JPH07151456A - Method and apparatus for recovering fluorine-based gas - Google Patents

Abstract

PURPOSE:To recover a large quantity in high purity by introducing liquid component, gas component and pressurizing gas retaining in a storage vessel by a suction pump to a cooling liquefying tank to be cooled to be liquefied, separating it to a fluorine-based gas and pressurizing gas, and liquefying the fluorine- based gas. CONSTITUTION:When a pressure in a recovery vessel 2 is raised by vaporizing liquefied halon and separating nitrogen gas dissolved in the halon, a switching valve 73 mounted via a vaporized gas discharge passage 13 for connecting an upper part of the tank 2 to a gas component recovery passage 7 to feed gas in the tank 2 from the passage 7 to a cooling liquefying tank 10. In this case, it is cooled to a temperature near a halon solidifying temperature to be separated to halon gas component and nitrogen gas component, the halon gas component is liquefied to be recovered, and the nitrogen gas component is discharged from a safe valve circuit 29. Thus, substantially entirety can be recovered without discharging the halon into the atmosphere.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for recovering fluorine-containing gas, and more particularly to a method and an apparatus for recovering Halon 1301 (CFC 13B1) used as a fire extinguishing agent.

[0002]

2. Description of the Related Art Conventionally, a fluorine-based gas has been used as a refrigerant or a fire extinguishing agent of a refrigerator by utilizing its chemical and thermal properties. And, conventionally, this fluorine-based gas has been released to the atmosphere at the time of periodic inspection of the fire extinguisher and at the time of discarding the refrigerator.

[0003]

However, when the fluorine-based gas is released into the atmosphere, it may cause the destruction of the ozone layer surrounding the earth. Therefore, the release of a certain fluorine-based gas into the atmosphere is subject to the regulation. Production was also suspended. However, in certain fields, it may be necessary to use halon gas or fluorine-based gas, so there is a need for a fluorine-based gas recovery technology.Currently, a method for efficiently recovering fluorine-based gas in high purity is required. Can't be seen. The present invention has been made paying attention to such a point, and an object thereof is to provide a recovery method and a recovery apparatus capable of recovering a large amount of fluorine-based gas with high purity.

[0004]

In order to achieve the above-mentioned object, the first aspect of the present invention uses the liquefied fluorine-based gas stored in a storage container, and most of the liquid component in the storage container itself. The first recovery procedure of collecting in the recovery tank by pressure, and after the completion of the first recovery procedure, the pressurizing gas is supplied from the pressurizing gas container to the storage container, the pressurizing gas is enclosed in the storage container, and the inside of the storage container is heated. A second recovery procedure in which the operation of pressing and recovering the liquid component in the recovery tank with this pressure is repeated a plurality of times until the liquid in the storage container reaches a predetermined liquid amount, and the gas component and the pressurizing gas in the storage container. Is supplied to the cooling liquefaction tank at the internal pressure in the storage container to separate the gas component and the pressurizing gas, and the third recovery procedure for liquefying the fluorine-based gas, and the liquid component and gas remaining in the storage container Coolant through components and pressurizing gas via suction pump Was introduced into the vessel, causes separated into fluorine-based gas and pressurization gas by cooling liquefaction,
A fourth recovery procedure for liquefying the fluorine-based gas and a fifth recovery for supplying the pressurizing gas to the cooling liquefaction tank and recovering the liquefied gas of the fluorine-based gas liquefied in the third recovery procedure and the fourth recovery procedure in the recovery tank. It is characterized in that it is collected by the procedure.

In the second aspect of the invention, a device for recovering the liquefied fluorine-based gas is connected to a recovery tank, which is connected to a storage container storing the liquefied fluorine-based gas, and the recovery passage is connected to a liquid tank. A component recovery path and a gas component recovery path are arranged in parallel, a cooling liquefaction tank is attached to the gas component recovery path, and a pressurizing gas container is connected to a storage container, and a pressurizing gas container and a cooling liquefaction tank are provided. It is characterized in that it is configured by connecting.

[0006]

According to the present invention, first, the liquid component of the liquefied fluorinated gas is transferred to the recovery tank by its own pressure in the storage container, and then the pressurizing gas such as nitrogen gas is fed to the storage container so as to Enclose the pressurizing gas in the above, pressurize the inside of the storage container with the pressure of the enclosed pressurizing gas, and transfer the liquid component in the storage container to the recovery tank with this pressurizing force. Repeated multiple times until, until the mixed gas of the gas component and the pressurizing gas in the storage container is introduced into the cooling liquefaction tank at the internal pressure of the storage container for cooling and liquefying, the fluorine-based gas and the pressurizing gas. To liquefy the fluorine-based gas, and introduce the remaining liquid component, gas component and pressurizing gas into the cooling liquefaction tank with a suction pump to liquefy and cool the fluorine-based gas and pressurizing gas. Liquefies the fluorine-based gas to cool and liquefy the tank Since the liquefied fluorine-based gas is transferred to the recovery tank, almost all of the liquefied fluorine-based gas in the storage container can be recovered in the recovery tank, and the pressurizing gas used for pressurization is cooled and liquefied. Since it is separated by doing so, the recovered liquefied fluorinated gas has a high purity in which the pressurizing gas is not mixed.

[0007]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The drawings are flowcharts of a fire extinguishing halon gas recovery apparatus showing an embodiment of the present invention. This fire extinguishing halon recovery device is a storage container that contains the halon to be recovered.
The pressurized gas supply path (5) for connecting the (1) and the recovery tank (2) to each other through the recovery path (3) and for supplying the pressurized gas from the pressurized gas container (4) to the storage container (1) ) Are connected in communication.

The recovery passageway (3) is constructed by connecting a liquid component recovery passageway (6) and a gas component recovery passageway (7) in parallel, and a heat exchanger is provided in the middle of the gas component recovery passageway (7). (8) and adiabatic storage tank
A cooling liquefaction tank (10) composed of (9) and (9) is interposed. A liquefied nitrogen storage container (11) is connected to the cooling liquefaction tank (10). Further, an extruding gas passage (12) branched from the pressurizing gas supply passage (5) communicates with the upper part of the cooling liquefaction tank (10).

A vaporized gas outlet passage (13) is led out from the upper part of the recovery tank (2), and the outlet end of the vaporized gas outlet passage (13) is a gas at the inlet side of the cooling liquefaction tank (10). Component recovery path
It is connected to (7). Also, the gas component recovery path (7)
Entrance to the cooling liquefaction tank (10) and the gas supply path for pressurization
Residual gas extraction and gas replacement passage (14) in a state of communicating with (5)
Is provided, and a diaphragm pump (15) for suction work is interposed in the residual gas extraction / gas replacement passage (14). The storage container (1) is connected to the portion of the residual gas extraction / gas replacement path (14) that serves as the suction path of the diaphragm pump (15), and the storage container (1) is connected to the residual gas extraction / gas replacement path (14). A discharge passage (16) is branched from a portion which serves as a discharge passage of the diaphragm pump (15).

In the figure, reference numeral (17) is an electronic digital platform scale on which the storage container (1) is mounted, (18) is a liquid level gauge for detecting the liquid level in the cooling liquefaction tank (10), and (19) is adiabatic storage. A thermometer for measuring the temperature of the condensate in the tank (9), (20) an on-off valve (21) arranged in the liquefied nitrogen supply path (21) for detecting the temperature of the condensate in the adiabatic storage tank (9) ( Temperature controller for opening and closing 22), (23) Liquefied nitrogen storage container (11)
It is a liquid level gauge that detects the amount of liquid inside.

A fire extinguishing halon recovery procedure in the fire extinguishing halon recovering device thus configured will be described. ◎ Preparation procedure First, the storage container (1) containing the collected halon is placed on the electronic digital platform scale (17), and the recovery path (3) is placed in the storage container.
Connect to the main valve (24) of (1), input the value obtained by adding a constant weight (eg 1 kg) to the empty container weight as a set value to the electronic digital platform scale (17), and activate the diaphragm pump (15). Replace the connection piping system with nitrogen gas.

Further, the amount of liquefied nitrogen in the liquefied nitrogen storage container (11) is confirmed by a liquid level gauge (23), and an on-off valve (22) installed in the liquefied nitrogen supply passage (21) by a temperature controller (20). Is controlled to cool the inside of the cooling liquefaction tank (10) to a predetermined temperature.

◎ First Recovery Procedure After the above preparatory work is completed, the on-off valve (25) mounted on the liquid component recovery path (6) is opened, and the container main valve (24) of the storage container (1) is opened. The valve is opened, and the halon liquid stored in the storage container (1) is pumped to the recovery tank (2) under the internal pressure of the storage container (1).

Second recovery procedure When the pressure switch (26) installed in the recovery path (3) detects that the internal pressure in the storage container (1) has dropped to a predetermined value, the liquid component recovery path (6) The on-off valve (27) installed on the pressurized gas supply path (5) while closing the on-off valve (25) installed on the
Open the valve to supply the nitrogen gas for pressurization from the nitrogen gas container for pressurization (4) into the storage container (1), pressurize the inside of the storage container (1) to a predetermined pressure, and supply the pressurized gas supply path ( Open / close valve attached to 5)
While closing (27), the on-off valve (25) mounted on the liquid component recovery passageway (6) is opened to pump the halon liquid to the recovery tank (2) by the internal pressure in the storage container (1). The electronic nitrogen balance (1
Repeat until the weight detected in 7) reaches the set value.

Third Recovery Procedure Next, the on-off valve (25) mounted on the liquid component recovery passageway (6) is closed and the on-off valve mounted on the gas component recovery passageway (7).
(28) is opened, and the mixed gas of the gaseous component of halon gas and the nitrogen gas for pressurization in the storage container (1) is introduced into the cooling liquefaction tank (10). At this time, since the cooling liquefaction tank (10) has been cooled to a predetermined temperature by the preparatory procedure, the introduced mixed gas is a liquid for cooling while flowing through the heat exchanger (8) of the cooling liquefaction tank (10). It is cooled by exchanging heat with nitrogen, and the halon gas is liquefied due to the difference in condensation temperature between the fluorine-based gas and the nitrogen gas, and stored in the adiabatic storage tank (9). In addition, this cooling liquefaction tank (10)
The cooling temperature at is the solidification temperature of the halon gas (for example, R13
In the case of B1, it is desirable to cool to around 168K). The confirmation of liquefaction is detected by a thermometer (19) that detects the temperature of the adiabatic storage tank (9), the on-off valve (28) attached to the gas component recovery path (7) is closed, and the safety valve circuit (29) is connected. On-off valve fitted (30)
Open the valve to release the nitrogen gas that has not condensed into a safety valve circuit.
Eject from (29). Then, the residual nitrogen gas in the adiabatic storage tank (9) is released to the atmosphere, the on-off valve (30) of the safety valve circuit (29) is closed, and the on-off valve (28) attached to the gas component recovery passageway (7) again. )
Open the valve to cool the mixed gas in the storage container (1) to the cooling liquefaction tank (10).
To introduce. This operation is repeated until the pressure switch (31) arranged in the gas component recovery path (7) reaches a predetermined pressure (approximately atmospheric pressure).

◎ Fourth recovery procedure The opening and closing valves (32) and (33) equipped with the residual liquid remaining in the storage container (1), the residual gas and the nitrogen gas for pressurization are attached to the residual gas extraction and gas replacement passage (14). Diaphragm pump with valve open (15)
Is operated to feed the cooling liquefaction tank (10) to liquefy it, and separate the halon gas and the nitrogen gas.

◎ Fifth recovery procedure The on-off valve (34) attached to the extrusion gas passage (12) is opened to supply the nitrogen gas for pressurization to the adiabatic storage tank (9) of the cooling liquefaction tank (10), Liquefaction stored in the adiabatic storage tank (9) by opening the on-off valve (35) arranged in the portion of the gas component recovery path (7) that is led out from the bottom wall of the adiabatic liquefaction tank (9). Halon is pumped to the recovery tank (2). Then, in order to prevent the nitrogen gas from flowing into the recovery tank (2), the liquid level gauge (18) that detects the liquid level in the adiabatic storage layer tank (9) is used to monitor a certain amount in the adiabatic storage tank (9). Close the on-off valve (35) with the CFC liquid remaining in.

After completion of the fifth recovery procedure, the residual gas extraction / gas replacement passage (14) was installed between the branched portion of the pressurized gas supply passage (5) and the connection portion to the storage container (1). The opening / closing valve (36) is opened to supply a small amount of nitrogen gas into the storage container (1), the main valve (24) of the storage container (1) is closed, and the storage container (1) is removed. Further, when the pressure inside the recovery container (2) rises due to the vaporization of the liquefied halon and the separation of the nitrogen gas dissolved in the liquefied halon, the upper part of the recovery tank (2) and the gas component recovery path.
The on-off valve (37) mounted by the vaporized gas discharge passageway (13) connecting with (7) is opened to move the gas body in the recovery tank (2) from the gas component recovery passageway (7) to the cooling liquefaction tank (10). ), And by cooling it to a temperature near the solidification temperature of halon, it is separated into a halon gas component and a nitrogen gas component, and the halon gas component is liquefied and recovered, and the nitrogen gas component is discharged from the safety valve circuit (29). Discharge.

As described above, according to the method of the present invention, almost all halon can be recovered without releasing it to the atmosphere.
Further, since the collected halon gas contains almost no impurities, it is possible to collect highly pure halon.

In the above embodiment, the case of recovering the fluorine-based gas used for extinguishing a fire has been described, but it goes without saying that it can be used for recovering the fluorine-based gas used as a cooling refrigerant.

[0021]

According to the present invention, the liquid component of the liquefied fluorinated gas is first transferred to the recovery tank by its own pressure in the storage container, and then the pressurizing gas such as nitrogen gas is fed to the storage container for storage. The operation of enclosing the pressurizing gas in the container, pressurizing the inside of the storage container with the pressure of the encapsulating pressurizing gas, and transferring the liquid component in the storage container to the recovery tank by this pressurization Repeated multiple times until the amount reaches a predetermined amount, and then introduce the mixed gas of the gas component and the pressurizing gas into the cooling liquefaction tank at the internal pressure of the storage container to liquefy the cooling, thereby producing the fluorine-based gas and pressurizing gas. Separated into gas, the fluorinated gas is liquefied, and the remaining liquid component, gas component, and pressurizing gas are introduced into the cooling liquefaction tank by the suction pump and liquefied for cooling to form the fluorine-based gas and the pressurizing gas. Separated and liquefied fluorinated gas, cooled Since the fluorine-based gas liquefied in the liquefaction tank is transferred to the recovery tank, almost all of the liquefied fluorine-based gas in the storage container can be recovered in the recovery tank and the pressurizing gas used for pressurization. Since the target gas is separated during cooling and liquefaction of the target gas, the recovered liquefied fluorinated gas can be made into a high-purity gas in which the pressurizing gas is not mixed.

[Brief description of drawings]

FIG. 1 is a schematic configuration diagram of an apparatus showing an embodiment of the present invention.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Storage container, 2 ... Recovery tank, 3 ... Recovery path, 4 ... Pressurization gas container, 6 ... Liquid component recovery path, 7 ... Gas component recovery path, 8 ... Heat exchanger, 9 ... Adiabatic storage tank, 10 ... Cooling liquefaction tank,
15 ... Suction pump, 17 ... Weight detector.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Etsuji Kawaguchi 1095 Katsube Town, Moriyama City, Shiga Prefecture Iwatanipran Tech Co., Ltd. Shiga Factory

Claims (7)

[Claims] 1. When recovering the liquefied fluorine-based gas stored in the storage container (1), first, most of the liquid component in the storage container (1) is stored in the recovery tank (2) by its own pressure. The first recovery procedure for recovering, and the pressurized gas is supplied from the pressurized gas container (4) to the storage container (1) after completion of the first recovery procedure to supply the pressurized gas to the storage container (1).
The inside of the storage container (1) is pressurized by pressurizing the inside of the storage container (1), and the liquid component is recovered in the recovery tank (2) by the applied pressure.
A second recovery procedure in which the liquid component in the storage container (1) is repeated a plurality of times until a predetermined liquid amount is reached, and the gas component and the pressurizing gas in the storage container (1) are stored in the storage container.
It is supplied to the cooling liquefaction tank (10) with the internal pressure in (1) to separate the gas component and the pressurizing gas, and the third recovery procedure for liquefying the fluorine-based gas and the residual gas in the storage container (1) remain. The liquid component and the gas component and the pressurizing gas are introduced into the cooling liquefaction tank (10) through the suction pump (15), and are liquefied by cooling to be separated into the fluorine-based gas and the pressurizing gas, and the fluorine-based gas. The fourth recovery procedure for liquefying the gas, and supplying the pressurizing gas to the cooling liquefaction tank (10) to recover the liquefied gas of the fluorine-based gas liquefied in the third recovery procedure and the fourth recovery procedure in the recovery tank (2). A method of recovering fluorine-based gas, which comprises a fifth recovery procedure. 2. A method for terminating the second recovery procedure by detecting the weight of the storage container (1) with a weight detector (17) and detecting the predetermined weight by the weight detector (17). Item 1. A method for recovering a fluorine-based gas according to Item 1. 3. The fluorine-based gas recovery method according to claim 1, wherein the cooling liquefaction tank (10) is lowered to a temperature near the solidification temperature of the fluorine-based gas. 4. The vaporized gas derived from the upper part of the recovery tank (2) is returned to the inlet of the cooling liquefaction tank (10) to separate the pressurizing gas dissolved in the recovered fluorine-based gas and The method for recovering a fluorine-based gas according to claim 1, wherein the system-based gas is reliquefied. 5. A recovery passageway (3) connected to a storage container (1) storing liquefied fluorine-based gas is connected to a recovery tank (2), and the recovery passageway (3) is a liquid component recovery passageway (6). ) And the gas component recovery path (7) are arranged in parallel to form a gas component recovery path (7).
Fluorine-based gas in which the cooling liquefaction tank (10) is attached to the storage container, the pressurizing gas container (4) is connected to the storage container (1), and the pressurizing gas container (4) and the cooling liquefaction tank (10) are connected. Recovery device. 6. The fluorine-based gas recovery apparatus according to claim 5, wherein the storage container (1) is mounted on the weight detector (17). 7. The fluorine-based gas recovery apparatus according to claim 5, wherein the cooling liquefaction tank (10) comprises a heat exchanger (8) for liquid nitrogen and an adiabatic storage tank (9).