw material containing wood chips as a main raw material from the supply unit into a treatment space of the sealed container of the treatment device; a first subcritical water treatment step in which steam having a temperature of 120 to 200° C. and a pressure of 4 to 15 atm is introduced into the treatment space into which the raw material has been charged, and the raw material is subjected to a subcritical water reaction treatment while stirring the raw material to obtain a first mixed solution containing fulvic acid, humic acid, and solid matter of wood chips and / or fragments thereof; an intermediate pressure reduction step of opening the steam exhaust valve to exhaust high-pressure steam from the treatment space to reduce the pressure in the treatment space from high pressure; A first liquid recovery step of opening the on-off valve to recover only the liquid that is the raw material for fulvic acid / humic acid from the treatment space; a closing step of closing the steam exhaust valve and the on-off valve; a second subcritical water treatment step in which the raw material is carbonized by a subcritical water reaction while stirring the raw material and introducing steam having a temperature of 200 to 250° C. and a pressure of 15 to 30 atm into the treatment space in which the solid is present, to obtain a second mixed solution containing a carbonized solid formed by the carbonization and wood acetic acid produced by the carbonization; a final depressurization step of opening the steam exhaust valve to exhaust high pressure steam from the treatment space to reduce the pressure in the treatment space from high pressure to atmospheric pressure; a second liquid recovery step of recovering only the liquid serving as a raw material for wood acetic acid from the treatment space by opening the on-off valve; and a solid recovery step of opening the opening / closing mechanism and recovering solid carbide from the treatment space; A method for producing a useful substance, comprising:

2. 2. The method for producing a useful substance according to claim 1, wherein in the first subcritical water treatment step, the maximum temperature is maintained for 15 to 20 minutes.

3. 3. The method for producing a useful substance according to claim 1 or 2, wherein in the second subcritical water treatment step, the maximum temperature is maintained for 15 to 20 minutes.

4. The method for producing a useful substance according to any one of claims 1 to 3, wherein the wood is felled wood or waste wood.

5. 5. The method for producing useful substances according to claim 4, wherein said felled wood is from broadleaf or coniferous trees.

6. 6. The method for producing a useful substance according to claim 5, wherein said broad-leaved tree is birch, willow, chestnut, oak or beech.

7. 6. The method for producing a useful substance according to claim 5, wherein said coniferous tree is pine, cedar, cypress or angelica tree.

8. The method for producing a useful substance according to claim 4, wherein the waste material is solid wood or plywood.

9. 6. The method for producing a useful substance according to claim 5, wherein the main raw material is broad-leaved wood, and the pressure of the steam introduced in the first subcritical water treatment step is 4 to 15 atm.

10. 6. The method for producing a useful substance according to claim 5, wherein the main raw material is coniferous wood, and the pressure of the steam introduced in the first subcritical water treatment step is 5 to 15 atm.

11. 11. The method for producing a useful substance according to claim 1, wherein the raw material is introduced into said treatment space in a volumetric ratio of 90% or less.

12. 11. The method for producing a useful substance according to claim 1, wherein the raw material is introduced into said treatment space in a volumetric ratio of 50 to 80%.

13. 13. The method for producing a useful substance according to any one of claims 1 to 12, wherein an alkaline solution is added as an additive in the raw material input step.

14. The method for producing a useful substance according to any one of claims 1 to 13, comprising the leaves of woody plants as a raw material.

15. The method for producing a useful substance according to any one of claims 1 to 14, wherein the treatment device is provided with a condensation means connected to the steam exhaust port, and volatile organic compounds derived from wood are condensed and recovered from the high-pressure steam ejected from the steam exhaust port by the condensation means.

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