WO2023063287A1

WO2023063287A1 - Method and apparatus for producing useful substance

Info

Publication number: WO2023063287A1
Application number: PCT/JP2022/037773
Authority: WO
Inventors: 三郎松井
Original assignee: Ｇ－８ＩｎｔｅｒｎａｔｉｏｎａｌＴｒａｄｉｎｇ株式会社
Priority date: 2021-10-12
Filing date: 2022-10-11
Publication date: 2023-04-20
Also published as: JP2023057596A

Abstract

A method according to the present invention for producing a useful substance by treating wood chips, which is a raw material, to produce at least two useful substances is characterized by comprising: a device preparation step for preparing a treatment device provided with an airtight container, a supply part, a steam jetting means, a discharge port part having an opening/closing valve and an opening/closing mechanism, and a steam discharge port having a steam discharge valve; a raw material introduction step for introducing a raw material containing wood chips as a main raw material from the supply part into a treatment space of the airtight container of the treatment device; a first subcritical water treatment step for introducing steam having a temperature of 120-200 °C and a pressure of 4-15 atm into the treatment space into which the raw material has been introduced while stirring the raw material and performing a subcritical water reaction treatment on the raw material to obtain a first mixed solution containing fulvic acid, humic acid, and solid matter of chips and/or fragments of wood; an intermediate pressure lowering step for opening the steam discharge valve and discharging high-pressure steam from the treatment space to lower the pressure in the treatment space from a high pressure; a liquid recovery step for opening the opening/closing valve to recover only a liquid serving as a raw material for fulvic acid/humic acid from the treatment space; a closing step for closing the steam discharge valve and the opening/closing valve; a second subcritical water treatment step for introducing a steam having a temperature of 200-250 °C and a pressure of 15-30 atm into the treatment space in which the solid matter is present while stirring the raw material to obtain a carbonized solid matter formed by carbonizing the raw material by means of a subcritical water reaction and a second mixed solution containing a wood vinegar generated according to the carbonization; a final pressure lowering step for opening the steam discharge valve and discharging high-pressure steam from the treatment space to lower the pressure in the treatment space from high pressure to atmospheric pressure; a liquid recovery step for opening the opening/closing valve to recover only the liquid to be a raw material for wood vinegar from the treatment space; and a solid recovery step for opening the opening/closing mechanism to recover the solid carbide from the treatment space.

Description

Manufacturing method and manufacturing apparatus for useful substance

The present invention relates to a method and apparatus for producing useful substances, and in particular, to a method and apparatus for producing useful substances that use wood as a raw material, particularly fulvic acid/humic acid and wood acetic acid.

Humic substances such as fulvic acid and humic acid are said to be a generic term for "organic substances with unspecified chemical structures (non-living organic substances)" that are organic substances that have decayed due to microbial and chemical action after the death of living organisms. there is It is empirically known that some humic substances exhibit functionality and others do not. It is considered that whether or not the intermediate product is included in the process has a large effect. A humic substance that exhibits functionality when it contains this intermediate product is sometimes referred to as a humic precursor. (Non-Patent Document 1)

Substances corresponding to this humic substance (or humic precursor) existed in the natural world. These effects have been used in various ways. On the other hand, in recent years, modern agriculture and raw material processing methods that actively use developed chemical substances are widely used. However, apart from such modern agriculture and raw material processing, the use of this humic substance, which has been utilized since ancient times, is beginning to be reconsidered, and artificially produced fulvic acid is selectively used in high concentrations. Some solutions, etc. containing it are also sold.

For example, Patent Document 1 discloses a wastewater treatment method using a bacterial group consisting of soil-dwelling facultative anaerobic bacteria cultivated to produce metabolites containing phenol and/or compounds with phenol-exposed groups. It is a technology related to This "metabolite containing a phenol or/and a compound with a phenol-exposed group" causes a polycondensation reaction of humification by reacting with silicic acid, etc., and is an excellent wastewater that utilizes humus. It is intended to disclose a processing method.

As seen in Patent Document 1 and Non-Patent Document 1, technologies using humic precursors and humic substances (humic plants) are being studied. Here, humic plants are known to contain humin, fulvic acid, humic acid, etc. as the degree of humification (degree of polycondensation reaction) of their components. Common humic substances contain fulvic acid and humic acid at a weight ratio of about 2:8.

As shown in Patent Document 1, in the process of treating wastewater containing organic substances, there are those that use substances corresponding to this humic substance, but fulvic acid, humic acid, etc. in humic substances are not simple substances, Because of the fact that all of them are regarded as a group of multiple organic compounds, and because it is difficult to separate them, there has not been sufficient research on which substances have what effects specifically. . However, commercially available solutions containing fulvic acid are also expected to be effective as (micro)biologically active liquids, and are also suitable for applications such as agriculture where large quantities of products are required to be provided at the lowest possible cost. In order to utilize , there is a demand for a product that selectively contains fulvic acid at a high concentration.

Therefore, in Japanese Patent Application Laid-Open No. 2017-112947 (Patent Document 2), regarding fulvic acid, which is expected to be used as a (micro)biologically active liquid among humic substances, compared to the ratio of general humic substances, humin The following production method has been proposed for the purpose of providing a method for producing a fulvic acid-rich liquid containing a high ratio of fulvic acid to acid.

In the method for producing a fulvic acid-containing liquid proposed in Patent Document 2, an organic substance mixed liquid in which an organic substance and fulvic acid-acclimated sludge are mixed is heated to a dissolved oxygen concentration of 0.1 mg-O / L or less for 4 hours. By culturing as described above, an anaerobic culture step in which the organic substance in the organic substance mixture is reduced by anaerobic culture to obtain an anaerobic culture solution, and a dissolved oxygen concentration of 0.2 mg-O / in the anaerobic culture solution. An aerobic culture step of increasing fulvic acid in the anaerobic culture solution to obtain a fulvic acid-containing culture solution by culturing at L or more for 6 hours or more, and completion of the culture cultured in the aerobic culture step It is characterized by obtaining a fulvic acid-containing liquid from the aerobic culture medium returning step of returning the previous culture medium to the anaerobic culture step and the fulvic acid-containing culture medium obtained from the aerobic culture step.

The applicant previously proposed in Japanese Patent No. 6286605 a method for producing a fulvic acid solution that is completely different from the method described in the above publication.

The method for producing fulvic acid proposed in this patent publication is
a sealed container having a closable processing space therein; steam ejection means for ejecting high-temperature and high-pressure steam into the closed container; , an apparatus preparation step of preparing a processing apparatus having an opening/closing mechanism and a discharge unit for discharging the processing liquid generated by processing the raw material with the steam to the outside;
A raw material charging step of charging a raw material containing wood chips as a main raw material from the supply unit into the processing space of the closed container of the processing apparatus;
While introducing steam having a temperature of 120 to 250° C. and a pressure of 12 to 35 atm into the processing space in which the raw material is charged, the raw material is subjected to subcritical water reaction treatment while stirring the raw material, a process step of obtaining a mixed solution containing a suspension of fulvic acid, humic acid and wood chips and/or fragments thereof, and
A method for producing a fulvic acid solution, comprising a step of obtaining a fulvic acid solution by separating fulvic acid from the obtained mixed solution.

Japanese Patent Publication No. 5-66199

JP 2017-112947 A

Japanese Patent No. 6286605

According to the method for producing fulvic acid described in the above patent publication, fulvic acid with good purity can be produced efficiently. However, wood contains a number of other useful substances (including useful substances derived from wood). was not utilized effectively.

Therefore, an object of the present invention is to provide a useful substance manufacturing method and a manufacturing apparatus for manufacturing two or more useful substances using wood as a raw material.

The above objects are 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 useful substances,
a closed container having a closable processing space therein; a supply unit for supplying raw materials into the closed container; steam jetting means for jetting high-temperature and high-pressure steam into the closed container; A treatment comprising an outlet part having an opening/closing valve for discharging only liquid and an opening/closing mechanism for discharging solid matter, and a steam outlet having a steam outlet valve for discharging high-pressure steam from the closed container. a device preparation step of preparing a device;
A raw material charging step of charging a raw material containing wood chips as a main raw material from the supply unit into the processing space of the closed container of the processing apparatus;
While introducing steam having a temperature of 120 to 200° C. and a pressure of 4 to 15 atm into the processing space in which the raw material is charged, the raw material is subjected to subcritical water reaction treatment while stirring the raw material, A first subcritical water treatment step of obtaining a first mixed solution containing solids of fulvic acid, humic acid, and wood chips and/or fragments thereof;
an intermediate pressure reduction step of opening the steam exhaust valve to exhaust high pressure steam from the processing space to reduce the pressure in the processing space from the high pressure;
a first liquid recovery step of opening the opening/closing valve to recover only the liquid that is the raw material of fulvic acid/humic acid from the processing space;
a closing step of closing the steam discharge valve and the on-off valve;
While introducing steam having a temperature of 200 to 250° C. and a pressure of 15 to 30 atm into the processing space where the solid matter exists, the raw material is carbonized by a subcritical water reaction while stirring the raw material. a second subcritical water treatment step of obtaining a second mixed solution containing the formed carbonized solid and pyroligneous acid produced along with the carbonization;
a final pressure reduction step of opening the steam exhaust valve to exhaust high pressure steam from the processing space to reduce the pressure in the processing space from high pressure to atmospheric pressure;
A second liquid recovery step of opening the opening/closing valve to recover only the liquid that will be the raw material of pyroligneous acid from the processing space, and a solid recovery step of opening the opening/closing mechanism to recover solid carbide from the processing space. ,
A method for producing a useful substance, comprising:
(2)
The method for producing a useful substance according to (1) above, wherein the maximum temperature holding time is 15 to 20 minutes in the first subcritical water treatment step.
(3)
The method for producing a useful substance according to (1) or (2), wherein the maximum temperature holding time is 15 to 20 minutes in the second subcritical water treatment step.
(4)
The method for producing a useful substance according to (1), wherein the wood is felled wood or waste wood.
(5)
The method for producing a useful substance according to (4) above, wherein the felled timber is from a broad-leaved tree or a coniferous tree.
(6)
The method for producing a useful substance according to (5) above, wherein the broadleaf 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 performed for 1 to 8 hours.
(10)
The method for producing a useful substance according to (5) above, wherein the main raw material is hardwood, 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 softwood, 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) above, wherein the raw material is introduced into 90% or less of the processing space in terms of volume ratio.
(13)
The method for producing a useful substance according to any one of the above (1) to (11), wherein the raw material is introduced in 50 to 80% of the processing space in terms of volume ratio.
(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 arranged in 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)
The method for producing a useful substance according to any one of (1) to (15) above, which contains woody leaves as a raw material.
(17)
The processing equipment includes a condensing means connected to the steam outlet, and the condensing means recovers the wood-derived volatile organic compounds from the high-pressure steam ejected from the steam outlet by condensing the (1) ) to (16).
(18)
A useful substance manufacturing apparatus for manufacturing at least two kinds of useful substances by processing wood chips as raw materials, comprising: a closed container having a closable processing space therein; and supplying raw materials into the closed container. a supply unit for the purpose, a steam ejection means for ejecting high-temperature and high-pressure steam into the sealed container, an opening/closing valve for discharging only the liquid from the closed container, and an opening/closing mechanism for discharging the solid matter. an outlet, a steam outlet having a steam outlet valve for discharging high-pressure steam from the closed container, and a wood-derived volatile organic compound connected to the steam outlet and ejected from the high-pressure steam ejected from the steam outlet. A useful substance manufacturing apparatus equipped with condensing means for condensing and recovering compounds.

As described above, according to the present invention, it is possible to produce at least two kinds of useful substances in a series of steps using mainly wood chips as raw materials, which is efficient and extremely economical. be.
Moreover, according to the present invention, it is possible to obtain a fulvic acid solution with high purity.

BRIEF DESCRIPTION OF THE DRAWINGS It is sectional drawing which shows an example of the manufacturing apparatus of the useful substance by embodiment of this invention. FIG. 2 is a diagram showing changes in treatment pressure and treatment temperature in a treatment step in the method for producing a useful substance of the present invention.

A useful substance manufacturing apparatus 10 according to an embodiment of the present invention will be described below.
The manufacturing apparatus 10 includes a sealed container 12 having a closed space S1, which is a processing space for containing raw materials, which are wood chips, and a steam jet for jetting high-temperature and high-pressure steam, which is subcritical water, into the closed container 12. means 14, a discharge port 16 provided on the bottom side of the sealed container 12 and having an opening/closing mechanism 26, and a separating and recovering means 18 for separating and collecting the raw material and the liquid which have been treated only by the direct discharge operation from the discharge port 16. and have. The shape of the closed container 12 may be, for example, a rectangular box shape, a three-dimensional polygonal cylinder shape, a cylindrical shape, a barrel shape, a drum shape, or any other shape. A shape that is ejected is preferred. It is preferable that the bottom surface of the closed container is inclined downward toward the outlet.

The separation and recovery means 18 includes a liquid recovery section 50 communicating with the inside of the sealed container 12 through the discharge port 16, and recovers only the liquid in the closed container 12 to the recovery section 50 by gravity flow through the discharge port 16. It is good also as having a gravity collection mechanism 52 and. The raw material as a solid content processed near the discharge port 16 remains in the closed container 12 as it is, and only the liquid naturally flows down to the recovery section 50 using gravity, so that the raw material and the liquid can be separated and recovered. The recovery unit 50 may have any configuration, such as a metal tank, a three-dimensional polygonal box, or a tubular body, as long as it has a closed space S2 for recovering the liquid. A plurality of accommodating portions may be formed.

In the above example, the separation means is incorporated in the processing apparatus, but the separation means may be provided separately in the processing apparatus itself.
The gravity recovery mechanism 52 also includes a liquid recovery channel 54 that communicates and connects the discharge port 16 of the sealed container 12 and the recovery unit 50 . It may be provided horizontally or downwardly toward the 50 side.

In addition, an opening/closing mechanism 26 is provided in the middle of the discharge route R1 from the discharge port 16 of the processed raw material, and the liquid introduction port 58 of the liquid recovery channel 54 is connected to the discharge upstream side of the opening/closing mechanism 26 .

In addition, the liquid recovery channel 54 is selected so as to block the channel during the processing of the raw material in the sealed container 12 and to allow the channel to communicate when only the liquid is recovered after the processing. An opening/closing valve 60 is provided for switching between them.

Also, the bottom surface of the closed space S2 of the recovery unit 50 may be provided lower than the position of the discharge port 16 of the sealed container 12.

The sealed container 12 is preferably formed in a sideways barrel shape in which a discharge port 16 is provided on the bottom side of the left-right central portion and the diameter gradually decreases from the left-right central portion toward the left and right end sides. A stirring member 30 is provided inside the sealed container 12 . The stirring means 30 is provided horizontally coaxially with the horizontal central axis of the sealed container 12, and has a rotating shaft 49 rotatably supported at both ends thereof. and a stirring blade 48 extending in the circumferential direction, and the length from the rotating shaft 49 of the stirring blade 48 to the tip of the blade corresponds to the overturned barrel shape of the closed container 12, as shown in the figure. It is preferable that it is formed so that it is large at the central position in the longitudinal direction of 49 and gradually becomes smaller toward both ends.

Also, the steam jetting means 14 includes a rotating shaft/steam jetting pipe 28 configured by forming a plurality of steam jetting holes 44 on the peripheral surface of the hollow tube with the rotating shaft 49 as a hollow tube. good too.

Although not shown, the sealed container 12 is preferably supported by supporting legs so as to be positioned at a certain height from the ground. It is preferable that the closed container 12 is formed by processing a metal plate so as to have heat resistance and pressure resistance, and that the closed space inside is provided with a size of about 2 m ³ or more. The airtight container 12 is provided with an inlet section 20 at the central upper portion and an outlet section 22 at the central bottom portion, and is provided with opening/

closing mechanisms

24 and 26, respectively, so that it can be opened and closed. The sealed container 12 is provided with, for example, a safety valve (not shown) capable of adjusting the set pressure, which releases the internal steam when the internal pressure becomes higher than the set value. In addition, a silencing/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 muted and deodorized before being discharged to the outside air.

The diameter of the discharge port 16 is, for example, about 300 mm. A downward projecting discharge tube 36 is connected to the discharge port 16 to form the discharge route R1 for the processed raw material. The opening/closing mechanism 26 for opening and closing the discharge port 16 is provided in the middle of the discharge path R1 of the discharge tube 36. As shown in FIG. That is, the discharge section 22 is configured to include the discharge port 16 , the discharge tube 36 , and the opening/closing mechanism 26 . Since the sealed container 12 is formed in a barrel-like shape lying down, the raw material inside tends to gather from the left and right toward the central portion where the discharge port 16 is provided due to gravity, and can be easily processed simply by opening the opening and closing mechanism 26. The finished raw material can be discharged from the discharge port 16 .

The input port 42 is opened in the center of the upper side of the sealed container 12 in the input part 20, and the input cylinder 43 projecting upward is attached to the input port 42, and the inside of the input cylinder 43 is opened and closed. The opening/closing mechanism 24 is provided as follows. Via the opening/closing mechanism 24, the input port 42 can be opened to input the raw material into the closed container, and closed during processing to maintain the closed state of the closed space S1 in the closed container 12.例文帳に追加

The steam ejecting means 14 ejects high-temperature, high-pressure steam into the sealed container 12, and sets the inside of the closed container 12 to a high-temperature, high-pressure state, and processes the raw material using the steam. As shown in FIG. 1, the steam ejection means 14 includes a steam ejection pipe 28 which is a hollow tube arranged in the sealed container 12 and formed with a large number of steam ejection holes 44 on the peripheral surface side, and a steam generator such as a boiler. A device 46 and a steam conduit 47 for supplying steam from the steam generator 46 into the steam jet 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 by closing the steam supply control valve 46a, the supply of steam can be temporarily stopped. It is possible. The steam supply control valve 46 a may be provided in the steam pipe 47 .
The steam jetted from the steam jetting means 14 into the sealed container 12 is set to a high temperature and high pressure that satisfies the conditions of subcritical water in order to properly treat the raw material. For example, the steam ejected from the steam ejection pipe 28 has a temperature of 120 to 250° C. and a pressure of 4 to 30 atm. The inside of the sealed container 12 is kept at a temperature of 120 to 250° C. and a pressure of 4 to 30 atm. The steam ejection pipe 28 is arranged long in the horizontal direction at a substantially central position in the vertical direction of the sealed container 12, and is rotatably supported via bearings 45 provided on both

end walls

12a and 12b of the sealed container. That is, the steam ejection pipe 28 is adapted to directly apply the steam to the raw material while rotating around the horizontal axis and ejecting the steam radially. The steam ejection pipe 28 is rotated by receiving rotational driving force from a rotational driving device (not shown) such as a motor through a chain 70 or the like. Further, the steam ejection pipe 28 is attached with a stirring blade 48 that constitutes the stirring means, and the steam ejection pipe 28 also serves as a rotating shaft 49 of the stirring means. That is, in the present embodiment, the steam ejecting means 14 is a rotating shaft and steam configured by using a hollow tube as the rotating shaft 49 of the stirring means and forming a plurality of steam ejecting holes on the peripheral surface of the hollow tube. Includes ejection tube 28 . The steam ejection means is not limited to this configuration, and may be of any other configuration, such as a configuration in which steam is ejected from the tip of a pipe inserted into a closed container, a configuration in which a plurality of steam ejection pipes are arranged, and the like. good.

The stirring means 30 is a means for stirring raw materials to be processed in a closed container, and can process the raw materials evenly and quickly. The stirring means 30 includes a rotating shaft 49 made up of the steam ejection pipe 28, and stirring blades 48 attached to the rotating shaft 49 and having portions extending 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 provided at a substantially central position in the axial direction of the rotating shaft 49 so as to be wound in opposite directions. As described above, the stirring blades 48 are provided such that the length from the rotating shaft to the tip of the blade gradually decreases in diameter from the left-right central portion toward both ends. As a result, the raw material can be reliably agitated corresponding to the overturned barrel shape of the closed container 12 . Furthermore, it is provided so as to form a certain amount of gap H between the tip of the blade and the inner wall of the closed container 12 . The

spiral blades

48a and 48b stir the raw material while crushing the solid raw material while conveying the raw material from the central portion toward the both end wall sides. The raw material conveyed to the side of both

end walls

12a and 12b by the stirring blade 48 is pushed by the raw material that is subsequently conveyed on the side of the

end walls

12a and 12b, along the inner wall of the sealed container 12 and through the gap H. Transported back to center. In addition, the stirring means 30 is not limited to the configuration described above, and may be of any other configuration.

The separation/recovery means 18 is a separation/recovery means that separates and recovers the processed raw material and the liquid in the sealed container 12 after steam treatment only by direct operation from the discharge port. As shown in FIG. 1, the separation and recovery means 18 includes a liquid recovery section 50 that communicates with the inside of the sealed container 12 through the discharge port 16, and the recovery section 50 recovers the liquid through the discharge port 16 by gravity flow. and a gravity recovery mechanism 52 .

The liquid recovery channel 54 has a liquid inlet port 58 connected to the discharge port 16 so as to form a liquid recovery route R2 branched from the processed raw material discharge route R1. In this embodiment, the liquid recovery channel 54 is provided by, for example, a metal tube having an inner diameter of about 6 mm. The liquid recovery channel 54 is provided with the opening/closing valve 60 for selectively switching the communication state of the channel, as described above. The opening/closing valve 60 is switched so as to block the flow path during the processing of the raw material in the closed container and open the flow path when only the liquid is separated and recovered after the processing. As a result, the moisture and steam contained in the raw material are liquefied at the same time as the raw material, and the liquid containing bacteria and malodorous components in the raw material can be treated with high-temperature, high-pressure steam. The liquid separated and recovered after the treatment can be recovered in a state such as sterilization or decomposition of odors and harmful components. Time can be shortened.

A volatile useful substance recovery mechanism 30 such as terpene oil is provided in the upper part of the closed container 12, and this volatile useful substance recovery mechanism 30 is connected to the high-pressure high-temperature steam discharge port 19 provided in the closed container 12. A high-temperature and high-pressure steam discharge pipe 31 communicating with the closed space S1 via a steam discharge valve 32 provided upstream of the high-temperature and high-pressure steam discharge pipe 31, and receiving the high-temperature and high-pressure steam from the steam discharge valve 32. Condensing means 34 for cooling and condensing said high pressure and high temperature steam to recover a liquid containing volatile organic compounds derived from wood, and a storage vessel to which the liquid from said condensing means 34 is conveyed via a line 35. 38.

The liquid stored in the storage container 38 is a liquid containing volatile organic compounds derived from wood as described above, and the volatile organic compounds are extracted from the liquid as necessary to produce products.

The manufacturing apparatus 10 is composed of a central processing circuit and the like, and according to a predetermined program stored in advance, the opening/closing mechanism 26, the steam discharge valve 32, the steam generator 46, the steam supply control valve 46a, the opening/closing valve 60, etc. A control circuit 100 is provided to control the operation.

Next, a method for manufacturing a useful substance according to an embodiment of the present invention using the manufacturing apparatus 10 described above will be described.
A method for producing a useful substance according to an embodiment of the present invention comprises an apparatus preparation step of preparing the processing apparatus as described above;
A raw material charging step of charging a raw material containing wood chips as a main raw material from the supply unit into the processing space of the closed container of the processing apparatus;
While introducing steam having a temperature of 120 to 200° C. and a pressure of 4 to 15 atm into the processing space in which the raw material is charged, the raw material is subjected to subcritical water reaction treatment while stirring the raw material, A first subcritical water treatment step of obtaining a first mixed solution containing solids of fulvic acid, humic acid, and wood chips and/or fragments thereof;
an intermediate pressure reduction step of opening the steam exhaust valve to exhaust high pressure steam from the processing space to reduce the pressure in the processing space from the high pressure;
A liquid recovery step of opening the opening/closing valve to recover only the liquid that is the raw material of fulvic acid/humic acid from the processing space;
a closing step of closing the steam discharge valve and the on-off valve;
While introducing steam having a temperature of 200 to 250° C. and a pressure of 15 to 30 atm into the processing space where the solid matter exists, the raw material is carbonized by a subcritical water reaction while stirring the raw material. a second subcritical water treatment step of obtaining a second mixed solution containing the formed carbonized solid and pyroligneous acid produced along with the carbonization;
a final pressure reduction step of opening the steam exhaust valve to exhaust high pressure steam from the processing space to reduce the pressure in the processing space from high pressure to atmospheric pressure;
A liquid recovery step of opening the opening/closing valve to recover only the liquid that will be the raw material of pyroligneous acid from the processing space, and a solid recovery step of opening the opening/closing mechanism to recover solid carbide from the processing space,
It has
In addition, in the above, it is preferable that the control circuit 100 automatically performs the steps after the raw material supply step according to a predetermined program.

Each step described above will be described in detail below.
《Equipment preparation process》
A manufacturing apparatus (processing apparatus) as described above is prepared with reference to the drawings.

《Raw material input process》
The main raw material is wood chips. The size of the chip is preferably about 50 to 150 cm on the long side and about 5 cm on the short side 2 . As a secondary material or additive, an alkaline solution can be added in order to efficiently produce more fulvic acid. The vapor pressure and temperature when adding the alkaline solution may be the same as when not adding.

As the wood, generally felled wood or waste wood can be used.
The felled wood may be either broad-leaved trees or coniferous trees.
As the broad-leaved tree, any broad-leaved tree may be used, but at present, for example, white birch, willow, chestnut, oak, beech, etc. are preferably used.
As the conifers, pine, cedar, Japanese cypress, Asunaro, etc. can be preferably used at present.
When using felled wood, it is not necessary to remove the bark or the like. It may also contain leaves, roots, or fruit shells such as coconut shells as they are or in the form of chips.

Waste materials include wood chips (square timbers, planks: solid timbers, laminated timbers/plywood timbers (plywood)) generated during the demolition of wooden houses. Since such wood waste is generally made into chips, it can be used as it is as a raw material.
The raw materials mentioned above may be mixed and used. For example, when trees are felled in ordinary households, felled wood of various kinds of trees is discharged. These woods may be used as a raw material by mixing the whole wood as chips without sorting them. Of course, waste chips may be mixed therein.

The raw materials, which are chips as described above, are put into the processing space, and the amount of raw materials is preferably 90% or less, particularly 50 to 80%, of the closed space S1 of the closed container 12, that is, the processing space. If the input amount of raw material is lower than this range, the treatment efficiency is poor, and if it exceeds this range, the steam may not act well on the raw material, resulting in insufficient production of fulvic acid.

<<First subcritical water treatment process>>
In this step, high-pressure high-temperature steam is introduced into the processing space in which the raw materials are charged, and the raw materials are subjected to a subcritical water reaction treatment while stirring the raw materials to obtain fulvic acid, humic acid, and wood chips. and/or obtain a first mixed solution containing solids of the fragments. The steam should have a temperature of 120 to 200° C. and a pressure of 4 to 15 atm. Therefore, the inside of the processing space is set to a processing temperature and pressure of 120 to 200° C. and a pressure of 4 to 15 atm. The amount of steam introduced depends on the volume of the processing space and the amount of raw material to be processed, but should be the amount that completely fills the surplus space (the space obtained by subtracting the volume of the raw material introduced from the processing space). is preferred.

When a broad-leaved tree is used as the felled wood, the high-pressure high-temperature steam supplied in the treatment process preferably has a temperature of 120 to 200° C. and a pressure of 4 to 15 atm.
On the other hand, when conifers are used as the felled wood, the high-pressure and high-temperature steam supplied in the treatment process preferably has a temperature of 140 to 200° C. and a pressure of 5 to 15 atm.
In this treatment step, as described above, steam is introduced into the treatment space into which the raw material is introduced, and the raw material is stirred to treat the raw material by the subcritical water reaction.
The duration of the treatment step is preferably 15 to 20 minutes at the maximum temperature/maximum pressure retention time, that is, the set treatment temperature/pressure. If the treatment time is shorter than the above range, the reaction time is insufficient, that is, the production of fulvic acid and humic acid is not sufficient, and a considerable amount of fulvic acid and humic acid remains in the raw material. If the above range is exceeded, the raw material will be carbonized, and unintended substances will be mixed into the solution.
In this treatment process, the raw material is subjected to subcritical water reaction treatment, and fulvic acid and humic acid are contained in the solution. This solution also contains a suspension of wood chips and/or fragments thereof. Thus, a mixed solution containing fulvic acid, humic acid and a suspension of wood chips and/or fragments thereof is obtained.
The mixed solution obtained in this step contains 3 to 12% of fulvic acid in the total amount of fulvic acid and humic acid (in solid content).

《Intermediate pressure reduction process》
After the first sub-critical water treatment step is completed, the steam exhaust valve 32 is opened to partially exhaust high-pressure steam from the processing space, thereby lowering the pressure in the processing space from the high pressure. This pressure drop is for enabling the next first liquid recovery step to be carried out safely and efficiently. It is not necessary to lower the pressure to atmospheric pressure. Although the temperature also drops with this pressure drop, it is extremely small, and the drop is about several degrees Celsius including the temperature drop in the next first liquid recovery step. The drop in temperature is due to natural cooling. In order to efficiently perform the second subcritical water treatment step to be performed later, it is desirable that the temperature drop be as small as possible.
The vapor discharged in this process is guided to the condensing means 34, where it is condensed with a liquid containing useful components such as volatile components, and collected in a storage container 38 via a conduit 35. be done.

<<First liquid recovery step>>
In this step, while the opening/closing mechanism 26 is kept closed, the opening/closing valve 60 is opened, and the liquid (mixed solution of fulvic acid/humic acid) that is the raw material of fulvic acid/humic acid is discharged from the processing space into a liquid recovery stream. It is recovered to the recovery section 50 via the path 54 .
Although the mixed solution may be used as it is, humic acid and fulvic acid are separated from this mixed solution to obtain a fulvic acid solution and a humic acid solution. The separation of humic acid and fulvic acid in this acquisition step is carried out by making the pH of the solution acidic and separating humic acid by precipitation or separation by filtration. The pH of the solution is preferably 2-3.
At this time, the solid content remains in the closed container 12 and waits for the next treatment.
The pressure reduction step and the first liquid recovery step are preferably performed by closing the steam supply control valve 46a and temporarily stopping the supply of steam to the sealed container 12. As shown in FIG.

《Closed process》
Then, the steam discharge valve 32 and the open/close valve 60 are closed.

<<Second subcritical water treatment process>>
In the second sub-critical water treatment step, the solids remaining in the treatment space are treated with sub-critical water with steam having a higher temperature and pressure than the steam used in the first sub-critical water treatment step.
That is, while introducing steam having a temperature of 200 to 250 ° C. and a pressure of 15 to 30 atm into the processing space, the raw material is carbonized by a subcritical water reaction while stirring the raw material. A second mixed solution is obtained which contains the carbonized solid matter and the pyroligneous acid produced along with the carbonization.
When coconut shell is used as the material, it becomes a well-known coconut shell activated carbon, which is a particularly preferable useful substance.

《Final pressure reduction process》
After the second subcritical water treatment step, which is the previous step, is completed, the steam discharge valve 32 is opened to discharge high-pressure steam from the processing space, thereby reducing the pressure in the processing space from high pressure to atmospheric pressure. .
At this time, if useful substances are expected to be present in the discharged pressure vapor, the discharged high pressure vapor is liquefied by the condensing means 34 and stored in the storage container 38 as in the case after the intermediate pressure reduction step. may be collected at Useful substances in this case include terpene oil and the like.
It should be noted that the temperature also drops with this pressure drop and the like, but this drop in temperature is due to natural cooling.

<<Second liquid recovery step>>
The on-off valve 60 is opened to recover only the liquid from the processing space. This liquid is a pyroligneous acid-rich liquid that can be used as a sterilizing liquid, a crop growth inhibitor, a crop growth promoter, a deodorant, etc., by simply diluting it to a predetermined dilution concentration without purification or the like. can be used.

《Solid recovery process》
After that, the first opening/closing mechanism 26 is opened to recover the solid carbide from the processing space.
This completes the method for producing two or more useful substances according to the embodiment of the present invention. FIG. 2 shows changes in processing pressure and processing temperature in the above processing steps.

REFERENCE SIGNS LIST 10 organic waste treatment apparatus 12 sealed container 14 steam ejection means 16 outlet 18 separation and recovery means 26 opening/closing mechanism 30 stirring means 32 steam discharge valve 50 recovery section 52 gravity recovery mechanism 54 liquid recovery channel 58 liquid inlet 60 Open/close valve 100 control circuit

Claims

A method for producing useful substances by treating wood chips as a raw material to produce at least two useful substances,
a closed container having a closable processing space therein; a supply unit for supplying raw materials into the closed container; steam jetting means for jetting high-temperature and high-pressure steam into the closed container; A treatment comprising an outlet part having an opening/closing valve for discharging only liquid and an opening/closing mechanism for discharging solid matter, and a steam outlet having a steam outlet valve for discharging high-pressure steam from the closed container. a device preparation step of preparing a device;
A raw material charging step of charging a raw material containing wood chips as a main raw material from the supply unit into the processing space of the closed container of the processing apparatus;
While introducing steam having a temperature of 120 to 200° C. and a pressure of 4 to 15 atm into the processing space in which the raw material is charged, the raw material is subjected to subcritical water reaction treatment while stirring the raw material, A first subcritical water treatment step of obtaining a first mixed solution containing solids of fulvic acid, humic acid, and wood chips and/or fragments thereof;
an intermediate pressure reduction step of opening the steam exhaust valve to exhaust high pressure steam from the processing space to reduce the pressure in the processing space from the high pressure;
a first liquid recovery step of opening the opening/closing valve to recover only the liquid that is the raw material of fulvic acid/humic acid from the processing space;
a closing step of closing the steam discharge valve and the on-off valve;
While introducing steam having a temperature of 200 to 250° C. and a pressure of 15 to 30 atm into the processing space where the solid matter exists, the raw material is carbonized by a subcritical water reaction while stirring the raw material. a second subcritical water treatment step of obtaining a second mixed solution containing the formed carbonized solid and pyroligneous acid produced along with the carbonization;
a final pressure reduction step of opening the steam exhaust valve to exhaust high pressure steam from the processing space to reduce the pressure in the processing space from high pressure to atmospheric pressure;
A second liquid recovery step of opening the opening/closing valve to recover only the liquid that will be the raw material of pyroligneous acid from the processing space, and a solid recovery step of opening the opening/closing mechanism to recover solid carbide from the processing space. ,
A method for producing a useful substance, comprising:
The method for producing a useful substance according to Claim 1, wherein the maximum temperature holding time is 15 to 20 minutes in the first subcritical water treatment step.
3. The method for producing a useful substance according to claim 1 or 2, wherein the maximum temperature holding time is 15 to 20 minutes in the second subcritical water treatment step.
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.
The method for producing a useful substance according to claim 4, wherein the felled timber is from a broad-leaved tree or a coniferous tree.
The method for producing a useful substance according to claim 5, wherein the broadleaf tree is birch, willow, chestnut, oak or beech.
The method for producing a useful substance according to claim 5, wherein the coniferous tree is pine, cedar, cypress or Asunaro.
The method for producing a useful substance according to claim 4, wherein the waste material is solid wood or plywood.
The method for producing a useful substance according to any one of claims 1 to 8, wherein the treatment step is performed for 1 to 8 hours.
The method for producing a useful substance according to claim 5, wherein the main raw material is hardwood, and the pressure of the steam introduced in the treatment process is 12 to 25 atm.
The method for producing a useful substance according to claim 5, wherein the main raw material is softwood, and the pressure of the steam introduced in the treatment process is 20 to 35 atm.
The method for producing a useful substance according to any one of claims 1 to 11, wherein the raw material is introduced into 90% or less of the processing space in terms of volume ratio.
The method for producing a useful substance according to any one of claims 1 to 11, wherein the raw material is introduced in 50 to 80% of the processing space in terms of volume ratio.
The method for producing a useful substance according to any one of claims 1 to 13, wherein the stirring in the treatment step is performed by a rotating stirring member arranged in the treatment space.
The method for producing a useful substance according to any one of claims 1 to 14, wherein an alkaline solution is added as an additive in the raw material charging step.
The method for producing a useful substance according to any one of Claims 1 to 15, which contains woody leaves as raw materials.
2. The processing equipment comprises condensing means connected to the steam outlet, and the condensing means recovers the wood-derived volatile organic compounds from the high-pressure steam emitted from the steam outlet by condensing. 16. A method for producing a useful substance according to any one of 16.
A useful substance manufacturing apparatus for manufacturing at least two kinds of useful substances by processing wood chips as raw materials, comprising: a closed container having a closable processing space therein; and supplying raw materials into the closed container. a supply unit for the purpose, a steam ejection means for ejecting high-temperature and high-pressure steam into the sealed container, an opening/closing valve for discharging only the liquid from the closed container, and an opening/closing mechanism for discharging the solid matter. an outlet, a steam outlet having a steam outlet valve for discharging high-pressure steam from the closed container, and a wood-derived volatile organic compound connected to the steam outlet and ejected from the high-pressure steam ejected from the steam outlet. A useful substance manufacturing apparatus equipped with condensing means for condensing and recovering compounds.