JP2009261992A - Subcritical water treatment apparatus of electromagnetic induction heating type - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a subcritical water treatment apparatus of an electromagnetic induction heating type which extracts useful substances in the living body in a short time by means of subcritical water of a predetermined temperature and pressure. <P>SOLUTION: A reaction oven 50 pressurizes and heats liquid water charged thereinto to change the water into a subcritical state and reacts the subcritical water with a raw material charged thereinto. A coil is wound twice or more around the reaction oven 50; the current passed through the coil is controlled by a current control section; and the inside of the reaction oven 50 is heated rapidly by electromagnetic induction heating control. The temperature and pressure of the subcritical water in the reaction oven 50 is adjusted with high precision, and a raw material and subcritical water charged in advance are allowed to react mutually in a short time, while the temperature, pressure and reaction time are controlled accurately, in order to extract useful ingredients. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a subcritical water treatment apparatus that adjusts the temperature and pressure of subcritical water with high accuracy and reacts materials such as plant tissue and animal tissue in a short time using subcritical water.

  Many useful substance components are contained in plant tissues and animal tissues, and these components have various uses, and various extraction methods have been tried. For example, there are methods of extraction using a solvent such as water, alcohol, and oil, or extraction by steam distillation.

  However, in many cases, many useful substances cannot be extracted by a simple method of immersing in a solvent. For example, hinokitiol contained in wood tissues such as hiba has a solubility in water of only 1 g / liter. The hinokitiol inside the wood chip tissue is difficult to extract with water, and the concentration process is also difficult.

As a method for decomposing plant tissue or animal tissue, there is a method using supercritical water or subcritical water.
Supercritical water is water in which the temperature and pressure exceed the critical point (374 ° C, 22.1 MPa). It has both the properties of gas and liquid, and supercritical water strongly decomposes organic substances. And is a fluid suitable for the decomposition of plant tissue and animal tissue biomass.
Subcritical water is slightly below the critical point (374 ° C., 22.1 MPa) and above the saturated vapor pressure curve. For example, subcritical water near 250 ° C. has high molecular weight such as protein and cellulose. The biomaterial is hydrolyzed at high speed to be decomposed into peptides, amino acids, oligosaccharides and monosaccharides, and further decomposed into organic acids such as acetic acid, propionic acid and lactic acid.

  In this way, focusing on the fact that supercritical water or subcritical water has a strong biomass resolving power, the conventional technology hydrolyzes high-molecular-weight biological substances such as proteins and cellulose from food residues, etc., and industrial waste. Expected to be used in processing equipment.

JP 2004-306021 A JP 2006-255676 A JP 2006-328304 A

  As described above, as a method of degrading biomass of plant tissue or animal tissue, a technique using supercritical water or subcritical water has attracted attention, and high molecular weight biological materials such as protein and cellulose are converted to low molecular weight materials such as peptides and amino acids. It can be broken down into organic matter.

  However, there are cases where useful components in the plant tissue or animal tissue to be extracted cannot be successfully extracted by the conventional technique using supercritical water or subcritical water. Useful components in plant tissues and animal tissues are present in the living body, and many are vulnerable to heat. For example, hemicellulose or cellulose hydrolyzate is thermally decomposed when exposed to higher temperatures. In addition, hinokitiol normally does not hydrolyze, but thermally decomposes at higher temperatures.

  Supercritical water and subcritical water are produced by heating in a closed kettle, etc., bringing the water to a high temperature and high pressure state, and heating until reaching a predetermined state beyond the critical point. If the food residue protein or cellulose is hydrolyzed at high speed and decomposed into low molecular weight organic substances as in the prior art, the food residue protein or cellulose in the heating process to produce supercritical water or subcritical water Although there is no problem even if it decomposes, useful substances such as hemicellulose, cellulose hydrolyzate, and hinokitiol are vulnerable to heat, and many of them are thermally decomposed during heating to subcritical water. . Furthermore, when it reaches a severer supercritical state, most useful substances such as hemicellulose, cellulose, hinokitiol and the like are thermally decomposed.

As described above, since many of the useful substances in the living body such as hemicellulose and cellulose hydrolyzate and hinokitiol are thermally decomposed at high temperature, the conventional technique has a method of extracting at low temperature for a long time in subcritical water. Has been sought.
As a method for extracting useful substances from biomass at low cost, the present inventor has found out conditions that allow extraction processing without decomposing useful substances while using subcritical water, and has developed a processing apparatus that enables the extraction conditions. went.

  In view of the above problems, an object of the present invention is to provide an electromagnetic induction heating type subcritical water treatment apparatus that extracts useful substances in a living body in a short time with subcritical water at a predetermined temperature and pressure. .

In order to achieve the above object, a first electromagnetic induction heating subcritical water treatment apparatus of the present invention comprises:
A reaction kettle that pressurizes and heats the liquid put into the kettle to a subcritical state, and reacts the material put into the kettle with the subcritical water;
A coil wound a plurality of times around the reaction kettle;
A current control unit for controlling a current flowing through the coil;
The current control unit controls the current flowing through the coil, and the temperature and pressure of the subcritical water in the reaction kettle are accurately adjusted by electromagnetic induction heating control, and the material in the reaction kettle and the subcritical water are controlled. It is characterized by reacting water in a short time.

  With the above configuration, the liquid in the reaction kettle can be rapidly heated and pressurized by electromagnetic induction heating to create a subcritical water state at the target temperature, and direct heat generation on the reaction kettle wall surface can be accurately performed by electromagnetic induction heating control. It can be controlled well and conditions such as temperature and pressure of subcritical water in the reaction kettle can be set optimally. This is not possible with conventional subcritical water treatment equipment.

In order to achieve the above object, the second electromagnetic induction heating subcritical water treatment apparatus of the present invention comprises:
A subcritical water generator for generating subcritical water;
An introduction pipe for taking out subcritical water that has reached a subcritical state from the subcritical water generator;
A reaction kettle for introducing the subcritical water from the introduction pipe and reacting the material introduced into the kettle with the subcritical water;
A coil wound a plurality of times around the reaction kettle;
A current control unit for controlling a current flowing through the coil;
The current control unit controls the current flowing through the coil, and the temperature and pressure of the subcritical water flowing in the reaction kettle are accurately adjusted by electromagnetic induction heating control. It is characterized by reacting critical water in a short time.

  With the above configuration, in continuous processing, the process of heating and pressurizing the liquid to create a subcritical water state and the extraction process of extracting useful substances from the material are separated, and the subcritical water at a predetermined temperature and pressure is immediately converted into the material. Subcriticality that can be applied to the material by accurately controlling direct heat generation on the reaction vessel wall surface by electromagnetic induction heating control, maintaining and adjusting the temperature and pressure of subcritical water in the reaction vessel with high accuracy Conditions such as water temperature, pressure and treatment time can be set optimally. This is not possible with conventional subcritical water treatment equipment.

  In the first and second electromagnetic induction heating subcritical water treatment apparatuses of the present invention, the following devices can be added.

  The first device is a structure in which a heat insulator is wound around the reaction kettle, and the insulating coating copper wire is wound around the reaction kettle around the reaction kettle. This is a device that prevents seizure of the coated copper wire.

The second device is provided with a plurality of groove structure voids on the outer peripheral surface of the heat insulator, and provided with cooling means such as a cooling fan for flowing cooling air along the groove structure voids. The coil-shaped insulating film copper wire is cooled on the outside of the heat insulator while keeping the temperature.
With the above-described configuration, the first and second devices are used to wrap the insulation around the reaction kettle to keep the temperature of the reaction kettle, and at the same time, ventilate the gaps in the groove structure provided on the outside of the heat insulation to make the insulation-coated copper wire. Can be effectively cooled to prevent seizure.

  A third device is a device that surrounds a metal projection such as a bolt provided in the reaction kettle with a magnetic material, shields leakage magnetic flux, and reduces eddy current generated in the metal projection. .

In the present invention, since eddy current is generated in the reaction kettle itself, it is desirable to reduce the number of places where eddy current is likely to be locally generated in the reaction kettle. As a result, it is possible to prevent parts from being burned.
In the first and second electromagnetic induction heating type subcritical water treatment apparatuses of the present invention having the above-described configuration, the control temperature of the subcritical water in the reaction vessel by the electromagnetic induction heating control is 50 to 400 ° C., and the pressure is saturated at the temperature. It can be maintained and adjusted freely above the water vapor pressure.

  Next, in the second electromagnetic induction heating type subcritical water treatment apparatus of the present invention, a bypass pipe branched from the introduction pipe is separately provided, and the subcritical water introduced from the subcritical water generator has a predetermined temperature range and When the pressure is not within the predetermined pressure range, it is preferable to escape with the bypass pipe, and when the pressure is within the predetermined temperature range and the predetermined pressure range, the pressure is preferably introduced into the reaction kettle through the introduction pipe.

Further, in the second electromagnetic induction heating subcritical water treatment apparatus of the present invention, when the subcritical water is introduced into the reaction kettle from the subcritical water generator via the introduction pipe, It is preferable to provide a pressurizing means capable of applying a gas pressure for maintaining the pressure of the water vapor above the saturated water vapor pressure in the reaction kettle. As the pressurizing means, there is a combination of a cylinder for supplying an inert gas and a pressure increasing device for applying the inert gas from the cylinder to the reaction kettle at a predetermined pressure.
With the above configuration, subcritical water in a predetermined temperature range and a predetermined pressure range can be stably and continuously supplied, and a gas pressure can be applied so that the pressure in the reaction kettle does not drop during the introduction, Extraction of components from the material using subcritical water in the reaction kettle can be carried out continuously under subcritical conditions.

According to the first electromagnetic induction heating type subcritical water treatment apparatus according to the present invention, in the so-called batch processing type subcritical water treatment apparatus, the direct heat generation from the reaction vessel wall surface is accurately controlled by electromagnetic induction heating control, The temperature and pressure of the subcritical water in the reaction kettle can be maintained and adjusted with high accuracy, and the conditions such as the temperature, pressure and processing time applied to the material can be set optimally.
Further, according to the second electromagnetic induction heating type subcritical water treatment apparatus according to the present invention, in the so-called continuous treatment type subcritical water treatment apparatus, the subcritical water in the predetermined temperature range and the predetermined pressure range is stably stabilized. It can be continuously supplied, and gas pressure can be applied so that the pressure in the reaction kettle does not drop during the introduction, and the extraction process of components from the material using subcritical water in the reaction kettle is performed. It can be carried out continuously under critical water conditions.

  Hereinafter, an electromagnetic induction heating type subcritical water treatment apparatus of the present invention will be described in detail based on preferred embodiments shown in the accompanying drawings. The present invention is not limited to these examples.

  Hereinafter, a configuration example of a first electromagnetic induction heating subcritical water treatment apparatus according to the present invention will be described with reference to the drawings.

The first electromagnetic induction heating type subcritical water treatment apparatus 100 is an apparatus that adapts subcritical water to a material by a so-called batch treatment method.
FIG. 1 is a conceptual diagram illustrating a configuration example of an electromagnetic induction heating subcritical water treatment apparatus 100 according to Embodiment 1 of the present invention. The electromagnetic induction heating type subcritical water treatment apparatus 100 includes a reaction kettle 50, a cooling pipe 70, an extract tank 80, and a needle valve 90.

  The reaction kettle 50 is a batch of raw materials such as biomass and liquid, and is heated and pressurized to bring the liquid into a subcritical water state. The temperature and pressure inside the kettle are accurately adjusted to the desired pressure and temperature. This is a part in which subcritical water is reacted for a desired time to extract a target useful substance.

  The reaction kettle 50 is provided with an electromagnetic induction heating mechanism 51 for adjusting and maintaining the introduced liquid at a desired pressure and a desired temperature quickly and accurately. If it is the electromagnetic induction heating mechanism 51, since it is excellent in responsiveness, the merit that temperature control is easy to be performed is acquired.

The electromagnetic induction heating mechanism 51 generates magnetic flux around the metal body, induces eddy currents inside the metal body, and directly heats the metal body. In this configuration example, a coil 52 which is an insulating film copper wire is wound around the reaction kettle 50 in a coil shape a plurality of times. Further, a current control unit (not shown) for controlling the current flowing through the coil 52 is provided.
The reaction kettle 50 is provided with a highly accurate temperature sensor and pressure sensor (not shown).

  For example, it is preferable that the control temperature of the subcritical water in the reaction vessel 50 by the electromagnetic induction heating mechanism 51 is in the range of 50 to 400 ° C. and the control pressure is adjusted to be equal to or higher than the saturated water vapor pressure. The conditions under which a useful substance can be selectively extracted from biomass without decomposing it using the subcritical water generator of the present invention are as follows: the temperature is in the range of 100 to 250 ° C., and the pressure is from 1 to the saturated water vapor pressure at that temperature. A range of 3 times is preferred.

  In this configuration example, the current flowing through the coil 52, which is an insulating film copper wire, is controlled by the current control unit, and the temperature and pressure of the subcritical water in the reaction kettle 50 are accurately adjusted by electromagnetic induction heating control. The components are extracted from the material in 50 in a short time by batch processing. In addition, the experimental example of the temperature and pressure of subcritical water with respect to the useful substance used as an extraction target, and processing time setting is mentioned later.

  The needle valve 90 is a valve for taking out from the reaction vessel 50 the extracted liquid after the reaction between the subcritical water and the material in the reaction vessel 50, and the extracted liquid is guided to the cooling pipe 70 when the needle valve 90 is opened.

The cooling pipe 70 is a device that cools the extraction liquid taken out from the reaction kettle 50 so that it can be safely taken out to the outside because it is still contained in the high-temperature and high-pressure subcritical water.
The extract tank 80 is a tank that stores the extract after being cooled by the cooling pipe 70.

  An example of extraction of useful substances using the electromagnetic induction heating subcritical water treatment apparatus 100 of the present invention having the above configuration will be shown, and excellent and accurate subcritical water treatment by the electromagnetic induction heating subcritical water treatment apparatus 100 of the present invention. Show about ability.

(Extraction experiment)
The electromagnetic induction heating type subcritical water treatment apparatus 100 of the conceptual diagram shown in FIG. 1 was actually manufactured and an extraction experiment was performed. As a material in the extraction experiment, 300 g of dried pieces of hiba from Wajima were used, and the contained hinokitiol was used as a target substance. In addition, it is estimated that about 300 to 350 mg of hinokitiol is contained in 300 g of dried hiba wood pieces.

In order to investigate the extraction conditions of hinokitiol, the temperature and pressure of subcritical water and the reaction time of subcritical water and hiba were set in various experiments.
The extraction experiment 1 was performed at five temperatures of 150 ° C., 180 ° C., 200 ° C., 230 ° C., and 250 ° C. as subcritical water temperatures. The pressure of subcritical water was set to be slightly higher than the saturated water vapor pressure at that temperature. The liquid was heated and pressurized, and when the target temperature was reached, the needle valve 90 was opened and taken out of the reaction vessel 50.

The extraction liquid collected in the extraction tank 80 in the extraction experiment 1 was observed. The observed color and odor of the extract sample are summarized in Table 1.

  As shown in [Table 1], the color became deeper as the extraction temperature increased, and a burnt odor appeared when the temperature exceeded 230 ° C. From the properties of the extract, it seems that around 200 ° C. is extracted in the best state for the human senses.

  Further, when the hibera taken out from the reaction kettle 50 after the extraction treatment was observed, the hibera became brittle when the temperature exceeded 230 ° C., and the internal structure began to be destroyed. This suggested that the wood component of the hiba was dissolved.

  That is, when subcritical water exceeds 230 degreeC, it turns out that the hydrolytic capability which supercritical water and subcritical water have becomes strong, and decomposition | disassembly and alteration of a wood component will advance. On the other hand, at 200 ° C. or lower, the concentration of wood-derived components contained in the extract seems to be thin.

  Actually, the concentration of hinokitiol contained in the subcritical water treatment extract at each temperature was measured. The measurement result of the extraction experiment 1 is shown in FIG. As shown in FIG. 2, the hinokitiol component increases as the subcritical water temperature rises to 150 ° C., 180 ° C., 200 ° C., and 230 ° C. However, when subcritical water at 250 ° C. is used, the amount of hinokitiol extracted conversely decreases. This is thought to be due to the degradation of hinokitiol due to thermal decomposition due to the properties of hinokitiol.

  From the measurement results of FIG. 2, it was found that hinokitiol was extracted most when subcritical water at 230 ° C. was used. However, as shown in Table 1, the lysis of the wood component started at 230 ° C. This is thought to be the result of more extraction of hinokitiol remaining deep inside. While more hinokitiol dissolves due to dissolution of the wood component, thermal decomposition may start as suggested by the measurement results in FIG.

  From the extraction results of FIG. 2 and the observation results of Table 1, it is good to obtain a good hinokitiol without a burning odor by using subcritical water at a temperature of 200 ° C. and a pressure slightly higher than the saturated water vapor pressure at that temperature. It turns out that it is a condition.

Next, the reaction time is verified.
Change the extraction time of the subcritical water and the material at 200 ° C (residence time in the reaction kettle of the subcritical water), take it out immediately (0 minutes), keep it for 5 minutes, take it out for 10 minutes Extraction experiment 2 was performed with three patterns of removal. FIG. 3 shows the measurement results of extraction experiment 2.

  As shown in FIG. 3, the amount of hinokitiol extracted increases as the extraction time increases to 0 minutes, 5 minutes, and 10 minutes. From this experimental result, it is understood that sub-critical water having a pressure slightly higher than the saturated water vapor pressure at 200 ° C. may be added to the reaction vessel 50 to ensure an extraction time of 10 minutes. Here, it is examined whether an extraction time of 10 minutes or more is necessary. The amount of hinokitiol contained in the extract when the extraction time of 10 minutes is taken is 336 mg, and it is estimated that about 300 to 350 mg of hinokitiol is contained in 300 g of the raw material hiba that has already been added. It can be seen that almost the entire amount of hinokitiol has been extracted. Therefore, it turns out that it is sufficient and effective if extraction time of 10 minutes or more is taken.

Next, experiments show that the temperature, pressure, and reaction time of subcritical water used for extraction differ depending on the target material to be extracted.
Extraction experiment with subcritical water is performed using Wajima hiba as the same as extraction experiment 1 and extraction experiment 2, and in this extraction experiment 3, the whole extract is distilled as it is to remove moisture, and all contained in the extract The amount of residue was measured.

In addition to hinokitiol, components extracted in the main extraction experiment 3 include cypress oil, lignin degradation products, cellulose degradation products, hemicellulose degradation products, and the like.
In the extraction experiment 3, the reaction kettle 50 is heated, and when the liquid in the reaction kettle 50 reaches subcritical states of 150 ° C., 180 ° C., 200 ° C., 230 ° C., and 250 ° C., the needle is immediately used. The valve 90 was opened and taken out, and the distillation residue amount of the extract at each temperature was measured.

FIG. 4 shows the amount of distillation residue in extraction experiment 3.
As shown in FIG. 4, the total amount of distillation residue suddenly increases when subcritical water exceeds 230 ° C.
When the properties of the distillation residue of the extract extracted with the subcritical water at 230 ° C. were examined, it was found that they were dissolved in ethanol and acetone. Substances contained in hiba that dissolve in ethanol and acetone are considered to be composed of hiba oil and lignin degradation products. That is, it can be seen that Hiba oil and lignin degradation products are not extracted with subcritical water at 200 ° C., but are extracted with subcritical water above 230 ° C.

  Next, when the distillation residue of the extract extracted with subcritical water at 250 ° C. is examined, the total amount of distillation residue decreases at 250 ° C. This is presumably because part of the extract was further decomposed at a high temperature of 250 ° C., resulting in thermal decomposition and low molecular weight. If the purpose is to extract the target substance, generation of pyrolyzate is inconvenient, and it is understood that the extraction temperature is preferably 230 ° C. or lower.

As can be seen from FIG. 4, when hinokitiol is used as the target substance, the extraction method using subcritical water at 200 ° C. is the best. Further, it is understood that the extraction method using subcritical water at 230 ° C. is the best when Hiba oil or lignin is used as a target substance.
Thus, it can be seen that the optimum extraction temperature differs depending on the target material.

  The results of extraction experiments 1, 2, and 3 can be summarized as follows: subcritical water temperature, pressure, and reaction time suitable for extraction, depending on the material and target material. It is effective to apply critical water to the material.

In the conventional subcritical water generator, it is difficult to raise the temperature of the reaction kettle 50 in a state where 1 L of water is put into the stainless steel kettle 50 having a volume of 2 L to 200 ° C. in a few minutes. Moreover, in the conventional subcritical water generator, it is difficult to control the temperature of the subcritical water in the stainless steel reaction vessel 50, and the fluctuation range is large. That is, it is difficult to keep the temperature in the stainless steel reaction vessel 50 constant at the target temperature after the temperature in the stainless steel reaction vessel 50 is raised to the target temperature.
On the other hand, the electromagnetic induction heating type subcritical water treatment apparatus 100 of the present invention directly heats the wall surface of the stainless steel reaction kettle 50 by the electromagnetic induction heating method, and can rapidly raise the temperature in a short time. Even in the reaction kettle 50, the temperature could be raised to 200 ° C. in about 5 to 6 minutes. Further, the temperature could be raised to 250 ° C. in about 10 minutes. In addition, the temperature in the reaction kettle 50 was finely controlled by electromagnetic induction heating control, so that the temperature in the reaction kettle 50 could be accurately controlled to a constant temperature.

  Although the above experiment was an extraction experiment of hinokitiol from hiba, the electromagnetic induction heating type subcritical water treatment apparatus of the present invention is not only useful for extracting useful substances from plant biomass, but also for animal biomass. It can also be applied. For example, it is possible to decompose fish scales and extract amino acids. When a hydrophilic amino acid such as serine, glutamic acid or aspartic acid was used as a target substance, it could be removed by reacting subcritical water at 200 ° C. or lower. Many hydrophilic amino acids are susceptible to thermal decomposition, and thermal decomposition occurred when reacted with subcritical water exceeding 200 ° C. When a hydrophobic amino acid such as isoleucine, leucine or glycine was used as a target substance, it could be removed without causing thermal decomposition even when subcritical water at around 250 ° C. was reacted.

  Moreover, the electromagnetic induction heating type subcritical water treatment apparatus of the present invention can be used not only for pyrolysis reaction of biomass or the like but also for various other reactions. For example, it can be used for various reactions such as hydrolysis of biomass and the like, gasification of biomass and the like, synthesis of inorganic particles, and oxidative decomposition. Even in these reactions, accurate temperature adjustment is required depending on the properties of the synthesis (reaction) product, but accurate temperature adjustment is difficult with the conventional subcritical water treatment apparatus. The heated subcritical water treatment device can adjust the subcritical water reaction temperature with high accuracy, so it can be applied to various reactions such as hydrolysis of biomass, gasification of biomass, synthesis of inorganic particles, and oxidative decomposition. be able to.

  The 2nd electromagnetic induction heating type subcritical water treatment apparatus of the present invention concerning Example 2 is explained. FIG. 5 is a conceptual diagram illustrating a configuration example of the second electromagnetic induction heating subcritical water treatment apparatus 100a of the present invention. The electromagnetic induction heating type subcritical water treatment apparatus 100a includes a distilled water tank 10, a high pressure pump 20, a subcritical water generation apparatus 30, an introduction pipe 40, a bypass pipe 41, a reaction vessel 50a, a pressurization apparatus 60, a cooling pipe 70, and an extraction. A liquid tank 80 and various valves 91 to 94 are provided. The second electromagnetic induction heating type subcritical water treatment apparatus 100a has a configuration capable of continuous treatment with respect to the supply of subcritical water.

  The distilled water tank 10 is a tank that stores distilled water, and supplies the distilled water to the subcritical water generator 30 via the high-pressure pump 20.

  The high-pressure pump 20 is a pump that sends distilled water from the distilled water tank 10 to the subcritical water generator 30.

  The subcritical water generator 30 is an apparatus that generates subcritical water by heating and pressurizing distilled water supplied from the high-pressure pump 20. The subcritical water generator 30 includes a heating mechanism (not shown) in order to bring distilled water into a subcritical state.

  The heating mechanism is not particularly limited, and an electric furnace heating mechanism, an electromagnetic induction heating mechanism, and the like are possible. However, the configuration of this embodiment is an electromagnetic induction heating mechanism. If it is an electromagnetic induction heating mechanism, the merit that quick heating is easy and the temperature control after a heating is easy to do is acquired. As will be described later, when subcritical water is introduced into the reaction vessel 50a, the material is immediately extracted in the reaction vessel 50a as a subcritical water state at a desired temperature and desired pressure within a predetermined extraction reaction time. It becomes easy.

  The introduction pipe 40 is a pipe that takes out the subcritical water that has reached the subcritical state from the subcritical water generator 30 and introduces it into the reaction vessel 50a.

  The bypass pipe 41 is a flow path provided separately from the introduction pipe 40 with respect to the subcritical water generator 30, and when the subcritical water introduced from the subcritical water generator 30 is not in the predetermined temperature range and the predetermined pressure range. In addition, when the subcritical water is in a predetermined temperature range and a predetermined pressure range, it is introduced into the reaction kettle 50a as it is through the introduction pipe 40 without being escaped by the bypass pipe 41 and introduced into the reaction kettle 50a.

  If subcritical water not in the predetermined temperature range and the predetermined pressure range enters the reaction kettle 50a, the reaction kettle 50a is not in the reaction temperature and reaction pressure, and the planned reaction process cannot be performed. End up. In the present invention, the reaction temperature and the reaction pressure are adjusted with high accuracy and reacted with the raw material to extract useful substances, so such a state is not preferable. Therefore, by providing the bypass pipe 41, the subcritical water that is not in the predetermined temperature range and the predetermined pressure range is allowed to escape to the bypass pipe 41 side so as not to enter the reaction vessel 50a. If only the subcritical water adjusted to the predetermined pressure range is introduced through the introduction pipe 40, the reaction temperature and the reaction pressure can be immediately adjusted with high accuracy by the electromagnetic induction heating mechanism 51 of the reaction vessel 50a described later.

  In order to switch between the introduction pipe 40 and the bypass pipe 41, a needle valve 91 and a needle valve 92 are provided as will be described later, and various sensors necessary for opening / closing control of the needle valve are also provided. (Not shown).

The reaction kettle 50a is charged with a material such as biomass and introduces the subcritical water generated by the subcritical water generator 30 through the introduction pipe 40, so that the subcritical water is accurately set to a desired pressure and a desired temperature. This is the part where the raw material and subcritical water are reacted for a desired time while adjusting to extract the target useful substance. In addition, it is good also as a structure provided with the feeder apparatus which throws in a predetermined amount of raw material.
Moreover, in the structure of the electromagnetic induction heating type subcritical water treatment apparatus according to the present invention, a plurality of reaction kettles can be arranged in parallel and the extraction process can be performed by a switching operation. In addition, reaction kettles can be arranged in series according to the purpose of the treatment. Furthermore, the positions of the inlet and outlet of the subcritical water can be appropriately selected from any of the upper part, the lower part, and the side part of the reaction kettle.

As in the first embodiment, the reaction vessel 50a includes an electromagnetic induction heating mechanism 51 for accurately adjusting and maintaining the subcritical water introduced from the subcritical water generator 30 at a desired pressure and a desired temperature. ing. In this configuration example, a coil 52, which is an insulating film copper wire, is wound around the reaction kettle 50a a plurality of times. Further, similarly to the first embodiment, a current control unit (not shown) for controlling the current flowing through the coil 52 is provided.
As in the first embodiment, a highly accurate temperature sensor and pressure sensor are also provided in the reaction kettle 50a (not shown).

  Also in the second embodiment, for example, it is preferable that the control temperature of the subcritical water in the reaction vessel 50a by the electromagnetic induction heating mechanism 51 is in the range of 50 to 400 ° C. and the control pressure is adjusted to be equal to or higher than the saturated water vapor pressure.

  In the configuration example of the second embodiment, subcritical water is generated by the subcritical water generator 30, the subcritical water is continuously flowed into the reaction vessel 50 a, and the current of the coil 52 is controlled by the current control unit. The temperature and pressure of the subcritical water passing through the reaction vessel 50a are adjusted with high accuracy by electromagnetic induction heating control, and the extract obtained by reacting with the raw material is continuously flowed out.

  The pressurizing device 60 adjusts the gas pressure for maintaining the pressure in the reaction kettle 50a to be equal to or higher than the saturated water vapor pressure when the subcritical water is introduced into the reaction kettle 50a from the subcritical water generator 30 through the introduction pipe 40. It is a device that can be applied to the reaction vessel 50a. For example, a gas cylinder that supplies an inert gas (such as nitrogen gas) and a booster that applies the inert gas from the gas cylinder to the reaction kettle at a predetermined pressure are provided. In order to maintain the subcritical water state, a pressure higher than the saturated water vapor pressure is required, but the gas cylinder pressure is about 10 MPa even at the highest pressure, and it is difficult to supply high-pressure gas that exceeds the pressure of the gas cylinder alone. It is preferable to have an apparatus.

  Even in the continuous treatment, since it is necessary to maintain a predetermined pressure at a predetermined temperature in the reaction vessel 50a, a needle valve 91 which will be described later is introduced when the subcritical water generated in the subcritical water generator 30 is introduced into the reaction vessel 50a. However, the pressure may drop below the saturated water vapor pressure. At this time, a gas pressure is applied by the pressurizing device 60 in order to immediately correct and adjust the pressure in the reaction vessel 50a to the saturated water vapor pressure or higher.

The cooling pipe 70 is a device for cooling because the extract taken out from the reaction kettle 50 is still contained in the high-temperature and high-pressure subcritical water.
The extract tank 80 is a tank that stores the extract after being cooled by the cooling pipe 70.

  The needle valve 91 is a valve that controls conduction between the introduction path 40 and the reaction vessel 50a. The needle valve 92 is a valve that controls conduction between the introduction path 40 and the bypass path 41. The introduction pipe 40 near the needle valve 91 is provided with a highly accurate temperature sensor and pressure sensor (not shown), and the opening / closing of the needle valve 91 and the needle valve 92 is controlled by a valve opening / closing control unit (not shown). .

  When the temperature and pressure of the subcritical water in the introduction pipe 40 are within a predetermined range, the needle valve 91 is opened and the needle valve 92 is closed, and the subcritical water generated in the subcritical water generator 30 is guided to the reaction kettle 50a. . When the temperature and pressure of the subcritical water in the introduction pipe 40 are not within the predetermined ranges, the needle valve 91 is closed and the needle valve 92 is opened, and the subcritical water generated by the subcritical water generator 30 is externally supplied from the bypass pipe 41. To escape.

  The needle valve 93 is a valve that controls conduction between the pressurizing device 60 and the reaction vessel 50a, and immediately corrects and adjusts the pressure in the reaction vessel 50a so that the pressure in the reaction vessel 50a becomes equal to or higher than the saturated water vapor pressure. If the pressure sensor (not shown) in the reaction vessel 50a causes the pressure in the reaction vessel 50a to fall below the saturated water vapor pressure as the needle valve 91 is opened, the subcritical water becomes water vapor. In conjunction with the opening of the valve 91, the needle valve 93 is opened, and nitrogen gas is applied from the pressurized gas cylinder 60 so that the pressure in the reaction vessel 50a becomes equal to or higher than the saturated water vapor pressure, and the subcritical state is maintained.

In the first embodiment, the needle valve 90 is provided, and the extraction of the extracted liquid from the reaction kettle 50 after the batch processing is controlled. However, the second embodiment is a continuous processing and corresponds to the needle valve 90. May be unnecessary. In the second embodiment, the needle valve 90 is not provided.
Instead, a control valve 94 is provided behind the cooling pipe 70. If the control valve 94 is provided, a merit that the pressure can be made constant automatically is obtained. For example, even when the valve becomes clogged due to the influence of insoluble components (pressure increases), the control valve 94 can be automatically opened and discharged, so that the pressure can be kept constant.

  As described above, according to the second electromagnetic induction heating type subcritical water treatment apparatus of the present invention, in a so-called continuous treatment type subcritical water treatment apparatus, subcritical water in a predetermined temperature range and a predetermined pressure range is stably and continuously supplied. Gas can be applied so that the pressure in the reaction kettle does not drop during the introduction, and the component extraction process from the material using subcritical water in the reaction kettle is continuous. It can be.

As an electromagnetic induction heating type subcritical water treatment apparatus of Example 3, an example incorporating a device for effectively preventing seizure of a coil which is an insulating film copper wire will be described.
In Example 3, a heat insulator is wound around the reaction kettle, and the insulation film copper wire is wound around the reaction kettle around the reaction kettle, and the insulation film copper wire is seized as a heat buffer. This is to prevent this.
The overall configuration of the electromagnetic induction heating subcritical water treatment apparatus according to the third embodiment may be the same as the apparatus configuration shown in the first embodiment, but the reaction kettle 50b is devised.

FIG. 6 is a diagram schematically showing the shape of the heat insulator around the reaction kettle 50b.
A heat insulator 53 is wound around the reaction kettle 50b. The heat insulator 53 functions as a heat buffer, and is designed to prevent heat conduction from the extraction pot to the insulating coating copper wire 52 at the same time as the temperature of the extraction pot 50 itself is kept. Further, the heat insulating material 53 also functions to prevent the insulating film copper wire 52 wound in a coil shape from coming into contact with the outer surface of the extraction pot 50.

  In the third embodiment, a large number of groove structures 54 are provided on the outer peripheral surface of the heat insulating body 53, a cooling fan (not shown) for flowing cooling air is provided along the groove structure 54, and the reaction vessel 50 b is formed by the heat insulating body 53. The coil-shaped insulating film copper wire 52 is cooled outside the heat insulator 53 while keeping the temperature.

  FIG. 6 is a cross-sectional view schematically showing the relationship between the numerous groove structures 54 and the coil 52, which is an insulating film copper wire, on the outer peripheral surface of the heat insulator 53.

  Since the groove structure 54 is provided on the outer peripheral surface of the heat insulator 53, the coil 52, which is an insulating film copper wire, does not adhere to the heat insulator 53 and a passage through which air passes is secured. When the cooling fan blows air to the gap of the groove structure 54, the heat conducted from the reaction kettle 50b can be effectively dissipated, and the insulating film will not be burned or burnt.

  As an electromagnetic induction heating type subcritical water treatment apparatus of Example 4, a vortex generated in a metal protrusion by surrounding a metal protrusion such as a bolt provided in a reaction kettle with a magnetic material and shielding leakage magnetic flux. An embodiment incorporating a device for reducing current will be described.

  FIG. 7 is a longitudinal sectional view showing only the reaction kettle 50c of the electromagnetic induction heating type subcritical water treatment apparatus taken out and shown in a longitudinal section.

When a current flows through the coil 52, which is an insulating film copper wire, a magnetic field is generated, and the magnetic flux becomes a leakage flux, and the magnetic flux passes through and around the wall surface of the reaction vessel 50c. Here, the reaction kettle 50c has a large bolt 55 that closes the kettle lid, but magnetic flux tends to concentrate on the tip of the bolt 55, and eddy current tends to occur. Therefore, seizure is likely to occur at the tip of the bolt 55.
Therefore, in the electromagnetic induction heating type subcritical water treatment apparatus of the fourth embodiment, magnetic flux is easily concentrated and metal protrusions that are likely to generate eddy current are surrounded by a magnetic material to prevent the passage of magnetic flux, thereby generating eddy current. Further, overheating is prevented.

  As shown in FIG. 7, a magnetic body 56 is provided so as to block the tip of the bolt 55. For example, a ferrite core may be used.

  Although the magnetic lines of force are not shown in FIG. 7, the magnetic lines of force generated from the current flowing through the coil 52, which is an insulating film copper wire, converge in the direction of the magnetic body 56, which is a ferrite core. Magnetic field lines do not pass through and no excessive eddy currents are generated.

  As mentioned above, although preferred embodiment in the example of composition of the electromagnetic induction heating type subcritical water treatment device of the present invention was illustrated and explained, various changes are possible without deviating from the technical scope of the present invention. Will be understood.

  The electromagnetic induction heating subcritical water treatment apparatus of the present invention can be widely applied to subcritical water treatment apparatuses for extracting useful substances from biomass such as plant tissues and animal tissues using subcritical water.

The conceptual diagram which illustrates one structural example of the electromagnetic induction heating type subcritical water processing apparatus 100 which concerns on Example 1 of this invention. The figure which shows the measurement result of extraction experiment 1 The figure which shows the measurement result of the extraction experiment 2 The figure which shows the evaporation residue amount of the extraction experiment 3 The conceptual diagram which illustrates one structural example of the electromagnetic induction heating type subcritical water processing apparatus 100a which concerns on Example 2 of this invention. Cross section schematically showing the heat insulator 52 around the reaction vessel 50b, the groove structure 53 provided on the outer peripheral surface thereof, and the insulating coating copper wire 51 Longitudinal cross section schematically showing bolt 55 of reaction kettle 50c and magnetic body 56 covering it

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 Distilled water tank 20 High pressure pump 30 Subcritical water generator 40 Introducing pipe 41 Bypass pipe 50 Reaction kettle 51 Electromagnetic induction heating mechanism 52 Insulation film copper wire 53 Insulation body 54 Groove structure 55 Bolt 56 Magnetic body 60 Pressurized gas cylinder 70 Cooling pipe 80 Extract liquid tank 90, 91, 92, 93 Needle valve 94 Control valve

Claims (8)

A reaction kettle that pressurizes and heats the liquid put into the kettle to a subcritical state, and reacts the material put into the kettle with the subcritical water;
A coil wound a plurality of times around the reaction kettle;
A current control unit for controlling a current flowing through the coil;
The current control unit controls the current flowing through the coil, and the temperature and pressure of the subcritical water in the reaction kettle are accurately adjusted by electromagnetic induction heating control, and the material in the reaction kettle and the subcritical water are controlled. An electromagnetic induction heating type subcritical water treatment apparatus characterized by reacting water in a short time. A subcritical water generator for generating subcritical water;
An introduction pipe for taking out subcritical water that has reached a subcritical state from the subcritical water generator;
A reaction kettle for introducing the subcritical water from the introduction pipe and reacting the material introduced into the kettle with the subcritical water;
A coil wound a plurality of times around the reaction kettle;
A current control unit for controlling a current flowing through the coil;
The current control unit controls the current flowing through the coil, and the temperature and pressure of the subcritical water flowing in the reaction kettle are accurately adjusted by electromagnetic induction heating control. An electromagnetic induction heating type subcritical water treatment apparatus characterized by reacting critical water in a short time.   A heat insulator is wound around the reaction kettle, and the coil is wound around the reaction kettle with the heat insulator sandwiched therebetween to prevent seizure of the coil as a heat buffer material. Item 3. The electromagnetic induction heating subcritical water treatment apparatus according to Item 1 or 2.   A plurality of groove structures are provided on the outer peripheral surface of the heat insulator, cooling means for flowing cooling air along the groove structure is provided, and the reaction kettle cools the coil outside the heat insulator while keeping heat by the heat insulator. The electromagnetic induction heating type subcritical water treatment apparatus according to any one of claims 1 to 3, which has a caulking structure.   The metal protrusion such as a bolt provided in the reaction kettle is surrounded by a magnetic material to shield leakage magnetic flux and reduce eddy current generated in the metal protrusion. The electromagnetic induction heating type subcritical water treatment apparatus according to any one of 4.   The electromagnetic induction heating method according to any one of claims 1 to 5, wherein a control temperature of the subcritical water in the reaction kettle by the electromagnetic induction heating control is 50 to 400 ° C, and a control pressure is equal to or higher than a saturated water vapor pressure. Subcritical water treatment equipment.   The reaction process with the material using the subcritical water in the reaction kettle is a continuous process, and a bypass pipe is provided in the subcritical water generator separately from the introduction pipe, and introduced from the subcritical water generator. When the subcritical water is not in a predetermined temperature range and a predetermined pressure range, it is released by the bypass pipe, and when it is in the predetermined temperature range and the predetermined pressure range, it is introduced into the reaction kettle through the introduction pipe. The electromagnetic induction heating type subcritical water treatment apparatus according to claim 2.   When introducing the subcritical water from the subcritical water generator into the reaction kettle through the introduction pipe, a gas pressure is maintained in the reaction kettle to keep the pressure in the reaction kettle above the saturated water vapor pressure. The electromagnetic induction heating type subcritical water treatment apparatus according to claim 7, further comprising a pressurizing means that can be applied.

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