JP2006312115A - Gas pressure-filling apparatus and gas pressure-filling method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a gas pressure-filling apparatus and a gas pressure-filling method capable of removing a remaining gas in a vessel and replacing it with a desired gas. <P>SOLUTION: The gas pressure-filling apparatus for pressure-filling a gas into a gaseous phase in a pressure-resistance vessel filled with a liquid is provided with a high pressure syringe 1 having an effective needle inserted into the vessel; a drive means 2 for sliding a plunger inserted into the syringe 1; a switching valve 3 connected to the plunger; and an ultrasonic wave excitation stirring apparatus 5 for imparting stirring and ultrasonic vibration to the liquid in the pressure-resistance vessel. The plunger is connected to a gas supplying source through the switching valve and discharges the gas in the pressure-resistance vessel by switching of the switching valve. The gas pressure-filling method using the apparatus is provided. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a gas press-in apparatus and a gas press-in method suitable for testing in a general chemical industry field, especially in a laboratory.

  Conventionally, a device for degassing a gas dissolved in a liquid is well known. For example, in Patent Document 1, as an apparatus for reliably degassing a gas in a liquid in a short time, an ultrasonic vibrator disposed near a container into which a liquid in which a gas is dissolved is injected, and an opening of the container There has been proposed a deaeration device composed of a vacuum chamber having an exhaust port and suction means connected to the exhaust port. According to this apparatus, sufficient deaeration is possible even for a limited time before the liquid resin is cured, so the appearance is improved by reducing the microvoids, and until the resin is cured by reducing the deaeration time. Time can be used more effectively, and cracks caused by the monomer generated by the polymerization of the resin being alienated by the dissolved gas can be prevented.

  In Patent Document 2, as a degassing device for high-performance liquid chromatography, helium gas is supplied into a pressure-resistant container for storing an eluent and maintained at a predetermined pressure, thereby re-dissolving air in the eluent. An apparatus for preventing the above and maintaining a deaerated state has been proposed.

JP 63-264107 A JP 2003-107063 A

  However, both of these proposals relate to an apparatus for degassing a gas dissolved in a liquid. However, in a gas reaction using a catalyst or the like, a reaction apparatus in which a catalyst, a solvent, a gas, a rotor, and the like are placed in a reaction container may be used. In this case, gas injection into the reaction container This is done by press-fitting the target gas into a container that can be pressurized with a cylinder pressure. Therefore, there is a problem that air or the like remains in the container or air or the like in the solvent cannot be removed, so that the inside of the container cannot be completely replaced with the target gas.

  The present invention has been made in view of the above-described conventional problems, and it is an object of the present invention to provide a gas press-in device and a gas press-in method that can remove residual gas in a container and reliably replace it with a target gas. And

  In order to solve the above-mentioned problems, the present inventors have intensively studied. As a result, they have found that the object can be achieved by the following configuration, and have completed the present invention.

That is, the present invention is as follows.
1) A gas press-fitting device for press-fitting a gas into a gas phase in a pressure-resistant container filled with a liquid, wherein a high-pressure syringe having a perforated needle inserted into the container and a plunger inserted into the syringe are slid Drive means for moving, a switching valve connected to the plunger, and an ultrasonic oscillation stirring device that applies stirring and ultrasonic vibration to the liquid in the pressure-resistant container, and the plunger supplies a gas supply source via the switching valve. A gas press-fitting device, wherein the gas press-fitting device is configured to exhaust the gas in the pressure vessel by switching the switching valve,
2) The gas press-fitting device according to 1), wherein the driving means is connected to an air damper,
3) The gas press-fitting device according to 1) or 2), wherein the exhaust pipe includes suction means for sucking a gas,
4) The gas press-fitting device according to any one of 1) to 3) including a fixing means for fixing the pressure vessel, and
5) A gas press-fitting method for press-fitting gas into a pressure-resistant container filled with a liquid, and at the time of gas press-fitting, the liquid in the pressure-resistant container is agitated and subjected to ultrasonic vibration and connected to the pressure-resistant container with a high-pressure syringe. A perforated needle was inserted, gas was supplied from the outside to a supply pipe connected to the plunger inserted into the high-pressure syringe via a switching valve, and the gas was pressed into the pressure vessel by raising and lowering the plunger. Thereafter, the gas in the container is exhausted through an exhaust pipe connected to the switching valve by switching the switching valve.

According to the above configuration of the present invention, the gas dissolved in the liquid in the container is discharged from the liquid by repeating the press-fitting and exhausting of the gas while applying stirring and ultrasonic vibration to the liquid in the pressure-resistant container. In addition, the gas in the container can be surely replaced with the target gas (pressed gas). For this reason, it is possible to improve the experimental accuracy. Furthermore, when carbon dioxide (CO ₂ ) gas is injected, the CO ₂ fixation reaction can be carried out efficiently and with high accuracy.

  In addition, by connecting the drive means to the air damper, it is possible to automatically raise and lower, the needle entry speed and angle are constant, syringe backlash is eliminated, the phenomenon of leakage from the septum during needle insertion, and syringe up and down The power of time is reduced.

  In addition, since the exhaust pipe is provided with suction means for sucking gas, the amount of gas discharged from the container through the exhaust pipe increases, so that the target gas can be replaced in a short time.

  Furthermore, according to the apparatus provided with the fixing means for fixing the pressure vessel to the gas press-fitting device, the gas supply (press-fitting) and the exhaust operation are smooth.

  Embodiments of the present invention will be described with reference to the drawings. FIG. 1 is a front external view showing the entirety of a gas press-fitting device according to an embodiment of the present invention. 2 is an enlarged front view around the high-pressure syringe, FIG. 3 is a front view of the damper portion, and FIG. 5 is an external perspective view showing an example of a pressure vessel that can be used in the gas press-fitting device of the present invention and a lid portion. It is an expanded sectional view.

  In FIG. 1, the gas injection device of the present invention slides a high-pressure syringe 1 having a perforated needle 15 for injecting gas into a gas phase in a pressure-resistant container filled with liquid, and a plunger inserted in the syringe. Drive means (handle) 2 to be switched, a switching valve (three-way cock) 3 connected to the plunger, and an ultrasonic oscillation stirring device 5 that applies stirring and ultrasonic vibration to the liquid in the pressure-resistant container, A gas supply source (cylinder) 8 is connected via the switching valve 3, and the gas in the pressure vessel is exhausted by switching the switching valve 3.

  In FIG. 1, the high-pressure syringe 1 is configured by a pressurizable syringe so that a gas reaction can be performed even in a pressurized state, and is fixed to the structure 9 by a fixing device 13 or the like. The plunger 11 inserted into the high pressure syringe 1 functions as a gas reservoir. The plunger 11 is connected to a switching valve (three-way cock) 3 fixed to the driving means 2, and the switching valve 3 is connected to a supply pipe 7 a connected to the gas supply source 8. The gas can be introduced into the plunger from the gas supply source. Thereafter, the plunger 11 is moved up and down (up and down) by moving the drive means up and down (up and down), whereby gas is injected into the container 20.

  FIG. 2 is an enlarged front view showing the periphery of the high-pressure syringe. The plunger 11 inserted into the high-pressure syringe 1 moves up and down while sliding in the syringe, but the switching valve 3 also serves as a lid for the plunger 11 as shown in FIG. Therefore, by closing the switching valve 3 before raising and lowering the plunger 11, and then raising and lowering the plunger 11, a certain amount of gas can be fed into the container. The gas fed from the plunger enters the container through the needle hole of the perforated needle (horizontal hole needle) 15 provided in the high pressure syringe 1. The perforated needle is connected to the syringe 1 with a screw 14.

  In addition, an air damper 4 connected to the drive member 2 is fixed to the structure 9. As the air damper 4, for example, as shown in FIG. 3, an air damper having an upper and lower opening is used, and the drive member can be automatically raised and lowered by alternately inserting compressed air from above and below the damper. Thereby, the penetration speed and angle of the needle are constant, the backlash of the syringe is eliminated, the leakage phenomenon from the septum at the time of inserting the needle and the force at the time of raising and lowering the syringe are reduced.

  In FIG. 1, a pressure vessel 20 into which gas is injected is filled with a liquid 22, and a stirrer 21 is contained in the vessel. At the time of gas injection and exhaust, it is desirable to arrange the pressure vessel 20 in a water vessel 23 placed on an ultrasonic oscillation stirrer. The presence of water around the pressure-resistant vessel 20 makes it possible to transmit ultrasonic waves to the inside of the vessel, and has the effect of increasing the solubility of the gas by stirring the liquid by stirring with a stirrer and vibration by ultrasonic waves. Here, the ultrasonic vibration stirrer is not limited as long as it has an ultrasonic oscillation function and a stirring function, and even if it functions as a unit, it functions as a separate body. Also good.

  In the gas press-fitting device, it is desirable to use fixing means such as a spring or rubber for fixing the container in order to facilitate gas supply (press-fitting) and exhaust operation. FIG. 4 is a schematic top view of the periphery of the fixed spring, showing a state in which the pressure-resistant container 20 is fixed by a spring. As shown in FIG. 4, the container 20 is installed between the two fixing springs 6 fixed to the structure 9 that becomes the mold.

  In the gas press-fitting apparatus and method of the present invention, a pressure-resistant container, particularly a pressure-resistant transparent container is preferably used. This is because a reaction experiment by injecting a gas such as carbon dioxide gas can be performed even in a pressurized state, and the light transmittance of the container itself is required to advance the reaction using the photocatalyst. is there. As the pressure-resistant transparent container, for example, a glass pressure-resistant transparent container or the like as shown in FIG. 5 can be used, and coating may be applied to the outside.

  In addition to the liquid used as the reaction solution, a catalyst used as necessary is added to the pressure-resistant transparent container 20. Since the pressure-resistant transparent container 20 is manufactured so that the lower end portion 20b of the upper lid and the upper end portion 20a of the main body are fitted with screws, the gas contained in the container does not leak. The upper lid has a syringe port 20e for press-fitting gas into the container, a silicon stopper 20d for preventing gas leakage during press-fitting, and a valve 20c for adjusting insertion of the syringe. ing. By pushing the valve 20c to the left or right, the valve opens and closes. By injecting gas with the valve opened, and closing the valve after the injection, the inside of the container is kept sealed.

  Next, a gas injection method using the gas injection device of the present invention will be specifically described with reference to FIG. First, after filling the pressure vessel 20 containing the stirrer 21 with a predetermined liquid 22, this vessel is placed in a water-filled vessel placed on an ultrasonic oscillation stirrer, and the liquid in the pressure vessel is changed. Apply agitation and ultrasonic vibration. Although it does not specifically limit as said liquid, The solvent (methanol, ethanol, water, etc.) made to react with injection gas, the solution which dissolved and disperse | distributed the additive, the catalyst, etc. in those solvents are used. .

  Next, after inserting the perforated needle 15 connected to the high pressure syringe 1 into the pressure vessel, the three-way cock 3 is switched, and the gas is supplied from the cylinder 8 to the supply pipe 7a, whereby the gas passes through the three-way cock. It is introduced into the connected plunger 11. After introducing gas into the plunger, the three-way cock on the plunger side is closed. Since the plunger moves up and down in conjunction with the raising and lowering of the handle, the plunger is raised and lowered to press-fit the gas in the plunger into the pressure-resistant container.

  Thereafter, the three-way cock 3 is switched in the opposite direction to that in FIG. 1, and the gas in the container 20 is exhausted through the exhaust pipe 7 b connected to the three-way cock 3. By connecting the exhaust pipe 7b to a suction means for sucking gas, such as a vacuum pump, the exhaust can be completed in a short time. Also, by operating the ultrasonic oscillation agitator during exhaust, the gas in the liquid becomes bubbles due to the cavitation phenomenon by the vibration and stirring by the ultrasonic waves, and the bubbles can be discharged from the liquid in a short time.

  Next, the three-way cock is switched to the direction shown in FIG. 1, and the above-described gas press-fitting operation is performed again. By alternately performing the gas injection operation and the exhaust operation, the gas in the container can be reliably replaced with the target gas.

  The above embodiment shows one embodiment of the present invention, and the present invention is not limited to the above embodiment, and various modifications are possible within the scope of the invention described in the claims. Needless to say, they are also included in the scope of the present invention.

It is a front external view which shows the whole gas press-fitting apparatus which concerns on the Example of this invention. It is a front view around the high pressure syringe of the gas press-fitting device shown in FIG. It is a front view of the air damper part of the gas press-fitting device shown in FIG. FIG. 2 is a schematic top view of a portion around a fixed spring of the gas press-fitting device shown in FIG. 1. FIG. 2 is an external view of the pressure vessel shown in FIG. 1 and a partially enlarged sectional view around the lid.

Explanation of symbols

1 High-pressure syringe 2 Drive member 3 Switching valve (3-way cock)
4 Air damper 5 Ultrasonic oscillation stirrer 6 Fixing means (fixing spring)
7a Supply piping 7b Exhaust piping 8 Gas supply source (cylinder)
9 Structure 11 Plunger 15 Perforated needle 20 Pressure-resistant container 21 Stirrer 22 Liquid 23 Water-filled container

Claims (5)

A gas press-fitting device for press-fitting a gas into a gas phase in a pressure-resistant container filled with a liquid, wherein a high-pressure syringe having a perforated needle inserted into the container and a plunger inserted into the syringe are slid Drive means, a switching valve connected to the plunger, and an ultrasonic oscillation stirring device that applies stirring and ultrasonic vibration to the liquid in the pressure-resistant container, and the plunger is connected to a gas supply source via the switching valve The gas press-fitting device is configured to exhaust the gas in the pressure-resistant container by switching the switching valve. The gas press-fitting device according to claim 1, wherein the driving means is connected to an air damper. The gas press-fitting device according to claim 1, wherein the exhaust pipe includes suction means for sucking gas. The gas press-fitting device according to any one of claims 1 to 3, further comprising fixing means for fixing the pressure vessel. A gas press-in method for press-fitting a gas into a pressure-resistant container filled with a liquid, and at the time of gas press-fitting, the liquid in the pressure-resistant container is agitated and subjected to ultrasonic vibration, and has a hole connected to the pressure-resistant container with a high pressure syringe After inserting the needle, supplying gas from the outside to the supply pipe connected to the plunger inserted into the high-pressure syringe through the switching valve, and performing the press-fitting of the gas into the pressure-resistant container by raising and lowering the plunger, A gas injection method characterized in that the gas in the container is exhausted through an exhaust pipe connected to the switching valve by switching the switching valve.

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