JP5500535B2 - Raw material supply method and apparatus - Google Patents

Description

  The present invention relates to a raw material supply method and an apparatus therefor, and in particular, in a hydrothermal synthesis that generates fine particles such as metal oxides in the presence of high-temperature and high-pressure hot water, the raw material can be stably supplied to the reactor side over a long period of time. The present invention relates to a raw material supply method and an apparatus therefor.

As an apparatus for producing fine particles using high-temperature and high-pressure water, there is one previously proposed by the same applicant (see Patent Document 1).
There, a fine particle production apparatus using high-temperature and high-pressure water has a water supply path for supplying water that becomes supercritical water or subcritical water from a distilled water tank that stores distilled water, and a metal salt that is a fluid raw material from the raw material supply tank. A raw material supply path for supplying an aqueous solution. In the raw material supply path, the aqueous metal salt solution is deaerated in the raw material degassing section, and the degassed metal salt aqueous solution is pressurized by the raw material pressurizing means comprising a high-pressure pump and is pumped to the reactor side.

JP-A-2005-21724

  However, in the hydrothermal synthesizer that pumps the fluid raw material to the reactor with a high-pressure pump, the fine particles in the raw material solution (slurry) get caught in or clog the seal part in the high-pressure pump. There was a problem of causing it. Such a problem is not limited to the hydrothermal synthesizer. Such a problem is a problem common to an apparatus for pumping slurry at a certain high pressure.

  The present invention has been made to solve such problems, and an object of the present invention is to provide a raw material supply method and apparatus capable of stably supplying raw materials to the reactor side over a long period of time. There is to do.

Raw material supply method of the present invention, a sheet cylinder tube is slidable within the cylinder tube, a plurality of double-acting with a piston that partitions the inside of the cylinder tube into a first chamber and a second chamber A plurality of water supply means that can prepare a fluid pressure cylinder and supply fluid raw material to one chamber of the first chamber or the second chamber by a raw material supply means and water to the other chamber at a pressure higher than that of the raw material supply means In the raw material supply method of supplying a fluid raw material to the reactor side by alternately supplying the water in the above, each double-acting fluid pressure cylinder is connected to a supply path for supplying the water, Each of the pistons of a plurality of double-acting fluid pressure cylinders can slide in the cylinder tube independently of each other, and the supply path has a plurality of branch portions each having at least one of an on-off valve and a three-way valve. And the plurality Each of the water supply means is connected to each of the plurality of double-acting fluid pressure cylinders via one of the branch portions, and each of the plurality of water supply means is connected to each of the plurality of double-acting fluid pressure cylinders. By supplying the water, the plurality of double-acting fluid pressure cylinders are replaced by supplying a fluid raw material to the reactor side . In this case, it is preferable to use a tubing pump as the raw material supply means .

According to this, the fluid raw material is fed to the double-acting fluid pressure cylinder by the raw material supply means , and the water is fed from the double-acting fluid pressure cylinder to the reactor side by feeding water to the double-acting fluid pressure cylinder. Since it can supply, a fluid raw material can be supplied to the reactor side, without using the conventional high pressure pump. That is, since a conventional high-pressure pump is not used as a pump for feeding a fluid raw material to a double-acting fluid pressure cylinder, fine particles in the raw material solution (slurry) are caught or clogged in a seal portion in the high-pressure pump. Can be avoided. In addition, since the water supply means for sending water to the double-acting fluid pressure cylinder sends water that does not contain fine particles, there is no problem such as biting of fine particles into the seal portion in the water supply means .

The material supply device of the present invention, a sheet cylinder tube is slidable within the cylinder tube, a plurality of double-acting with a piston that partitions the inside of the cylinder tube into a first chamber and a second chamber A fluid pressure cylinder; a raw material tank; a raw material supply means for supplying a fluid raw material from the raw material tank to one of the first chamber or the second chamber; and the other chamber of the first chamber or the second chamber. and a plurality of water supply means for supplying water at a high pressure than the raw material supply means, said first chamber or fluid material in the raw material supply means to the one chamber of the second chamber, alternately water into other chamber A raw material supply apparatus configured to supply a fluid raw material to the reactor side by supplying , further comprising a supply path for supplying the water, to which each of the double-acting fluid pressure cylinders is connected. The pistons of the plurality of double-acting fluid pressure cylinders Each of them can slide in the cylinder tube independently of each other, and the supply path has a plurality of branch portions each having at least one of an on-off valve and a three-way valve, and the plurality of water supply means Each is characterized in that it is connected to each of the plurality of double-acting fluid pressure cylinders via any one of the branch portions . In this case, it is preferable to use a tubing pump as the raw material supply means . Moreover, it is preferable to further comprise a stirring device that stirs the inside of the first chamber and the second chamber on the side to which the fluid raw material is supplied.

According to this, the fluid raw material is fed to the double-acting fluid pressure cylinder by the raw material supply means , and the water is fed from the double-acting fluid pressure cylinder to the reactor side by feeding water to the double-acting fluid pressure cylinder. Since it can supply, a fluid raw material can be supplied to the reactor side, without using the conventional high pressure pump. That is, since a conventional high-pressure pump is not used as a pump for feeding a fluid raw material to a double-acting fluid pressure cylinder, fine particles in the raw material solution (slurry) are caught or clogged in a seal portion in the high-pressure pump. Can be avoided. In addition, since the water supply means for sending water to the double-acting fluid pressure cylinder sends water that does not contain fine particles, there is no problem such as biting of fine particles into the seal portion in the water supply means .

  According to the present invention, by employing a double-acting fluid pressure cylinder, it is possible to stably supply a fluid raw material containing fine particles to the reactor side over a long period of time without using a conventional high-pressure pump. There is an effect.

It is a flowchart of the raw material supply apparatus in the hydrothermal synthesis which shows one Example of this invention.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

As shown in FIG. 1, the raw material supply apparatus 1 concerning this embodiment is used for hydrothermal synthesis. The raw material supply apparatus 1 according to the present embodiment is capable of sliding inside a cylindrical cylinder tube 2 and the cylinder tube 2, and divides the inside of the cylinder tube 2 into a first chamber 3 and a second chamber 4. A double-acting fluid pressure cylinder 6 having a piston 5, a raw material tank 7 storing a fluid raw material such as a metal salt aqueous solution to be subjected to a hydrothermal synthesis reaction, and a first raw material chamber 3 of the cylinder tube 2 for supplying the fluid raw material from the raw material tank 7 And a high pressure pump 18 for supplying high pressure water to the second chamber 4 and a high pressure pump 20. Entrances (supply / discharge ports) 9 and 10 are provided at the ends of the first chamber 3 and the second chamber 4, respectively. A stirring device 24 is attached in the first chamber 3. The pressurizing pump 18 and the high-pressure pump 20 can supply fluid at a higher pressure than the low-pressure pump 8. Furthermore, the raw material supply apparatus 1 according to the present embodiment is slidable inside a cylindrical cylinder tube 2 ′ and the cylinder tube 2 ′, and the inside of the cylinder tube 2 ′ is connected to the first chamber 3 ′ and the second chamber 2 ′. A double-acting fluid pressure cylinder 6 ′ having a piston 5 ′ partitioned into a chamber 4 ′ is also provided. Entrances (supply / discharge ports) 9 ′ and 10 ′ are also provided at each end of the first chamber 3 ′ and the second chamber 4 ′. The piston 5 of the double-acting fluid pressure cylinder 6 and the piston 5 'of the double-acting fluid pressure cylinder 6' can slide in the cylinder tube 2 or the cylinder tube 2 'independently of each other. The low-pressure pump 8 supplies the fluid raw material to the second chamber 4 and the second chamber 4 ′, and the pressurizing pump 18 or the high-pressure pump 20 supplies high-pressure water to the first chamber 3 and the first chamber 3 ′. May be.

  The inlet / outlet 9 of the first chamber 3 of the cylinder tube 2 and the raw material tank 7 are connected by a raw material supply path 11 to the cylinder. The inlet / outlet port 9 ′ of the first chamber 3 ′ of the cylinder tube 2 ′ and the raw material tank 7 are also connected by a raw material supply path 11 to the cylinder. The raw material supply path 11 to the cylinder is provided with a low pressure pump 8 for supplying fluid raw material from the raw material tank 7 to the first chamber 3 of the cylinder tube 2 and the first chamber 3 ′ of the cylinder tube 2 ′. A first on-off valve 12 is provided between the low pressure pump 8 and the inlet / outlet 9 of the supply passage 11. A first on-off valve 12 'is provided between the low pressure pump 8 and the inlet / outlet 9'. The inlet / outlet 9 of the first chamber 3 of the cylinder tube 2 and the reactor 13 are connected by a raw material supply path 14 to the reactor 13 side, and the raw material supply path 14 is provided with a second on-off valve 15. The inlet / outlet 9 ′ of the first chamber 3 ′ of the cylinder tube 2 ′ and the reactor 13 are also connected by a raw material supply path 14 to the reactor 13 side, and the raw material supply path 14 is provided with a second on-off valve 15 ′. .

  The entrance / exit 10 of the second chamber 4 of the cylinder tube 2 and the filling water tank 16 are connected by a high-pressure water supply path 17. The high pressure water supply path 17 is provided with a pressurizing pump 18 for supplying high pressure water to the second chamber 4. The inlet / outlet port 10 ′ of the second chamber 4 ′ of the cylinder tube 2 ′ and the filling water tank 16 are connected by a high-pressure water supply path 17 ′. The high-pressure water supply path 17 ′ is also connected to the pressurizing pump 18.

  The inlet / outlet port 10 of the cylinder tube 2 and the high-pressure pump 20 are connected by a water supply path 19. That is, since the pipe branches from the water supply path 19 (the fourth on-off valve 25 is provided in the middle of the pipe) and the pipe is connected to the high-pressure water supply path 17, the inlet / outlet of the cylinder tube 2 is provided. 10 and the high-pressure pump 20 are connected to each other. The inlet / outlet port 10 ′ of the cylinder tube 2 ′ and the high pressure pump 20 are also connected by a water supply path 19. That is, the pipe branches from the water supply path 19 (a fourth on-off valve 25 ′ is provided in the middle of the pipe), and the pipe is connected to the high-pressure water supply path 17 ′. The inlet / outlet 10 'and the high-pressure pump 20 are connected to each other. The high-pressure pump 20 and the reactor 13 are connected by a water supply path 19. A third on-off valve 21 is provided between the high-pressure pump 20 and the reactor 13.

  Next, a method for supplying the raw material to the reactor 13 using the raw material supply apparatus 1 configured as described above will be described.

  It is assumed that the fluid raw material is filled in the first chamber 3 ′ of the cylinder tube 2 ′ in advance or near full. Now, the first on-off valve 12 and the second on-off valve 15 'are opened, the second on-off valve 15 and the first on-off valve 12' are closed, and the low pressure pump 8 is driven to drive the first chamber 3 of the cylinder tube 2. A fluid raw material is supplied through the inlet / outlet 9. The fluid raw material in the first chamber 3 is stirred by the stirring device 24. Thereby, the fine particles in the fluid raw material are uniformly dispersed. During this time, the high pressure pump 20 supplies high pressure water to the second chamber 4 ′ of the cylinder tube 2 ′ via the water supply passage 19 and the high pressure water supply passage 17 ′ (the pressurization pump 18 supplies high pressure water. Alternatively, the pressurizing pump 18 and the high-pressure pump 20 may supply high-pressure water in cooperation with each other). When high pressure water is supplied to the second chamber 4 ′ of the cylinder tube 2 ′, the pressure of the high pressure water acts on the piston 5 ′, and the piston 5 ′ moves toward the first chamber 3 ′. The fluid raw material is extruded and supplied to the side of the reactor 13 from the inlet / outlet 9 ′. Thereafter, when the fluid raw material in the first chamber 3 ′ becomes empty or near empty, a sensor 23 ′ composed of a magnetic proximity switch or the like attached to the end of the first chamber 3 ′ detects the position of the piston 5 ′, and the fourth The on-off valve 25 inputs the detection signal and opens, and high-pressure water is supplied to the second chamber 4 of the cylinder tube 2 through the water supply path 19 and the high-pressure water supply path 17. Simultaneously with the start of the supply, the first on-off valve 12 and the second on-off valve 15 ′ are closed, and the second on-off valve 15 and the first on-off valve 12 ′ are opened. When high-pressure water is supplied to the second chamber 4 in this state, the pressure of the high-pressure water acts on the piston 5, and the piston 5 moves toward the first chamber 3, so that the fluid raw material enters the inlet / outlet 9 from the first chamber 3. And fed to the reactor 13 side. On the other hand, since the second on-off valve 15 ′ is closed, the first on-off valve 12 ′ is opened, and the low-pressure pump 8 is driven, the fluid raw material enters and exits the first chamber 3 ′ of the cylinder tube 2 ′. Is supplied through. The fluid raw material in the first chamber 3 'is stirred by the stirring device 24'. Thereby, the fine particles in the fluid raw material are uniformly dispersed. Thereafter, when the fluid raw material in the first chamber 3 becomes empty or near empty, the sensor 23 including a magnetic proximity switch attached to the end of the first chamber 3 detects the position of the piston 5, and the fourth on-off valve 25 ' The detection signal is input and opened, and high-pressure water is supplied to the second chamber 4 ′ of the cylinder tube 2 ′ through the water supply channel 19 and the high-pressure water supply channel 17 ′. Simultaneously with the start of the supply, the first on-off valve 12 'and the second on-off valve 15 are closed, and the second on-off valve 15' and the first on-off valve 12 are opened. This is possible because signals are communicated via a communication path that has been made or a communication path that is not shown). When high-pressure water is supplied to the second chamber 4 ′ in this state, the pressure of the high-pressure water acts on the piston 5 ′ and the piston 5 ′ moves toward the first chamber 3 ′, thereby fluid from the first chamber 3 ′. The raw material is extruded and supplied toward the reactor 13 through the inlet / outlet 9 ′.

As described above, the fluid raw material is supplied to the first chamber 3 of the double-acting fluid pressure cylinder 6 and the first chamber 3 of the double-acting fluid pressure cylinder 6 by the low-pressure pump 8, and the second chamber 4 and the second chamber 4 ′. a high pressure pump 20 to (or, as described above, at least one among the pressurizing pump 18 and the high-pressure pump 20) by alternately supplying high-pressure water, without using a conventional high-pressure pumps, double Instead of the dynamic fluid pressure cylinder 6 and the double-acting fluid pressure cylinder 6 ′, a fluid material can be supplied to the reactor 13 side.

  In the raw material supply apparatus in the hydrothermal synthesis of the illustrated example, another double-acting fluid pressure cylinder 6 'is arranged in parallel with the double-acting fluid pressure cylinder 6 so that one double-acting fluid pressure is provided. When the fluid raw material in the cylinder 6 is supplied to the reactor 13 side and the remaining amount becomes small, the fluid raw material can be continuously supplied to the reactor 13 side from another double-acting fluid pressure cylinder 6 '. The raw material supply device may be configured by only one double-acting fluid pressure cylinder 6. Below, the method to supply a raw material to the reactor 13 side using the raw material supply apparatus comprised in that way is demonstrated.

  Now, the first on-off valve 12 is opened, the second on-off valve 15 is closed, and the low-pressure pump 8 is driven to supply the fluid raw material to the first chamber 3 of the cylinder tube 2 through the inlet / outlet 9. When the first chamber 3 is full or nearly full, the sensor 22 comprising a magnetic proximity switch attached to the end of the second chamber 4 detects the position of the piston 5, and the low-pressure pump 8 detects the detection signal. To automatically stop the drive and stop the supply of fluid raw material. Simultaneously with this supply stop, the first on-off valve 12 is closed, the second on-off valve 15 is opened, and at least one of the pressurizing pump 18 and the high-pressure pump 20 is driven to supply high-pressure water to the second chamber 4. Supplying through the inlet / outlet 10, the pressure of the high-pressure water acts on the piston 5, and the piston 5 moves toward the first chamber 3, whereby the fluid raw material is directed from the first chamber 3 toward the reactor 13 through the inlet / outlet 9. Extruded.

  When the fluid raw material has been extruded from the first chamber 3, the sensor 23 detects the position of the piston 5, and the pump that has been supplying high-pressure water inputs the detection signal to automatically stop the drive and to the second chamber 4. The high pressure water is stopped, and the low pressure pump 8 is driven again as described above to supply the fluid raw material to the first chamber 3. In addition, such a drive start and an automatic stop of such a pump are enabled by communicating a signal through the communication path shown in figure and the communication path not shown in figure.

  Thus, the fluid raw material is supplied to the first chamber 3 of the double-acting fluid pressure cylinder 6 by the low-pressure pump 8, and the second chamber 4 is supplied by the pressurization pump 18 (or among the pressurization pump 18 and the high-pressure pump 20. By supplying high-pressure water alternately (at least one), the fluid raw material can be supplied to the reactor 13 without using a conventional high-pressure pump.

  Incidentally, the raw material supply apparatus 1 according to the present embodiment may be used for applications other than hydrothermal synthesis. Also in this case, when the fluid raw material containing the slurry and other fine particles is supplied to the reactor, the fluid raw material can be stably supplied over a long period of time.

  Further, the stirring devices 24 and 24 'are not necessarily required.

DESCRIPTION OF SYMBOLS 1 Raw material supply apparatus in hydrothermal synthesis 2, 2 'Cylinder tube 3, 3' First chamber 4, 4 'Second chamber 5, 5' Piston 6, 6 'Double acting fluid pressure cylinder 7 Raw material tank 8 Low pressure pump 9, 9 ', 10, 10' Entrance / exit 13 Reactor 18 Pressure pump 20 High pressure pump 24, 24 'Stirrer

Claims (5)

And Shi cylinder tube is slidable within the cylinder tube, providing a plurality of double-acting hydraulic cylinder with a piston that partitions the inside of the cylinder tube into a first chamber and a second chamber, wherein The fluid raw material is supplied to one chamber of the first chamber or the second chamber by the raw material supply means , and the water is alternately supplied to the other chamber by a plurality of water supply means capable of supplying water at a higher pressure than the raw material supply means. A raw material supply method for supplying fluid raw material to the reactor side ,
Each of the double-acting fluid pressure cylinders is connected to a supply path for supplying the water;
The pistons of the plurality of double-acting fluid pressure cylinders can slide in the cylinder tube independently of each other;
The supply path has a plurality of branch portions each having at least one of an on-off valve and a three-way valve;
Each of the plurality of water supply means is connected to each of the plurality of double-acting fluid pressure cylinders via any of the branch portions,
Each of the plurality of water supply means supplies the water to each of the plurality of double-acting fluid pressure cylinders to supply a fluid raw material to the reactor side instead of the plurality of double-acting fluid pressure cylinders. A raw material supply method. The raw material supply method according to claim 1, wherein the raw material supply means is a tubing pump. And Shi cylinder tube is slidable within the cylinder tube, a plurality of double-acting hydraulic cylinder with a piston that partitions the inside of the cylinder tube into a first chamber and a second chamber, and the raw material tank , A raw material supply means for supplying fluid raw material from the raw material tank to one of the first chamber or the second chamber, and water at a higher pressure than the raw material supply means to the other chamber of the first chamber or the second chamber. A plurality of water supply means for supplying fluid, and reacting the fluid raw material by alternately supplying the fluid raw material to the one chamber of the first chamber or the second chamber by the raw material supply means and water to the other chamber A raw material supply device configured to supply to the vessel side ,
Each of the double-acting fluid pressure cylinders is connected to a supply path for supplying the water;
The pistons of the plurality of double-acting fluid pressure cylinders can slide in the cylinder tube independently of each other;
The supply path has a plurality of branch portions each having at least one of an on-off valve and a three-way valve;
Each of the plurality of water supply means is connected to each of the plurality of double-acting fluid pressure cylinders via any one of the branch portions . The raw material supply apparatus according to claim 3, wherein the raw material supply means is a tubing pump.   4. The raw material supply apparatus according to claim 3, wherein the raw material supply apparatus further includes a stirring device for stirring the inside of the first chamber and the second chamber on the side to which the fluid raw material is supplied. .

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