JP6836046B1 - Subcritical or supercritical continuous processing equipment and methods for organic substances - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method, an apparatus and a system capable of semi-continuously processing subcritical / supercritical processing. SOLUTION: One or a plurality of kinds of solid raw materials to be subjected to subcritical / supercritical treatment are crushed and mixed as they are, or are mixed with a fluid raw material and then charged, and the raw materials are received from a pretreatment pressure vessel and a pretreatment pressure vessel connected to a hopper. The first is a treatment step in which the treatment material is held in the subcritical / supercritical state in the primary main treatment pressure vessel, and a part of the treatment material in the primary subcritical / supercritical treatment completion state is extracted. The step of transferring the fluid into the secondary treatment pressure vessel and temporarily holding it, the step of replenishing the same amount of the same amount of the processed material as the extracted treatment material from the pretreatment pressure vessel into the primary main treatment pressure vessel, and the above-mentioned extraction. Including the step of post-treating the fluid in the secondary treatment pressure vessel or the step of discharging it to the main treatment material receiving vessel as it is, the decrease in pressure and temperature of the primary main treatment pressure vessel caused by extraction A quasi-continuous method in which raw materials are subcritically or supercritically treated and post-treated, which is a means for adjusting. It also includes an IoTAI control management system for smooth subcritical / supercritical processing and quasi-continuity. [Selection diagram] Fig. 1

Description

The present invention relates to inorganic substances such as soil and rocks, municipal waste, kitchen waste, livestock manure, sewage sludge, organic composite sludge such as dams, lakes, moats and coasts, plant residues, thinned wood, clothing, and organic substances such as plastics. The present invention relates to a semi-continuous method of critical / supercritical processing and subsequent processing, and an apparatus and system thereof.

Subcritical / supercritical treatments and post-treatments have been used for various purposes such as treatment of biomass, plastics, soil, sewage sludge, and plant residues. The equipment for subcritical / supercritical processing is mainly a batch type, and it returns to normal temperature and pressure by discharging and post-processing. Therefore, it was necessary to raise and raise the temperature of the next raw material to the subcritical / supercritical state again.
Therefore, after the processing of the subcritical / supercritical device, it takes time to add the raw material and change the temperature and pressure to the subcritical / supercritical temperature pressure again before the next processing, and the raw materials are continuously used. Could not be processed. For example, in the case of saccharification treatment by subcritical treatment of 10 tons of biomass per batch, the subcritical treatment time is 30 minutes, but it takes 2 hours to perform the next treatment including pre- and post-treatment.
In addition, it is difficult to respond to a wide range of raw materials immediately by batch-type, and there is a situation where it has to be a one-off business development, and even in research and development at universities etc., it takes a lot of time to grasp and summarize the events. It was also a factor that required.

This meant that mass processing was not possible, and that subcritical / supercritical processing was not industrially profitable unless it was expensive. However, waste plastics such as soil / rocks, municipal waste, kitchen waste, sewage sludge, and plant residues have become a global problem these days, and it is necessary to efficiently carry out subcritical / supercritical treatment and subsequent treatment for mass treatment. Is occurring.

Japanese Patent No. 5032713

The above-mentioned problems are not limited to the combined process processing in the batch processing process, and in the case of discharge after the processing, the temperature returns to room temperature, and it is necessary to raise the temperature to a predetermined temperature again. .. Moreover, this problem is not limited to hydrothermal treatment, but is a problem that occurs widely when subcritical / supercritical reactions are used. That is, in order to perform the next treatment, it is necessary to put the fluid to be subcritical / supercritical after lowering the temperature in the reactor and the next raw material into the device, and then heat and pressurize the raw material. It could not be processed continuously.
The present invention solves the above problems and provides equipment and a method capable of continuously processing raw materials.

The present invention connects a processing object supply device that supplies a treatment object containing an organic substance, a heated water supply device that supplies subcritical or supercritical water, and the treatment object supply device via a distribution control means. A pretreatment pressure vessel for mixing and stirring the treatment target supplied from the treatment target supply device and the subcritical or supercritical water supplied from the heated water supply device, and the pretreatment pressure. First, the container is connected to the vessel via a flow control means, and the treatment object discharged from the pretreatment pressure vessel and the subcritical or supercritical water supplied from the heated water supply device are mixed and stirred. The next treatment pressure vessel and the primary treatment pressure vessel are connected to each other via a flow control means, and are supplied from the treatment target discharged from the primary treatment pressure vessel and the heated water supply device. By controlling the pressure of each of the secondary treatment pressure vessel, the pretreatment pressure vessel to the secondary treatment pressure vessel, and the flow control means for mixing and stirring the subcritical or supercritical water. , Automatic transportation of the object to be treated from the pretreatment pressure vessel to the secondary treatment pressure vessel while performing mixing and stirring treatment in each of the pretreatment pressure vessel and the secondary treatment pressure vessel in parallel. It is a subcritical or supercritical continuous processing facility for organic substances, which is provided with a control means for performing the operation.

Further, the present invention comprises a step of mixing and stirring a treatment target containing an organic substance and subcritical or supercritical water using a pretreatment pressure vessel, and a treatment target discharged from the pretreatment pressure vessel. A step of mixing and stirring subcritical or supercritical water using a primary treatment pressure vessel, and a second treatment object discharged from the primary treatment pressure vessel and subcritical or supercritical water. By controlling the respective pressures of the pretreatment pressure vessel, the primary treatment pressure vessel, and the secondary treatment pressure vessel in the step of mixing and stirring using the secondary treatment pressure vessel, in those treatment pressure vessels. The subcriticality of the organic substance is characterized by including a step of automatically transporting the treatment object from the pretreatment pressure vessel to the secondary treatment pressure vessel while performing the mixing and stirring treatment of the treatment target in parallel. Alternatively, it is a supercritical continuous processing method.

In the conventional method of subcritical / supercritical treatment and post-treatment, even if the next raw material and fluid are post-treated, the gas of the post-treatment residue of the previous raw material has a thermal conductivity of gas even if the temperature is lowered. It is low and difficult to lower. On the other hand, in the case of the method according to the present invention, the next post-treatment does not require lowering the temperature of the post-treatment device, and a part of the object to be treated in the subcritical / supercritical state is extracted. Can be post-treated as it is, or by slightly heating and pressurizing. Therefore, since it is not necessary to lower the temperature, the treatment can be performed continuously as compared with the conventional case.

Furthermore, when replenishing the primary treatment pressure vessel with the same amount of material as the extracted object to be treated from the pretreatment pressure vessel, the replenished material must be at normal temperature or close to normal temperature. Even if it is replenished, it can be replenished by heating and pressurizing in advance in the pretreatment pressure vessel, so the inside of the primary treatment pressure vessel is maintained in the subcritical / supercritical state and the treatment is continuous. You can.

In addition, in the conventional pressure vessel, it was necessary to lower the temperature to room temperature or a temperature close to it and then raise the temperature to subcritical / supercritical temperatures, whereas in the case of the present invention, the object to be treated was extracted. As a result, the temperature and pressure will drop slightly, but the pressure and temperature drop time will be short.

Whether the post-treatment is a subcritical supercritical treatment with different conditions from the subcritical supercritical treatment of the primary treatment pressure vessel, blasting treatment, or discharge as it is, the secondary treatment pressure at some point. The pressure release side of the vessel comes into contact with the atmosphere. However, since the secondary pressure vessel is under high pressure during the post-treatment in the secondary treatment pressure vessel, there is no room for air to enter. Also, as soon as the discharge is completed, the valve between the high pressure side and the low pressure side is closed, so the time for the atmosphere to enter is short. Even if the atmosphere flows into the secondary treatment pressure vessel, the pressure of the subcritical / supercritical fluid sent from the primary treatment pressure vessel is high, so the atmosphere is compressed to a small volume.

When the influence of oxygen is disliked, the valve may be closed when the pressure of the fluid in the post-treatment is higher than the normal pressure to some extent. Moreover, the time of contact between the atmosphere and the subcritical / supercritical fluid in the secondary treatment pressure vessel is short. Therefore, the influence of the atmosphere is almost negligible. As described above, in the present invention, subcritical / supercritical treatment and post-treatment can be performed without being affected by the atmosphere and oxygen without lowering to room temperature.

If the post-treatment is to slowly reduce the pressure, the rate-determining factor for continuous treatment should be the post-treatment, but in such a case, multiple secondary treatment pressure vessels should be provided. Therefore, the total processing time can be speeded up and can be performed continuously.

It is a block diagram which shows the basic part of this invention. It is an overall block diagram of this invention.

Hereinafter, embodiments of the present invention will be described with reference to FIG.

As shown in FIG. 1, the subcritical or supercritical continuous treatment equipment includes a treatment target supply device 11 for supplying a treatment target containing an organic substance and a heated water supply device 5 for supplying subcritical or supercritical water. , Subcritical or subcritical, which is connected to the treatment object supply device 11 via a flow control means 12 such as a valve, and the treatment target supplied from the waste supply device 11 and the heated water supply device 5. The pretreatment pressure vessel 1 for mixing and stirring the supercritical water and the pretreatment pressure vessel 1 are connected to the pretreatment pressure vessel 1 via the flow control means 12, and the treatment object discharged from the pretreatment pressure vessel 1 and the heated water are supplied. The primary treatment pressure vessel 2 for mixing and stirring the subcritical or supercritical water supplied from the apparatus 5 and the primary treatment pressure vessel 1 are connected to the primary treatment pressure vessel 1 via the flow control means 12, and are primary. The secondary treatment pressure vessel 3 for mixing and stirring the treatment object discharged from the treatment pressure vessel 2 and the subcritical or supercritical water supplied from the heated water supply device 5, and the pretreatment pressure vessels 1 to 1 By controlling each pressure of the secondary treatment pressure vessel 3 and each of the flow control means 12, the mixing and stirring treatment in each of the pretreatment pressure vessel 1 to the secondary treatment pressure vessel 3 is carried out in parallel. At the same time, the control means 8 for automatically transporting the processing object from the pretreatment pressure vessel 1 to the secondary treatment pressure vessel 3 is provided. The treatment conditions such as the treatment temperature and the pressure may be different for each of the pretreatment pressure vessel 1 and the secondary treatment pressure vessel, but the treatment time is basically the same.

The object to be treated includes one or more kinds of organic substances such as wood, bamboo, construction waste, plastic, euglena, sludge, radioactive waste, municipal waste, industrial waste, agricultural, fishery and livestock waste, and the object to be treated. The supply device 11 includes a crusher, a hopper, a kneader, and the like.
The object to be processed is crushed and refined so as to be easily put into the pretreatment pressure vessel 1. The amount to be charged into the pretreatment pressure vessel 1 can be calculated by a method of directly measuring and a method of determining the amount to be replenished from the physical properties that fluctuate with the extraction of pressure or the like.

The pretreatment pressure vessel 1 is an apparatus for mixing and stirring a treatment object and subcritical or supercritical water to form a slurry. The processing temperature and pressure for that purpose may be, for example, 100 to 200 ° C. and 2 to 25 atm. An opening / closing door 13 is provided at the inlet of the pretreatment pressure vessel 1. Further, the distribution control means 12 on the downstream side of the discharge port may be provided with a high-pressure pump 34 made of a gear pump or the like. Then, the object to be processed can be easily sent to the primary processing pressure vessel 2 held in the high-pressure subcritical / supercritical state. The distribution control means 12 can be configured only by the high pressure pump 34 without using a valve.
The primary treatment pressure vessel 2 is an apparatus for hydrolyzing and saccharifying the object to be treated, and has the highest temperature and pressure among the pretreatment pressure vessel 1 to the secondary treatment pressure vessel 3. For example, the processing temperature and pressure may be, for example, 150 to 600 ° C. and 2 to 25 atm.
The secondary treatment pressure vessel 3 is an apparatus for performing additional hydrolysis, saccharification, and temporary storage of the object to be treated. The processing temperature and pressure for that purpose may be equal to or lower than those of the primary processing pressure vessel 2. A pressure release valve 4 is provided on the downstream side of the discharge port of the secondary treatment pressure vessel 3.

The pressure release valve 4 causes the processing object once held in the secondary processing pressure vessel 3 to flow into the receiving tank container 5. The pressure release valve 4 may explode the solid raw material by releasing the vitality of the ball valve in an instant, or may gradually reduce the pressure by releasing the pressure release valve 4 little by little.
The heated water supply device 5 is composed of a gas boiler, an electric boiler, and the like, but a pressurizing pump 31 may be further combined. The pressurizing pump 31 is very effective in quickly recovering the drop in pressure when the object to be treated is discharged from the pretreatment pressure vessel 1 to the secondary treatment pressure vessel 3.
The receiving tank container 5 may be provided with a solid-liquid separating device 6 as needed.

As the control means 8, for advanced equipment management, an IoTAI controller is used to perform remote network AI management control, and a chemical change sensor is placed at an appropriate position in the pretreatment pressure vessel 1 to the secondary treatment pressure vessel 3. It is advisable to install 7 mag.

The control means 8 performs the mixing and stirring process in parallel in each of the pretreatment pressure vessel 1 to the secondary treatment pressure vessel 3 while maintaining the temperature and pressure as described above, and the pretreatment pressure vessel 1 to the second Next processing The automatic transportation of the processing object up to the pressure vessel 3 is performed. This automatic transportation can be easily realized by temporarily increasing the pressure of the pressure vessel of the transportation source to be higher than the pressure of the pressure vessel of the transportation destination.

In parallel implementation of the mixing and stirring treatment in each of the pretreatment pressure vessel 1 to the secondary treatment pressure vessel 3, there is a method of heating and pressurizing both the primary treatment pressure vessel and the secondary treatment pressure vessel. .. As another method, there is also a method of heating and pressurizing the primary treatment pressure vessel 2 so that the temperature and pressure become desired when the vessel is transferred to the secondary treatment pressure vessel 3. In this method, the primary processing pressure vessel 2 may be heated and pressurized higher than the desired temperature and pressure so that the object to be processed sent to the secondary processing pressure vessel 3 has a desired temperature and pressure. ..

Alternatively, considering that the object to be treated is held in the primary treatment pressure vessel 2 for a long time, the primary treatment pressure vessel 2 is set to a desired temperature and pressure, and the temperature and pressure of the secondary treatment pressure vessel 3 are set. Sometimes you don't have to worry about it. Further, as another method, when the primary treatment pressure vessel 2 is replenished with the same amount as the extracted object to be processed, not only the quantity but also the temperature and pressure are extracted. There is also a method of replenishing the primary treatment pressure vessel 2 with the one previously heated and pressurized in the pretreatment pressure vessel 1 so as to have the same level as the above.

Which one to take depends on whether the size of the primary treatment pressure vessel can be physically made sufficiently wider than that of the secondary treatment pressure vessel, and the raw material may be left at a high temperature for a long time. It depends on whether or not the difference in temperature and pressure between the primary treatment pressure vessel and the secondary treatment pressure vessel affects the post-treatment, and one of the methods is appropriately selected. Note that these methods may be used in combination.

As described above, in the present invention, the treatment of mixing and stirring the same object to be treated containing an organic substance and subcritical or supercritical water is performed under different conditions in each of a plurality of pressure vessels connected in series. It is characterized in that it is carried out in order. This enables subcritical or supercritical continuous treatment of organic substances, shortens the treatment time, and can be expected to extend the life of the pressure vessel by suppressing changes in temperature and pressure of each pressure vessel.

The subcritical / supercritical fluid is described in the example of water, but it is clear that the same applies to subcritical / supercritical fluids other than water.

Specific examples and the like will be described below, but the present invention is not limited thereto.
As shown in FIG. 1, a raw material supply hopper 11 for high-speed saccharification of municipal waste and other biomass resources into fuel or organic fertilizer, a boiler for heated steam 5, a pressure pump 31, a pretreatment pressure vessel 1, a first A semi-continuous facility was used in which a secondary treatment pressure vessel 2, a secondary treatment pressure vessel 3, and a solid-liquid separator 6 were deployed, and a treatment condition and a valve control system were constructed by an IoTAI controller 8.
In the conventional 15 m2 batch type equipment, it took 2 hours to saccharify municipal waste and other biomass resources, but the equipment according to the present invention can process 3.5 times in the same time.
The equipment according to the present invention is a plant in which two pressure vessels are added as compared with the conventional batch type processing equipment, but the size of the equipment is increased by 10%, and most of the peripheral equipment including the control management system is used. Since they are the same, it has been demonstrated that the economic efficiency can be increased 2.5 to 3 times.
In addition, the life of the pressure vessel was affected by repeating subcritical supercritical from normal temperature and pressure each time the batch type equipment was processed, but the equipment according to the present invention is expected to be significantly improved and can be used for 20 years or more. It is possible. In other words, the combined merit of increasing the economic effect and extending the operating life has been clarified.

In Fig. 2, the IoT AI network is used to sequentially manage the generation of biomass resources in the region to facilitate fluidity, determine the content of resources when resources are aggregated and mixed, and the amount input to the subcritical supercritical processing plant. Adjustment, subcritical supercritical treatment conditions are managed by AI, and the process of converting subcritical supercritical treated materials into methane gas, ethanol, solid fuel, power generation, and organic fertilizer for distribution are comprehensively properly managed. Provide a system to do.

1 Pretreatment pressure vessel 2 Primary treatment pressure vessel 3 Secondary treatment pressure vessel 5 Heated water supply device 6 Solid-liquid separation device 8 Control means 11 Treatment target supply device 12 Flow control means (valve)
34 high pressure pump

Claims (5)

A processing object supply device that supplies a processing object containing an organic substance,
A heated water supply device that supplies subcritical or supercritical water,
It is connected via a flow control means to said processing object feeder, a subcritical or supercritical water has been supplied to the processing object that has been supplied from the processing object supply device from the heating water supply device Mix and stir with a pretreatment pressure vessel,
The pretreatment pressure vessel is connected to the pretreatment pressure vessel via a flow control means, and the treatment object discharged from the pretreatment pressure vessel and the subcritical or supercritical water supplied from the heated water supply device are mixed. The primary treatment pressure vessel to be agitated and
The primary treatment pressure vessel is connected to the primary treatment pressure vessel via a flow control means, and the treatment object discharged from the primary treatment pressure vessel and the subcritical or supercritical water supplied from the heated water supply device. A secondary treatment pressure vessel that mixes and stirs water,
By controlling the pressure of each of the pretreatment pressure vessel to the secondary treatment pressure vessel and each of the flow control means, the mixing and stirring treatment in each of the pretreatment pressure vessel to the secondary treatment pressure vessel is performed. The subcritical or supercritical organic material is provided with a control means for automatically transporting the processing object from the pretreatment pressure vessel to the secondary treatment pressure vessel while carrying out the above in parallel. Continuous processing equipment. According to claim 1, a solid-liquid separation device which is connected to the secondary treatment pressure vessel via a flow control means and solid-liquid separates the treatment object discharged from the secondary treatment pressure vessel is further provided. A subcritical or supercritical continuous processing facility for organic substances, which is characterized by being equipped. The subcritical or supercritical continuous processing equipment for organic substances according to claim 1 or 2, wherein each of the distribution control means is composed of any one or a combination of a valve and a high pressure pump. A step of mixing and stirring a treatment target containing an organic substance and subcritical or supercritical water using a pretreatment pressure vessel.
A step of mixing and stirring the treatment object discharged from the pretreatment pressure vessel and subcritical or supercritical water using the primary treatment pressure vessel.
A step of mixing and stirring the treatment object discharged from the primary treatment pressure vessel and subcritical or supercritical water using the secondary treatment pressure vessel.
By controlling the pressures of the pretreatment pressure vessel, the primary treatment pressure vessel, and the secondary treatment pressure vessel, the mixing and stirring treatment of the objects to be treated in those treatment pressure vessels is carried out in parallel. However, a subcritical or supercritical continuous treatment method for organic substances, which comprises a step of automatically transporting a treatment object from the pretreatment pressure vessel to the secondary treatment pressure vessel. In claim 4, the pretreatment pressure vessel, the primary treatment pressure vessel, and the treatment in which the same treatment object containing the organic substance and subcritical or supercritical water are mixed and stirred in series are connected in series. Secondary treatment A subcritical or supercritical continuous treatment method for organic substances, which is carried out in order in each of the pressure vessels under different conditions.

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