JP4365170B2 - Method of supplying material to be processed in reaction device of organic substance by supercritical fluid or subcritical fluid - Google Patents

Description

The present invention relates to treated material supplying method in repeat cyclically compressed and expanded reactor organic matter with supercritical fluid or subcritical fluid. Specifically, by the supercritical fluid or subcritical fluid that supplies the material to be processed without causing the material of the material to be introduced into the reaction chamber or the like in the reaction apparatus to bite the seat portion of the intake valve or the spray valve. it relates workpiece supply method in the reactor of the organic matter.

  As a treatment method for materials to be treated such as organic substances such as biomass, a method and apparatus for decomposition with supercritical water or subcritical water has been developed in place of the former chemical oxidation method, photooxidation method and combustion method. (Patent Document 1).

  Furthermore, as a method for reacting a material to be treated such as an organic substance with a supercritical fluid or a subcritical fluid, for example, supercritical water under a critical condition of water, that is, a critical temperature of 374 ° C. and a critical pressure exceeding 218 atm. A method of decomposing a material to be treated such as paraffinic hydrocarbon and benzene, which can be controlled by the temperature and pressure, is also known (Patent Document 2).

  In Patent Document 2, for example, by maintaining a supercritical or subcritical state by rapidly heating a high-pressure fluid in which an organic substance such as wood powder as a material to be treated is dispersed, the supercritical or subcritical fluid vapor is maintained. A reaction apparatus capable of causing saccharification reaction of wood flour or the like to sugar by a chemical reaction in a state is disclosed. That is, a means for compressing to obtain a supercritical fluid or subcritical fluid, a means for bringing the supercritical fluid or subcritical fluid into contact with a material to be treated such as an organic substance, and a chemical reaction, and a production generated by the chemical reaction It is a reaction apparatus comprising means for expanding and depressurizing a fluid containing an object.

  Furthermore, in Patent Document 2, a means for obtaining a supercritical fluid or subcritical fluid by compressing fluid vapor, and a chemical reaction is performed by bringing the supercritical fluid or subcritical fluid into contact with a material to be treated such as an organic substance. And a cylinder and a piston (compression plunger) provided in the cylinder as a means for expanding and depressurizing the fluid containing the product generated by the chemical reaction, and operating the piston (compression plunger) After the chemical reaction is completed, the fluid vapor is compressed, and the piston (compression plunger) is operated in the opposite direction to lower the temperature and pressure. The fluid containing the obtained product is taken out from the cylinder and new fluid vapor is removed from the cylinder. A method and apparatus for operating periodically by blowing into it are disclosed.

On the other hand, in a reaction apparatus such as an organic substance using a supercritical fluid or a subcritical fluid, it is important how the material to be treated is uniformly dispersed in the supercritical fluid or the subcritical fluid. In order to disperse and introduce the material to be treated into the cylinder, the material to be treated is introduced into the rotary feeder and at the same time pressurized water is fed, and the material to be treated is injected and reacted by the rotary feeder while diffusing the material to be treated in the rotary feeder. Although it is shown that it is supplied indoors, details of the feeder section and the like are not shown.
Japanese Patent Publication No. 1-38532 JP 2002-263465 A

  In a conventional reaction apparatus, if a material to be treated such as an organic substance is to be introduced directly into a reaction vessel of the supercritical fluid or subcritical fluid, the material to be treated must be injected into the reaction chamber using a high-pressure pump. However, in the case of the conventional reaction apparatus, the material to be processed is bitten by the sheet portion of the injection valve in the supply nozzle, or the material to be processed is separated from the fluid when the material to be processed is supplied to the rotary feeder. It becomes difficult to disperse a certain amount of the material to be treated uniformly every time in the reaction chamber in the cylinder of the reaction apparatus.

Therefore, the present invention eliminates the above-described difficulties, disperses a certain amount of the material to be treated in the fluid vapor, and can introduce the material to be treated without causing biting in the seat portion or the like in the reaction engine or It aimed at providing a material to be treated supply method in the reactor of organic matter by subcritical fluid.

In order to achieve the above object, a method for supplying a material to be processed in a reaction apparatus for an organic substance or the like using a supercritical fluid or a subcritical fluid according to the present invention comprises a cylinder and a compression plunger provided in the cylinder. By operating, the fluid vapor accompanying the material to be treated introduced into the cylinder is compressed, and after the chemical reaction of the material to be treated by this compression is completed, the temperature and pressure of the fluid vapor are adjusted by operating the compression plunger in the reverse direction. In a reaction apparatus comprising a reaction engine that periodically performs intake and exhaust strokes by taking out the fluid containing the obtained product from the cylinder and blowing new fluid vapor into the cylinder, the reaction chamber or intake air of the reaction apparatus A line for supplying the material to be processed at a low pressure and a line for spraying the fluid at a high pressure are provided so as to communicate with the port, and a part of both lines is formed. The switching valve is provided, by moving the switching valve is provided in the cylinder such that a portion of the line that was filled with the material to be treated is communicated to the high pressure fluid line in fluid, within the period for sucking fluid vapor Further, the material to be treated is placed in a high-pressure fluid spray and dispersedly introduced into the intake port.

The material to be treated supply method in the reactor of the organic matter with supercritical fluid or subcritical fluid of the present invention as described above, the following effects are exhibited. According to the method for supplying a material to be processed according to the present invention, since the material to be processed is put on a high-pressure fluid spray and introduced into the cylinder or the intake port of the reaction apparatus, the fluid vapor sucked into the cylinder is generally reduced. It becomes possible to disperse uniformly.

  In the method of dispersing the material to be treated in the cylinder or the intake port by the injection valve together with the high pressure fluid, the material to be treated expands rapidly from the high pressure compression state in the cylinder or the intake port. The chemical reaction of the material to be treated in the reaction engine is further promoted.

  In addition, since the material to be treated is injected into the cylinder or the intake port as a single injection amount of “fluid-processed material mixed fluid-fluid”, injection is performed at the end of one injection of the material to be processed. Biting of the material to be processed into the valve seat can be prevented.

  In addition, since the material to be processed before being introduced into the cylinder or intake port by being placed on the high-pressure jet fluid has a mechanism that can be supplied at a low pressure, the concentration of the material to be processed that is easily separated from the fluid such as water is almost constant. This makes it possible to maintain a constant amount of the material to be treated over a long period of time.

  Next, the best mode for carrying out the present invention will be described with reference to the drawings. As shown in FIG. 1, a reaction engine 1 in the reaction apparatus is provided with a cylinder 2 having a compression plunger 4. The cylinder 2 is provided with a cylinder head 3 at the top thereof. The cylinder head 3 is provided with a treated material reservoir 7 so as to communicate with a treated material introduction port 7a provided outside in the intake port 3a, and a fluid spray valve 8 is provided in the vicinity thereof. In this reaction engine 1, water is used as a fluid for obtaining a supercritical fluid or a subcritical fluid. In addition, carbon dioxide, nitrous oxide, freon 12, freon 13, ethane, ethylene, propane, propylene are used as the fluid. , Butane, hexane, methanol, benzene, toluene, ammonia, and other substances can be selected and used. Examples of the material to be treated include organic substances such as wood powder.

  A treated material reservoir 7 in the intake port 3a of the cylinder head 3 is introduced with a constant flow rate or a constant amount of treated material from the treated material introduction port 7a. Reference numeral 5 denotes an intake valve, and reference numeral 6 denotes a tappet provided at the head of the intake valve 5.

  As shown in FIG. 1, a cam shaft mounting base 9 is provided on the upper portion of the cylinder head 3. The camshaft mount 9 is provided with a camshaft (not shown) orthogonal to the intake valve 5. The cam shaft rotates, and the cam provided on the cam shaft opens and closes the intake valve 5 via the tappet 6 provided at the end of the cam shaft.

  The treated material accumulated in the treated material reservoir 7 is dispersed in the intake port 3a by being put on the high-pressure jet fluid from the fluid jet valve 8 during the opening period of the intake valve 5 of the cylinder 2. It is introduced into the cylinder 2 together with the steam.

  1 is a method in which a material to be treated is dispersed in the intake port 3a by a jet from a fluid spray valve 8 provided separately, but the material to be treated shown in FIG. There is a method in which the material to be treated is directly injected into the cylinder 2 and the intake port 3a together with the fluid by the injection valve 11.

  Here, a case where the fuel is injected into the cylinder 2 will be described. The cylinder head 3 is provided with an injection valve main body 11, a nozzle main body 11 a is provided at the tip of the injection valve main body 11, and a nozzle hole 11 b is provided in the nozzle main body 11 a. The material to be treated passes through the injection valve body 11 and is injected from the injection port 11 b together with the high-pressure fluid and introduced into the cylinder 2. Since the fluid vapor introduced into the cylinder 2 is rapidly adiabatically compressed by the compression planner 4 to change into a supercritical fluid or subcritical fluid state, the material to be treated and the supercritical fluid or subcritical fluid are changed. The material to be treated is treated by a hydrolysis reaction, a thermal decomposition reaction, or the like.

  In the reaction engine 1, the material to be treated is injected into the low-pressure cylinder 2 together with the high-pressure fluid from the nozzle hole 11b of the water nozzle body 11. However, if the particle size of the injected fluid or the material to be treated is large, the material is injected. Since it becomes difficult to reach the processing temperature in a short time after being made, atomization by high pressure injection is required. On the other hand, when the fluid is injected at high pressure, the spray reach distance is increased, the material to be treated adheres to the sliding surface of the cylinder 2, enters the clearance of the compression plunger 4, and the sliding surface of the cylinder 2 is damaged. , Sometimes leads to seizure. However, the pressure in the cylinder 2 at the timing when the material to be treated is injected into the cylinder 2 is low, and the material to be treated that has been injected at a high pressure rapidly expands in volume and is finely pulverized. Thus, when the compression plunger 4 is generally aimed at the center of the cylinder 2 in the vicinity of the bottom dead center, the adhesion to the sliding surface of the cylinder 2 can be prevented. In addition, miniaturization of the material to be processed by high pressure injection increases the surface area relative to mass, and the chemical reaction of the material to be processed by the supercritical fluid or subcritical fluid proceeds rapidly, allowing the reaction of the material to be processed efficiently. It becomes.

  FIG. 3 shows a longitudinal sectional view of the injection valve main body 11 for injecting the material to be processed into the cylinder 2 at a high pressure, and FIG. 4 shows a sectional plan view thereof. Both are shown in partial cross-sectional views that are partially external views.

  The high-pressure fluid sent from a fluid pump not shown is guided from the fluid inlet 12 to the injection valve body 11. The high-pressure fluid is guided from the fluid inlet 12 via the path (A) 12a to the switching valve hole 14 penetrating in the lateral direction of the central portion of the injection valve body 11, and then to the nozzle body 11a via the path (B) 12b. And is injected into the cylinder 2 from the nozzle 11b.

  In addition to the fluid inlet 12 for high-pressure fluid, the injection valve main body 11 has a path (C) 13a that communicates with the workpiece inlet 13 and the switching valve hole 14 as a path (A) 12a and a path (B) for high-pressure fluid. ) It is attached to 12b almost in parallel. However, depending on the type of the material to be treated, if the fluid mixed with the material to be treated is sent at a high pressure, the concentration changes with time, making it difficult to continue feeding a certain amount. Therefore, the material to be treated inlet 13 and the path (C) A discharge path (D) 13b and a processing material discharge port 13c are provided opposite to 13a, and the fluid mixed with the processing material is circulated through these paths at a low pressure to maintain a constant concentration.

  A switching valve 15 is provided in the switching valve hole 14, and the switching valve 15 is set to move by the pressure of the fluid applied to the working fluid injection holes 14 a and 14 b provided at both ends of the switching valve hole 14. ing.

  On the outer periphery of the switching valve 15 built in the switching valve hole 14 provided in the substantially central portion of the injection valve body 11, there are a high-pressure fluid path (A) 12a, a path (B) 12b, and a path of the material to be processed (C ) 13a, corresponding to the openings of the path (D) 13b, grooves (A) 15a and grooves (B) 15b are provided.

  When the material to be treated is not ejected, the working fluid is injected into the working fluid injection hole 14a of the switching valve hole 14, and the switching valve 15 is moved to the working fluid injection hole 14b side as shown in FIG. In this state, the high-pressure fluid pressurized by a fluid pump not shown in the figure is fluid introduction port 12-route (A) 12a-switching valve groove (A) 15a-route (B) 12b-nozzle body 11a-nozzle It is injected into the cylinder 2 via 11b. At this time, the material to be treated is sent from a material storage tank (not shown) by a material pressure feeding pump (not shown) at a low pressure, and the material inlet 13-path (C) 13a-switching valve groove ( B) 15b-Route (D) 13b-Return to the material storage tank via the discharge port 13c.

  On the other hand, when injecting the material to be processed, the working fluid is injected into the working fluid injection hole 14b of the switching valve hole 14, and the switching valve 15 is moved to the working fluid injection hole 14a side. In this case, as shown in FIG. 6, the amount of movement is an amount that allows the switching valve groove (B) 15b to communicate with the opening of the high-pressure fluid path (A) 12a. Accordingly, the high-pressure fluid pressurized by a fluid pressure pump (not shown) passes through the fluid inlet 12-path (A) 12a-switching valve groove (B) 12b-nozzle body 11a-injection hole 11b. Is injected into. At this time, since the switching valve groove (A) 15a is filled with high-pressure fluid and the groove (B) 15b is filled with the material to be treated, the high-pressure fluid injected from the injection port 11b of the injection valve 11 is At the same time as the material to be treated is ejected, the fluid to be ejected becomes the material to be treated, which is aligned with "fluid-fluid to be treated-fluid", and the fluid present in the sheet portion at the end of ejection. Does not contain the material to be treated. That is, after the seat portion is washed with the fluid, the valve is seated to prevent the material to be treated from being caught in the seat portion. In addition, by appropriately setting the volume and the injection amount of each path, the ratio of the fluid and the material to be processed in one injection amount can be set, and the condition setting suitable for the type of the material to be processed and the fluid becomes possible. .

On the other hand, at this time, the material to be treated is sent at a low pressure from a material storage tank (not shown) by a material feeding pump (not shown), and is stopped at the material inlet 13-path (C) 13a. However, when the spraying of the material to be processed is completed, the working fluid is again injected into the working fluid injection hole 14a of the switching valve hole 14, and the switching valve 15 is moved to the working fluid injection hole 14b side as shown in FIG. Therefore, the material to be treated flows through the material to be treated inlet 13-path (C) 13a-switching valve groove 15b-path (D) 13b-processed material outlet 13c, and the fluid in the switching valve groove 15b is pushed away. The material to be processed is filled again in the switching valve groove 15b. However, since the fluid that does not contain the treated material that has been swept away enters the treated material storage tank, it is possible to provide a device for periodically checking the concentration and separating the excess fluid.

It is a partial longitudinal sectional front view illustrating the structure of the processed material supply method in the best reactors organic matter with supercritical fluid or subcritical fluid in the form for example of the present invention. It is a partial longitudinal sectional front view illustrating the arrangement state of the injection valve body in the material to be treated supply method in the best reactors organic matter with supercritical fluid or subcritical fluid in the form for example of the present invention. It is a longitudinal sectional view illustrating the injector body structure in the processed material supplying method in a reactor organic matter with supercritical fluid or subcritical fluid in the best mode for carrying out the present invention. A plan sectional view illustrating the injector body structure in the processed material supplying method in a reactor organic matter with supercritical fluid or subcritical fluid in the best mode for carrying out the present invention. It is a partial cross-sectional plan view illustrating the function of the switching valve in the injection valve body in the material to be treated supply method in the reactor of the organic matter according to a preferred embodiment of a supercritical fluid or subcritical fluid for implementation of the present invention. It is a partial cross-sectional plan view illustrating the function of the switching valve in the injection valve body in the material to be treated supply method in the reactor of the organic matter according to a preferred embodiment of a supercritical fluid or subcritical fluid for implementation of the present invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Reaction engine 2 Cylinder 3 Cylinder head 3a Intake port 4 Compression plunger 5 Intake valve 6 Tappet 7 To-be-processed material storage part 7a To-be-processed material inlet (A)
8 Fluid injection valve 9 Cam shaft mount 10 Reaction chamber 11 Injection valve body 11a Nozzle body 11b Injection hole 12 Fluid introduction port 12a Route (A)
12b Route (B)
13 Processed material introduction port 13a Route (C)
13b Route (D)
13c Material discharge port 14 Switching valve hole 14a Working fluid injection hole (A)
14b Working fluid injection hole (B)
15 Switching valve 15a Groove (A)
15b Groove (B)

Claims (1)

The cylinder is composed of a cylinder and a compression plunger provided in the cylinder, and the fluid vapor accompanying the material to be treated introduced into the cylinder is compressed by operating the compression plunger, and after the chemical reaction of the material to be treated by this compression is completed The compression plunger is operated in the opposite direction to lower the temperature and pressure of the fluid vapor, the fluid containing the obtained product is taken out from the cylinder, and a new fluid vapor is blown into the cylinder to periodically intake and exhaust strokes. In a reaction apparatus including a reaction engine for performing a reaction , a line for supplying a material to be treated at a low pressure and a line for spraying a fluid at a high pressure are provided in addition to a reaction chamber or an intake port of the reaction apparatus, and a part of both lines And a part of the line filled with the material to be treated is communicated with the high-pressure fluid line of the fluid by moving the switching valve. In provided in the cylinder such, within the period for sucking fluid vapor, put the workpiece to high pressure fluid spray, organic matter with supercritical fluid or subcritical fluid, characterized in that the dispersion introduced into the intake port To- be-processed material supply method in the reaction apparatus.

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