WO2019092934A1 - 無菌液化ガス装置、及び無菌液化ガス装置の取り合い管 - Google Patents
無菌液化ガス装置、及び無菌液化ガス装置の取り合い管 Download PDFInfo
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- WO2019092934A1 WO2019092934A1 PCT/JP2018/027919 JP2018027919W WO2019092934A1 WO 2019092934 A1 WO2019092934 A1 WO 2019092934A1 JP 2018027919 W JP2018027919 W JP 2018027919W WO 2019092934 A1 WO2019092934 A1 WO 2019092934A1
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- liquefied gas
- gas
- supply
- storage tank
- sterilization
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- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2227/00—Transfer of fluids, i.e. method or means for transferring the fluid; Heat exchange with the fluid
- F17C2227/03—Heat exchange with the fluid
- F17C2227/0302—Heat exchange with the fluid by heating
- F17C2227/0309—Heat exchange with the fluid by heating using another fluid
- F17C2227/0323—Heat exchange with the fluid by heating using another fluid in a closed loop
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2227/00—Transfer of fluids, i.e. method or means for transferring the fluid; Heat exchange with the fluid
- F17C2227/03—Heat exchange with the fluid
- F17C2227/0337—Heat exchange with the fluid by cooling
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2227/00—Transfer of fluids, i.e. method or means for transferring the fluid; Heat exchange with the fluid
- F17C2227/03—Heat exchange with the fluid
- F17C2227/0337—Heat exchange with the fluid by cooling
- F17C2227/0341—Heat exchange with the fluid by cooling using another fluid
- F17C2227/0353—Heat exchange with the fluid by cooling using another fluid using cryocooler
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2227/00—Transfer of fluids, i.e. method or means for transferring the fluid; Heat exchange with the fluid
- F17C2227/03—Heat exchange with the fluid
- F17C2227/0367—Localisation of heat exchange
- F17C2227/0369—Localisation of heat exchange in or on a vessel
- F17C2227/0376—Localisation of heat exchange in or on a vessel in wall contact
- F17C2227/0379—Localisation of heat exchange in or on a vessel in wall contact inside the vessel
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2250/00—Accessories; Control means; Indicating, measuring or monitoring of parameters
- F17C2250/04—Indicating or measuring of parameters as input values
- F17C2250/0404—Parameters indicated or measured
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2250/00—Accessories; Control means; Indicating, measuring or monitoring of parameters
- F17C2250/04—Indicating or measuring of parameters as input values
- F17C2250/0404—Parameters indicated or measured
- F17C2250/043—Pressure
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2265/00—Effects achieved by gas storage or gas handling
- F17C2265/01—Purifying the fluid
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2270/00—Applications
- F17C2270/05—Applications for industrial use
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2270/00—Applications
- F17C2270/05—Applications for industrial use
- F17C2270/0509—"Dewar" vessels
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2270/00—Applications
- F17C2270/05—Applications for industrial use
- F17C2270/0518—Semiconductors
Definitions
- the present invention relates to a sterile liquefied gas apparatus and a connecting pipe of the sterile liquefied gas apparatus, and more particularly to a technique suitable for use in producing, storing and supplying liquefied gas such as liquid nitrogen in a sterile condition.
- a technique suitable for use in producing, storing and supplying liquefied gas such as liquid nitrogen in a sterile condition.
- liquefied gases such as aseptic liquid nitrogen are increasingly used. With this, there is a need for a sterile liquefied gas production device.
- Patent Document 1 proposes a method of heating and sterilizing the inside of a liquid nitrogen filling apparatus with a high temperature gas to maintain the sterility of the apparatus.
- Patent Document 2 describes that liquid nitrogen is sterilized using a filter having a cryogenic resistance.
- Patent Document 3 describes cooling and liquefying a sterilized gas, and sterilizing piping and the like with steam.
- Patent Document 4 describes an isolator having a working chamber for performing work on biological material. As described in Patent Document 4, in the isolator, it is necessary to maintain the working chamber in a sterile state.
- Patent Document 2 there is no filter that can maintain the function of sterilizing liquid nitrogen for a long time, and it is not easy to actually produce sterile liquid nitrogen continuously.
- Patent Document 3 describes cooling and liquefying a sterilized gas, and sterilization of piping and the like with steam.
- the supply amount of liquefied gas can not be changed, and high temperature gas is used, and as described later, there is a problem that sterility in liquid nitrogen can not be maintained.
- each of the isolators as described in Patent Document 4 is smaller than, for example, a semiconductor manufacturing facility. For this reason, there is a need for equipment that supplies liquid nitrogen suitable for the size of the scale in which the isolator is used. Furthermore, there is also a demand for being able to supply sterile liquid nitrogen to a plurality of isolators in a single facility, but at the same time there is also a demand not to increase the size of the liquid nitrogen production apparatus.
- the present invention has been made in view of the above-mentioned circumstances, and enables production and supply of sterile liquefied gas (liquid nitrogen), which enables continuous production and sustained supply of sterile liquefied gas, and guarantees sterility.
- An object of the present invention is to provide an aseptic liquefied gas apparatus which can be selectively supplied to a plurality of isolators and the like and which can save labor in the working process.
- a sterile liquefied gas device includes a liquefied gas storage tank, a raw material gas supply device for supplying a raw material gas to the liquefied gas storage tank, and the liquefied gas storage tank
- a cooling device for cooling the inside and liquefying the raw material gas
- a supply pipe connecting the raw material gas supply device and the liquefied gas storage tank
- a sterilization filter provided on the supply pipe, and a downstream side of the sterilization filter It has a sterilizer which sterilizes the sterilizing area located in a part by sterilizing gas, and a sterilizing gas removing device which removes the sterilizing gas after sterilizing.
- the liquefied gas obtained by liquefying the raw material gas may be liquid nitrogen.
- the aseptic liquefied gas device according to the first aspect of the present invention may include a moving device that transports at least the liquefied gas storage tank.
- the sterile liquefied gas device according to the first aspect of the present invention is connected to the liquefied gas storage tank, supplies the liquefied gas stored in the liquefied gas storage tank toward the downstream side of the liquefied gas storage tank, and seals the liquefied gas storage tank.
- a possible supply and a supply sterilizer for sterilizing the supply may be provided.
- the supply unit sterilizing apparatus can supply the liquefied gas in a sterile state to the liquefied gas supply target when the supply unit is connected to the liquefied gas supply target.
- the feeder sterilizer may be capable of performing a sterilization process to sterilize the feeder.
- the sterile liquefied gas device according to the first aspect of the present invention includes a connection sensor that detects that the supply unit is connected to the liquefied gas supply target, and the supply sensor and the liquefied gas supply target are detected by the connection sensor.
- the supply unit sterilizer may be capable of initiating the sterilization process when a connection with it is confirmed.
- the sterile liquefied gas device includes a movement sensor that detects that the liquefied gas storage tank is moving, and detects that the sterile liquefied gas device is moving by the movement sensor.
- the liquefaction process may be made stoppable.
- the intake pipe of the aseptic liquefied gas device is an intake pipe connected to the liquefied gas storage tank and the liquefied gas supply target, and the liquefied gas storage tank and the liquefied gas supply target And an evacuable device capable of evacuating the gas in the inside of the connection pipe in a state in which the inside of the connection pipe is sealed by the valve.
- a sterilizer capable of supplying a sterilizing gas to the inside of the joint pipe in an evacuated state is connected to the joint pipe.
- a sterile liquefied gas device comprises a liquefied gas storage tank, a raw material gas supply device for supplying a raw material gas to the liquefied gas storage tank, and cooling the inside of the liquefied gas storage tank.
- a sterilizer for sterilizing with gas and a sterilizing gas removing device for removing the sterilizing gas after sterilizing are provided.
- the sterilizing gas is supplied from the sterilizer to at least the sterilizing filter, the supply pipe, and the liquefied gas storage tank, which are the sterilizing regions located downstream of the sterilizing filter.
- the sterilization area is gas-sterilized
- the sterilizing gas removing device removes the sterilizing gas, water and the like generated by the gas sterilization
- the sterilizing gas is removed from the sterilization area, and the sterilization process of the sterilization area is completed.
- the raw material gas is supplied from the raw material gas supply device to the aseptic state liquefied gas storage tank through the sterilizing filter, and the inside of the liquefied gas storage tank is cooled by the cooling device to liquefy the raw material gas.
- the sterile liquefied gas is stored in a liquefied gas storage tank. This makes it possible to supply the aseptic liquefied gas produced as needed to the outside.
- the production process of aseptic liquefied gas and the sterilization process incidental to the production process are pressurized in the storage tank and the area where the liquefied gas is produced. There is no For this reason, it is not necessary to maintain the pressure resistance to high pressure in this area, and it becomes possible to save space and reduce the size of the device. Furthermore, the amount of work required for maintenance can be reduced to reduce manufacturing costs and supply costs. In particular, it becomes unnecessary to install large-scale equipment such as large-sized tank installation.
- aseptic means a sterilized state
- sterilization means killing or removing all the microorganisms and viruses present in the object regardless of harm or harm.
- SAL sterility assurance level
- SAL ⁇ 10 -6 Probability of survival of the microorganism to the object after sterilization operation is less than 1,000,000. Means that).
- the liquefied gas is a gas having a normal boiling point of less than -50 ° C., and examples thereof include nitrogen, oxygen, liquid air and argon.
- the sterilizing gas removal apparatus supplies inert gas to discharge and remove sterilizing gas remaining in the sterilizing area, to remove generated water, and the like. Therefore, after the sterilizing apparatus supplies the sterilizing gas and performs sterilization processing, the sterilizing gas removing apparatus supplies the inert gas to the sterilizing area, thereby at least the sterilizing filter, the supply pipe, and the liquefied gas being the sterilization area. It adheres to the inside of the storage tank or discharges and removes the sterile gas stored in the liquefied gas storage tank to the outside.
- the inert gas supplied to the sterilization area by the sterilizing gas removal apparatus can be nitrogen gas at a temperature higher than room temperature, preferably, nitrogen gas at 100 ° C. or more.
- the purity of the production gas is not adversely affected, which is preferable.
- the procedure of using the air at the beginning and switching from the air to the inert gas at a later time to perform sterilization is excellent in cost, and the above-mentioned adverse effects can be avoided, and both advantages can be compatible. Therefore, it is preferable.
- the gas supply flow rate in the sterilization gas removal process is set larger than the supply flow rate from the raw material gas supply device at the time of producing the liquefied gas, in order to shorten the sterilization gas removal process.
- region can be set lower than 100 degreeC by pressure-reducing sterilization area
- the sterilization apparatus and the sterilization gas removal apparatus are in a sterilization area. It will be in the state connected more upstream.
- sterilization processing and sterilization gas removal processing can be performed on the entire sterilization area, it becomes possible to manufacture sterile liquefied gas with the entire sterilization area kept aseptic, and manufactured. It is possible to guarantee the sterility of liquefied gas.
- the supply pipe is connected to the upper portion of the liquefied gas storage tank, thereby eliminating the need to penetrate the supply pipe to the side surface and the bottom surface of the liquefied gas storage tank. Therefore, the surface treatment on the inner surface of the liquefied gas storage tank can be easily brought into a predetermined state.
- the surface to be in contact with the liquefied gas or the inner surface of the sterilization area is in a state where the sanitary specification is satisfied.
- sanitary standards are standards used in the manufacture of food, dairy, brewery, beverages, confectionery, fishery, medicine, cosmetics, chemical products, soft drinks, beer, liquor, meat processing, chemical liquids, semiconductors, etc.
- the cooling device includes a refrigerator
- the inside of the liquefied gas storage tank can be easily cooled to the temperature at or below the liquefied gas temperature of the raw material gas, and the liquefied gas stored in the liquefied gas storage tank can be stored. It can be manufactured in large quantities.
- the liquefied gas obtained by liquefying the raw material gas is changed to liquid nitrogen, so that the working room is maintained in a sterile state, which could not conventionally be realized. It is possible to easily supply sterile liquid nitrogen to an isolator or the like that needs to be done, while ensuring sterility.
- the aseptic liquefied gas apparatus which concerns on the 1st aspect of this invention is equipped with the transfer apparatus which makes at least the said liquefied gas storage tank portable.
- liquefied gas liquid nitrogen
- the storage tank is moved after production of the liquefied gas is finished, and the sterile condition is maintained in a desired device etc.
- the storage tank acts as a mere dewar, so to speak.
- the power supply necessary for the sensor and control to the sterile liquefied gas device is simply performed. And do not always need the high power needed during liquefied gas production. For this reason, it can be set as a portable structure only by UPS (uninterruptible power supply).
- UPS uninterruptible power supply
- the sterile liquefied gas device is connected to the liquefied gas storage tank, and supplies the liquefied gas stored in the liquefied gas storage tank toward the downstream side of the liquefied gas storage tank.
- a supply sterilizer for sterilizing the supply part According to this configuration, the storage tank is moved and connected to the supply target, and the supply portion sterilizing apparatus sterilizes the pipes and the like in the supply portion and the isolator which is the connection target.
- the liquefied gas stored in the storage tank can be easily supplied to the connection target through the sterile supply unit, the connection target piping, and the like in a sterile state. This makes it possible to supply sterile liquefied gas to a plurality of supply targets at a desired location and at any timing.
- the supply unit sterilizing device is configured to supply the liquefied gas in a sterile state as the liquefied gas supply target when the supply unit is connected to the liquefied gas supply target. It is possible to supply, and the supply unit sterilizer is capable of performing a sterilization process to sterilize the supply unit. With this configuration, only by moving the storage tank and connecting it to the supply target, the supply unit sterilizer starts sterilization processing for the supply unit with this supply unit, and the liquefied gas stored in the storage tank is kept aseptic, It can be easily supplied to the connection target through a sterile supply.
- the sterile liquefied gas device includes a connection sensor that detects that the supply unit is connected to the liquefied gas supply target, and the supply sensor and the liquefied gas are detected by the connection sensor.
- the supply unit sterilizer can start the sterilization process when the connection with the supply target is confirmed. With this configuration, after the connection sensor confirms the connection to the supply target of the connection unit, the sterilization process is started to prevent the connection target to be supplied from becoming non-sterile, and storage in the storage tank With respect to the aseptic liquefied gas that has been supplied, it is possible to reliably supply aseptically guaranteed conditions.
- the sterile liquefied gas device includes a movement sensor that detects that the liquefied gas storage tank is moving, and the sterile liquefied gas device is moving by the movement sensor.
- the liquefaction process can be stopped if it detects. According to this configuration, since the liquefaction process is not performed during the movement of the aseptic liquefied gas device, it is possible to prevent the liquefied gas from leaking from the storage tank. Due to the connection between the storage tank and the external space, the internal space of the storage tank and the stored liquefied gas can be prevented from being contaminated and becoming non-sterile.
- the intake pipe of the aseptic liquefied gas device is an intake pipe connected to the liquefied gas storage tank and the liquefied gas supply target, and the liquefied gas storage tank and the liquefied gas supply target And an evacuable device capable of evacuating the gas in the inside of the connection pipe in a state in which the inside of the connection pipe is sealed by the valve.
- a sterilizer capable of supplying a sterilizing gas to the inside of the joint pipe in an evacuated state is connected to the joint pipe.
- connection portion when the sterile liquefied gas is supplied to the liquefied gas supply target, the connection portion is sterilized in a state where the liquefied gas storage tank and the liquefied gas supply target are connected, and the sterile liquefied gas stored is stored. It is possible to supply a sterile liquefied gas to a liquefied gas supply target while maintaining the sterile condition.
- the sterilizing gas is used to sterilize and remove the sterilizing area where the liquefied gas is produced and stored.
- the sterilizing gas is used to sterilize and remove the sterilizing area where the liquefied gas is produced and stored.
- FIG. 1 is a schematic cross-sectional view showing a sterile liquefied gas device in the present embodiment, and in the figure, reference numeral 10 is a sterile liquefied gas device.
- the aseptic liquefied gas device 10 includes a liquefied gas storage tank 11, a raw material gas supply device 12, a cooling device 13, a supply piping 14, a sterilization filter 14d, and a sterilization device.
- a sterilizing gas removing device 17 and a liquefied gas supply unit 18 (connection pipe) are provided.
- the liquefied gas storage tank 11 is, as shown in FIG. 1, a closed cylindrical container with a bottom, and has a sanitary specification as described later. As shown in FIG. 1, the liquefied gas storage tank 11 is provided with a supply pipe 14, a connection pipe 18, and a cooling device 13 penetrating through a lid portion 11 a which is an upper end.
- the bottom portion 11b of the liquefied gas storage tank 11 is formed with a slope which gently falls from the connection position between the bottom portion 11b and the side wall 11c toward the center of the bottom portion 11b.
- a recess is formed in the center of the bottom portion 11b, and the recess forms a reservoir recess 11d.
- the bottom portion 11b is formed, for example, in the shape of a curved surface obtained by cutting a spherical surface, and when the pressure difference is generated between the liquefied gas storage tank 11 and the outside, the strength of the liquefied gas storage tank 11 can be maintained. It is done.
- the source gas supply device 12 is configured to supply a source gas, which is a source of liquefied gas, to the liquefied gas storage tank 11, and is connected to the supply piping 14 via a valve 14a.
- the source gas supply device 12 supplies nitrogen gas as the source gas to the liquefied gas storage tank 11.
- the source gas supply device 12 supplies, for example, a source gas at about room temperature to the liquefied gas storage tank 11.
- the raw material gas supply device 12 according to the present embodiment has a nitrogen generator (PSA) using an adsorbent, efficiently separates oxygen and nitrogen from air, and up to 99.99% nitrogen gas. It can be supplied to the liquefied gas storage tank 11.
- the configuration of the source gas supply device 12 is not limited to the above configuration as long as the source gas can be supplied to the liquefied gas storage tank 11.
- the cooling device 13 is a refrigerator system, and as shown in FIG. 1, it is connected to a cooling unit 13a of a mechanical refrigerator penetrating the lid 11a which is the upper end of the liquefied gas storage tank 11, and the cooling unit 13a.
- a compressor 13 b for supplying and recovering a refrigerant gas and a water cooling unit 13 c connected to the compressor 13 b are provided.
- the cooling unit 13a penetrates the lid 11a and protrudes inside the liquefied gas storage tank 11, and is configured so that the raw material gas exchanges heat with the cooling unit 13a of the mechanical refrigerator and is liquefied.
- the cooling unit 13a can cool the refrigerant (for example, helium gas) supplied from the compressor 13b to, for example, an ultra-low temperature of 80 K by performing Simon expansion.
- the compressor 13 b has, for example, a configuration in which helium gas is circulated between the cooling unit 13 a and the compressor 13 b to take heat from the cooling unit 13 a. This heat is dissipated to the outside by the water cooling unit 13c.
- the structure (air cooling) which carries out a waste heat directly outside by compressor 13b without providing the water cooling part 13c is also employable.
- the cooling unit 13a protruding into the liquefied gas storage tank 11 is configured such that the surface thereof meets the sanitary specification.
- the downstream side of the supply pipe 14 penetrates the lid portion 11 a, which is the upper end of the liquefied gas storage tank 11, and is positioned in the axial direction at the center of the liquefied gas storage tank 11. It is provided to extend vertically in the interior of the. A large number of through holes are provided over the entire length of the supply pipe 14 extending inside the liquefied gas storage tank 11 over the entire length, and the inside of the supply pipe 14 extending inside the liquefied gas storage tank 11 and the liquefaction The interior of the gas storage tank 11 is in communication.
- a sterilization filter 14 d is provided on the upstream side of the supply pipe 14. Furthermore, the piping located upstream of the sterilizing filter 14 d is formed to branch into three.
- the source gas supply device 12, the sterilizer 16, and the sterilizing gas removing device 17 are connected to the branched piping through the valves 14a, 14b, and 14c, respectively.
- bulb 14a, 14b, 14c can also be comprised with three independent valve
- the sterilizing filter 14 d is provided in the supply pipe 14 and is a filter that can sterilize the source gas supplied from the source gas supply device 12.
- the filtration performance of the sterilizing filter 14d can be exhibited at around room temperature.
- the sterilization filter 14 d is formed of a material and a shape in which the filtration performance is not reduced by the sterilizing gas supplied from the sterilization device 16.
- the sterile filter means a sterile filter that can be sterilized.
- the sterile filter 14d, the supply pipe 14 located downstream of the sterile filter 14d, the inside of the liquefied gas storage tank 11, and the connecting pipe 18 extending to the valve 18a are used as a sterile area S.
- the sterilization area S is sterilized from the start of the production of the liquefied gas to the end of the supply in order to make the produced liquefied gas aseptic as well as supply the stored liquefied gas to the liquefied gas storage tank 11 in the aseptic condition. Maintaining the Condition
- the sterilization filter 14d for example, a hydrophobic PTFE membrane filter for gas sterilization manufactured by PALL can be employed.
- the sterilization filter 14d has a configuration in which a plurality of flow paths can be switched inside the sterilization filter 14d, and for example, two or three filters can be switched in parallel. There is.
- the sterilizing filter 14d can be provided with an integrity test device 19A for confirming and testing that the sterility of the sterilizing filter 14d can be maintained.
- the integrity test apparatus 19A includes a valve 19Aa provided upstream of the sterilization filter 14d of the supply piping 14, a valve 19Ab provided downstream of the sterilization filter 14d of the supply piping 14, a valve 19Aa and a sterilization filter 14d. Between the valve 19Ac provided at a position between the supply pipe 14 and the valve 19Ac, a valve 19Ad provided at a position between the valve 19Ab and the sterilizing filter 14d so as to branch from the supply pipe 14, and a valve 19Ac And a integrity test unit 19B connected to branch from the supply pipe 14 at the branch position.
- the integrity testing apparatus 19A After the valves 19Aa, 19Ab, 19Ac are closed and the valve 19Ad is opened, for example, pure water is supplied from the integrity testing unit 19B and passes the sterilization filter 14d. The purified water is collected from the valve 19Ad. The collected pure water is inspected to confirm that the aseptic condition in the filter is maintained.
- valves 19Ab, 19Ad are closed, the valves 19Aa, 19Ac, 19Ad are opened, and then the valve 14c is opened.
- Supply purge gas As a result, it is possible to remove water and the like remaining after the integrity test, and to perform water removal and drying in the sterilization area S.
- valves 19Ab, 19Ac are closed, and the valves 19Aa, 19Ad, 14c are opened, and then a purge gas such as an inert gas is supplied from the sterile gas removal device 17.
- a purge gas such as an inert gas
- the "integrity test” in the present invention includes methods that differ depending on the filter used.
- the “integrity test” is aseptically carried out based on “JIS K 3832 or JIS K 3833 or the adopted instruction manual of the filter as described in page 3 of JIS K 3835, 6.3 (1) (b). Conduct integrity testing to ensure that there are no defects such as breakage of the test filter. "
- the invention is characterized in that the integrity testing device can additionally be attached to a sterile liquefied gas device not equipped with the integrity testing device.
- the integrity testing device can additionally be attached to a sterile liquefied gas device not equipped with the integrity testing device.
- “being able to perform an integrity test according to the method specified in JIS K 3832 or JIS K 3833 or the filter instruction manual adopted is a necessary configuration according to the present invention.
- the sterile liquefied gas device 10 can perform an integrity test by separating the filter portion from the system of the present device (sterile liquefied gas device 10).
- the valve 19Aa for closing the upstream pipe and the valve 19Ab for closing the downstream pipe are required, and the sterilization filter 14d to the integrity tester 19B.
- the integrity tester 19B There is a need for an arrangement with a blank flange that allows connection and disconnection of the flow path towards the.
- valves 19Ad and 19Ac drain valves
- the integrity tester 19 B is built into the sterile liquefied gas device 10.
- the integrity tester 19B is not a device always required for the sterile liquefied gas device 10.
- the piping connected to the filter 18b and the arrangement of the valves provided in this piping are the same as the arrangement of the piping connected to the sterilizing filter 14d described above and the valves provided in this piping , I omit the explanation.
- the configuration in which the integrity tester 19B is permanently installed in the sterile liquefied gas device 10 is safer. Therefore, in the following description, the case where the integrity tester 19B is permanently installed in the sterile liquefied gas apparatus 10 is described.
- JIS K 3833 is used as an integrity test.
- the “2. diffusion flow rate test” described in JIS K 3833 and the description after paragraph 0045 are basically similar. Therefore, for details, it is preferable to reflect the description of JIS K 3833.
- All the filters were wetted according to the procedure of "7.1. (2)" described in JIS K 3833. The procedure is as follows: “7.1. (2) (e)” by charging pure water from the integrity tester side and filling the primary side with pure water with the valve 19 Ac closed or opened slightly. To achieve.
- the sterilizer 16 can supply a sterilizing gas such as hydrogen peroxide or ethylene oxide gas to the sterilizing area S, for example, and is connected to the branched supply pipe 14 via the valve 14 b.
- a sterilizing gas supply device capable of generating a sterilizing gas such as a hydrogen peroxide gas or an ethylene oxide gas can be employed.
- hydrogen peroxide gas is given high frequency or microwave energy under high vacuum and 100% ionized (ionized), that is, hydrogen peroxide gas supplied
- ionized 100% ionized
- hydrogen peroxide gas supplied Apply a configuration utilizing low temperature gas plasma method or a configuration utilizing hydrogen peroxide gas low temperature sterilization (hydrogen peroxide vapor sterilization method) to vaporize hydrogen peroxide with a heating vaporizer and supply the vapor thereof It is possible.
- a sterilizing gas of a type conforming to the standard of the supply target to which the sterilizing gas is supplied from the sterilizer 16 can be used, and besides hydrogen peroxide gas, ethylene oxide, propylene oxide, formaldehyde , it is possible to use ozone, a gas such as NO 2.
- the valve 14b is opened, the valve 14a and the valve 14c are closed, and the sterilizing gas is supplied to the inside of the aseptic liquefied gas apparatus 10 by the sterilizer 16 to provide the sterilization area S located downstream of the sterilization filter 14d. Gas sterilization is possible.
- the inside of the sterilization area S is depressurized by an exhaust device such as a vacuum pump, the substance (gas, liquid, etc.) in the sterilization area S is exhausted, and the sterilizing gas is introduced into the sterilization area S.
- an exhaust device such as a vacuum pump is disposed on the downstream side of the connection pipe 18, for example, at the downstream position of the valve 18a or at the downstream position (outside position) of the valve 18c so as to spread the sterilizing gas throughout the sterilization area S.
- the pump can also be provided or connectable to this position.
- the concentration of the sterilizing gas is increased by evacuating the sterilization area S and replacing the residue in the sterilization area S with the sterilization gas, and the sterilization area S is uniformly sterilized. It becomes possible.
- the sterilizing gas removal apparatus 17 supplies a purge gas such as an inert gas toward the inside of the aseptic liquefied gas apparatus 10 to remove the sterilizing gas remaining after gas sterilization, water generated by the gas sterilization, and the like.
- the inside of the sterilization area S is degased and dried.
- the inert gas to be supplied may be, for example, nitrogen gas.
- water in the sterilization area S can also be removed along with the removal of residual sterilization gas, if further drying is required, nitrogen gas is supplied at a large flow rate with respect to the raw material gas supply amount of liquefied gas. It is preferable to make it possible.
- the inside of the sterilization area S is depressurized by an exhaust device such as an exhaust pump, and the substance (gas, liquid, etc.) in the sterilization area S is exhausted. It is also possible to carry out the removal of In this case, in order to be able to remove the sterilizing gas from the entire sterilization area S, an exhaust device such as a pump at the downstream side of the connection pipe 18, for example, the downstream position of the valve 18a or the downstream position (outside position) of the valve 18c. Or the pump can be connectable to this position.
- an exhaust device such as a pump at the downstream side of the connection pipe 18, for example, the downstream position of the valve 18a or the downstream position (outside position) of the valve 18c.
- the pump can be connectable to this position.
- connection pipe 18 (supply part) penetrates the lid portion 11 a which is the upper end of the liquefied gas storage tank 11 and is located in the central axial direction of the liquefied gas storage tank 11.
- the gas storage tank 11 is provided so as to extend vertically inside.
- connection pipe 18 is maintained at a position lower than the liquid level of the liquefied gas stored in the liquefied gas storage tank 11 when the liquefied gas is supplied to the liquefied gas storage tank 11, and the liquefied gas storage tank It is sufficient that the liquefied gas stored in 11 can be supplied to the outside through the connection port 18 through the outlet.
- the upstream end of the connection pipe 18 be disposed so as to substantially contact the storage recess 11 d.
- the upstream end of the connection pipe 18 can be arranged to be in substantially contact with the central portion which is the lowest position of the storage recess 11d.
- the connection pipe 18 can be used as a drain capable of discharging the water and the like accumulated in the storage recess 11 d at the time of sterilization by disposing the upstream end of the connection pipe 18.
- a valve 18a is provided downstream of the connection pipe 18 at a position serving as an outlet for supplying the liquefied gas stored in the liquefied gas storage tank 11 to the outside, and the connection pipe 18 and the liquefied gas storage tank 11 are exposed to the outside And can be sealed.
- a flow branched from the flow path (first flow path) extending from the liquefied gas storage tank 11 to the valve 18a at a position between the valve 18a and the liquefied gas storage tank 11 A passage (second flow passage) is provided.
- the branched flow path (second flow path) is provided with a valve 19Ae, a filter 18b, and a valve 18c described later.
- valve 18c The downstream side of the valve 18c communicates with the outside, and when the liquefied gas is stored in the liquefied gas storage tank 11, excess gas that evaporates is released to the outside so that the internal pressure of the liquefied gas storage tank 11 does not rise.
- the valve 18c may be configured to operate as a safety valve that operates when the internal pressure of the liquefied gas storage tank 11 rises above a predetermined value.
- the filter 18b is provided with an integrity test device 19A connected to the integrity test unit 19B described above as a device for confirming and checking that the sterility of the filter can be maintained. It can also be done.
- the integrity testing device 19A for the filter 18b is a valve 19Ae branched from the connection pipe 18 and provided upstream of the filter 18b, and a valve 19Af provided to branch from the pipe between the valve 19Ae and the filter 18b.
- a valve 19Ag provided to branch from the pipe between the valve 18c and the filter 18b, a pipe 19Aw connected to the integrity test unit 19B at a branch position of the valve 19Af, a pipe 19Aw, and a supply pipe 14
- a valve 19Av connecting the downstream position of the valve 19Ab.
- the integrity testing apparatus 19A for the filter 18b for example, pure water is supplied from the integrity testing unit 19B after the valves 19Ae, 19Av, 18c are closed and the valves 19Af, 19Ag are opened. Pure water having passed through the filter 18b is collected from the valve 19Ag. The collected pure water is inspected to confirm that the aseptic condition in the filter is maintained.
- valves 19Ae and 18c are closed, and the valves 19Af, 19Ag and 19Av are opened, and then the valve 14c is opened, and an inert gas or the like is output from the sterilizing gas removing device 17 described later.
- Supply purge gas As a result, it is possible to remove moisture and the like remaining after the integrity test and to remove and dry the moisture of the connection pipe 18 and the like.
- the integrity test for the sterilizing filter 14d and the integrity test for the filter 18b can be performed simultaneously.
- connection pipe 18 downstream of the valve 18a is directly connected to the area such as an isolator using sterile liquefied gas in the medical, pharmaceutical, food and research fields, etc. via the pipe, and from this outlet It is possible to supply the aseptic liquefied gas taken out outside.
- the liquefied gas storage tank 11 is provided with a pressure detection device that measures the internal pressure, a temperature detection device that measures the internal temperature, and an internal state display device 11 f that displays the detection results of these.
- a pressure detection device that measures the internal pressure
- a temperature detection device that measures the internal temperature
- an internal state display device 11 f that displays the detection results of these.
- the devices that need to be communicated to the outside of the liquefied gas storage tank 11 are all disposed so as to penetrate the lid portion 11 a which is the upper end of the liquefied gas storage tank 11.
- a plurality of temperature detection devices can be provided inside the liquefied gas storage tank 11.
- the upper position of the side wall of the liquefied gas storage tank 11 as a position where the temperature detection device is installed
- the position in the vicinity of the cooling unit 13a which can detect the temperature of the cooling unit 13a, the position in the vicinity of the bottom 11b which is the lower end of the liquefied gas storage tank 11, and the like can be mentioned.
- the supply piping 14 which is the sterilization area S, the sterilization filter 14 d, the liquefied gas storage tank 11, the connection piping 18 connected to the cooling unit 13 a, the valve 18 a, and the connection piping 18 connected to the valve 18 c.
- the surface or the inner surface of the pressure detection device or the temperature detection device is configured to meet the sanitary specification.
- stainless steel materials in particular, SUS316 and SUS316L can be mentioned.
- a mirror polishing process for polishing the surface of a stainless steel material using a # 400 polishing agent and an electrolytic polishing process are performed to achieve specifications conforming to a stainless steel sanitary pipe or the like defined in JIS standards.
- the surface of the above-described stainless steel material or the surface subjected to the above-described treatment may be covered with a metal such as Au or Pt.
- joints of piping, O-ring, etc. which were mentioned above can use fluororubber etc., such as a product made from silicone, fluorine resin, vinylidene fluoride type (FKM) etc., as a sanitation standard.
- fluororubber etc. such as a product made from silicone, fluorine resin, vinylidene fluoride type (FKM) etc., as a sanitation standard.
- FIG. 2 is a flow chart showing a liquefied gas production process in the sterile liquefied gas device according to the present embodiment.
- the method for producing sterile liquefied gas in the sterile liquefied gas device 10 includes integrity test step S21, sterilization step S1, sterilization gas removal step S2, and raw material gas supply step S3. And liquefaction cooling step S4.
- integrity test process S21 may not be performed, when the integrity test process S21 is performed, the integrity test process is performed at a predetermined periodic timing and is not always an essential process.
- the sterile liquefied gas production method in the sterile liquefied gas device 10 first sterilizes the sterilization area S as a sterilization step S1 shown in FIG.
- the sterilization step S1 first, the valve 14a and the valve 14c are closed, the valve 14b is opened, the cooling device 13 is stopped, the source gas supply device 12 is stopped, and the valve 18a is opened. , And the valve 18c is opened.
- the sterilizer 16 is operated, and the sterilizing gas as hydrogen peroxide gas set to about 100 ° C. supplied from the sterilizing gas supply device is supplied to the branched supply pipe 14 through the valve 14 b.
- the sterilizing gas is an outlet located on the downstream side of the connection pipe 18 connected to the valve 18a through the supply pipe 14, the sterilization filter 14d, the liquefied gas storage tank 11, and the connection pipe 18 which are the sterilization area S via the valve 14b.
- the filter 18b provided in the branched flow path (second flow path), it is discharged from the valve 18c.
- the sterilizing gas comes in contact with the inner surface of the sterilizing region S, and the sterilizing process is performed on the inner surface of the sterilizing region S in contact with the sterilizing gas, thereby killing the bacteria from the inner surface of the sterilization region S.
- the processing conditions in the sterilization step S1 can adopt the sterilization conditions necessary in, for example, a lyophilizer for medicine, in order to obtain complete aseptic conditions. Under such processing conditions, the sterilization area S is exposed to hydrogen peroxide gas for about 30 minutes to 45 minutes to kill bacteria by maintaining the exposure state.
- the valve 18a is closed, the valve 18c is closed, the pressure in the sterilization area S is reduced, and the substance in the sterilization area S is exhausted. Thereafter, the sterilizer 16 can be operated to assist the introduction of sterilizing gas to the sterilizing area S.
- an exhaust device such as a vacuum pump
- the valve 18a is closed, the valve 18c is closed, the pressure in the sterilization area S is reduced, and the substance in the sterilization area S is exhausted. Thereafter, the sterilizer 16 can be operated to assist the introduction of sterilizing gas to the sterilizing area S.
- the valve 14b is closed, the valve 14c is opened, the valve 18a is opened, and the valve 18c is opened.
- the sterilizing gas removal apparatus 17 is operated to supply the supply pipe 14 with an inert gas having a temperature higher than room temperature, preferably 100 ° C. or more.
- the inert gas to be nitrogen gas passes through the valve 14 c through the supply piping 14, the sterilization filter 14 d, the liquefied gas storage tank 11, and the connection piping 18 which are the sterilization area S, and the valve at the lower end of the discharge piping 18. It is discharged from the lower end of the outlet located on the side 18a and the lower end of the branch pipe (second flow path) located on the side of the valve 18c.
- the sterilization gas used in the gas sterilization in the sterilization step S1 is discharged and removed to clean and dry the inside of the sterilization area S.
- the flow rate is compared with the supply of the source gas from the source gas supply device 12 in the liquefaction cooling step S4 described later.
- a high temperature inert gas is supplied from the sterilizing gas removal unit 17
- the high temperature inert gas supplied from the sterilizing gas removal apparatus 17 is supplied into the sterilization area S in the aseptic condition in which the bacteria are killed by passing through the aseptic filter 14d.
- the sterilizing gas removal step S2 water and the like adhering to the inner surface of the sterilizing area S is evaporated by the high temperature inert gas supplied from the sterilizing gas removal apparatus 17 and discharged from the connection pipe 18. After confirming that the water adhering to the inside of the liquefied gas storage tank 11 and the inner surface of the sterilization area S is completely discharged to the outside, the operation of the sterilization gas removal apparatus 17 is stopped and the sterilization gas removal process S2 is finished. Do.
- the integrity test with respect to the above-mentioned sterilization filter 14d and filter 18b is performed according to the procedure of the JIS description mentioned above.
- the integrity test step S21 is performed prior to the sterilization step S1. This is because there is a possibility that the portions of the sterilization filter 14d and the filter 18b may become wet, and also to prevent contamination from the outside by opening and closing the valves 19Ad and 19Ac (drain valves).
- the valve 14c is closed and the valve 14a is opened.
- the valve 18a located on the outlet side is closed, and the valve 18c is closed.
- the source gas supply device 12 is operated to supply nitrogen gas, which is the source gas, to the liquefied gas storage tank 11.
- the raw material gas supplied from the raw material gas supply device 12 flows through the supply pipe 14 through the sterilizing filter 14d and flows into the liquefied gas storage tank 11, but the range where the raw material gas flows in is from the sterilizing filter 14d. It is the downstream sterile area S. Since all sterilization processing by the sterilization apparatus 16 is completed, the portion to be the sterilization area S downstream of the sterilization filter 14d can maintain sterility.
- the cooling device 13 is operated as a liquefaction cooling step S4 shown in FIG. 2, and the compressor 13b circulates helium gas between the compressor 13b and the cooling unit 13a to remove heat from the cooling unit 13a. Is discharged to the outside by the water cooling unit 13c. As a result, the cooling unit 13a which penetrates the lid 11a and protrudes inside the liquefied gas storage tank 11 is cooled, thereby cooling the inside of the liquefied gas storage tank 11 and liquefying the raw material gas.
- the liquefied source gas is stored inside the liquefied gas storage tank 11. As needed, by pressurizing the inside of the liquefied gas storage tank 11 with the sterilizing gas removal apparatus 17 etc., the aseptic liquefied gas stored in the liquefied gas storage tank 11 is made to the outside from the outlet through the valve 18a in the open state. It becomes possible to supply.
- the raw material gas can be supplied to the liquefied gas storage tank 11 while the valve 18a or the valve 18c located on the outlet side is open. This is because the inside of the liquefied gas storage tank 11 in the sterilization gas removal step S2 is higher than the atmospheric pressure (1 atm + ⁇ ), and the temperature is also high. This is because even if the cooling device 13 is operated, it does not cool immediately, and the pressure in the liquefied gas storage tank 11 rises to the supply pressure of the source gas supply device 12.
- the raw material gas supply by the raw material gas supply device 12 is adjusted so that the inside of the liquefied gas storage tank 11 becomes the atmospheric pressure + ⁇ in order to make the flow of gas one direction so that bacteria do not enter.
- the valve 18a is closed and the valve 18c is opened and the liquefaction cooling step S4 is started, bacteria are not introduced from the valve 18c because the filter 18b is provided.
- the valve 18a located on the outlet side is maintained in the closed state, and the valve 18c provided in the branched flow path is maintained in the open state. Furthermore, when the liquid of the liquefied gas is stored in a state where the raw material gas is not supplied and liquefied gas production is not performed, the pressure in the liquefied gas storage tank 11 is increased by evaporation of the raw material gas due to heat input. Therefore, the internal pressure of the liquefied gas storage tank 11 is controlled to be lowered to the set value by interlocking the pressure detection device (not shown) and the valve 18c. When the valve 18c is operated as a safety valve, the valve 18c is maintained in the open state.
- the sterilization area S is made sterile by the sterilization step S1 and the sterilization gas removal step S2. Since the sterility process can be performed to liquefy the raw material gas, the aseptic liquefied gas can be produced. Furthermore, since the sterility is maintained in this way, it is possible to guarantee the sterility of the produced aseptic liquefied gas.
- the sterilization filter 14d is made sterile by the sterilization step S1 and the sterilization gas removal step S2.
- the raw material gas is supplied from the raw material gas supply device 12 to the liquefied gas storage tank 11 through the supply piping 14 so that the raw material gas in a sterile state is transferred to the inside of the liquefied gas storage tank 11 via the sterilization filter 14d. It is possible to carry out liquefaction processing.
- the upstream end portion of the connection pipe 18 is provided at a position close to a position where the storage recess 11d contacts the storage recess 11d. For this reason, it becomes possible to supply the liquefied gas stored in the liquefied gas storage tank 11 for as long as possible. Further, since the storage recess 11d is provided on the bottom surface of the bottom portion 11b of the liquefied gas storage tank 11, the liquefied gas is collected along the inclined surface (angle) formed on the bottom surface of the bottom portion 11b to store the stored liquefied gas. It becomes possible to supply outside.
- FIG. 3 is a schematic front view showing the sterile liquefied gas device in the present embodiment.
- the present embodiment differs from the above-described first embodiment in terms of the supply unit.
- the same members as in the first embodiment are given the same reference numerals, and the description thereof will be omitted or simplified.
- an intake pipe 19 (supply unit) is provided on the downstream side of the valve 18 a of the connection pipe 18.
- the intake pipe 19 is connected to the sterile liquefied gas device 10 and an external device to be supplied with liquefied gas from the sterile liquefied gas device 10. That is, the connection pipe 19 has a function as a supply unit.
- sterilization processing is performed to maintain the sterilization state of the device to be supplied (the opposite device) and the supplied liquefied gas.
- FIG. 3 illustration of a part of integrity test apparatus 19A is abbreviate
- connection pipe 19 is connected to the downstream side of the valve 18 a of the connection pipe 18.
- the other end of the intake pipe 19 is a main pipe 19a connected to the pipe 51 of the isolator 5 (target for supplying liquefied gas) to which the liquefied gas stored in the liquefied gas storage tank 11 is supplied, and a branch pipe 19b branched from the main pipe 19a.
- the main pipe 19a has clamps 19c and 19d (connecting members) located at both ends of the main pipe 19a.
- the clamp 19 c can be connected to the end of the pipe 51 of the isolator 5.
- the clamp 19 d can be connected to the lower end (extraction port) of the connection pipe 18 connected to the liquefied gas storage tank 11.
- the clamps 19c and 19d are both one-touch clamps, and can be easily removed.
- a joint made of a sanitary ferrule is used so as not to cause a step.
- the clamp 19 c is provided with a connection sensor that detects a connection state when the connection pipe 19 and the pipe 51 are connected.
- a connection sensor that detects a connection state when the connection pipe 19 and the pipe 51 are connected.
- a proximity sensor can be used, or a voltage of about 5 V can be applied to the pipe, and detection can be performed using a current flowing at the time of connection.
- connection pipe 19b communicates with the main pipe 19a, and the other end of the branch pipe 19b is connected to a vacuum pump 19f via a valve 19e.
- the vacuum pump 19 f can depressurize the internal space of the connection pipe 19 to exhaust the gas inside the connection pipe 19.
- the branch pipe 19b is also connected to a device capable of supplying a sterilizing gas via a valve 19g, specifically, a measuring device 19h connected to the sterilizer 16 and measuring the degree of vacuum inside the branch pipe 19b. It is provided.
- the measuring device 19h it is preferable to use a diaphragm vacuum gauge as a measuring device which is not affected by the sterilizing device.
- These connection tubes 19 are configured such that their surface or inner surface meets the sanitary specification.
- stainless steel materials in particular, SUS316 and SUS316L can be mentioned.
- a mirror polishing process for polishing the surface of a stainless steel material using a # 400 polishing agent and an electrolytic polishing process are performed to achieve specifications conforming to a stainless steel sanitary pipe or the like defined in JIS standards.
- the surface of the above-described stainless steel material or the surface subjected to the above-described treatment may be covered with a metal such as Au or Pt.
- joints of piping, O-ring, etc. which were mentioned above can use fluororubber etc., such as a product made from silicone, fluorine resin, vinylidene fluoride type (FKM) etc., as a sanitation standard.
- fluororubber etc. such as a product made from silicone, fluorine resin, vinylidene fluoride type (FKM) etc., as a sanitation standard.
- connection pipe 19 valves 18a of the connection piping 18, clamps 19c and 19d, valves 51a, valves 19e and 19g, vacuum pump 19f, measuring device 19h, and sterilizer 16 constitute a feeder sterilizer.
- the intake pipe 19 is used when supplying the liquefied gas stored in the liquefied gas storage tank 11 to the isolator 5 or the like. Therefore, in the sterile liquefied gas device 10, the intake pipe 19 may or may not be connected to the sterile liquefied gas device 10 while the liquefied gas production process is being performed.
- connection pipe 19 is connected to the connection pipe 18 by the clamp 19 d.
- the clamp 19d when it is set as the structure which always installs the intake pipe 19 in the aseptic liquefied gas apparatus 10, it is also possible not to provide the clamp 19d.
- the intake pipe 19 is connected to the sterile liquefied gas device 10 in advance, it is also possible to sterilize the interior of the intake pipe 19 by the sterilization step S1 in the above-described liquefied gas production.
- the connecting pipe 19 is connected to the pipe 51 by the clamp 19 c. In this state, in order to maintain the aseptic condition of the supplied liquefied gas, the connection pipe 19, the connection pipe 18, and the pipe 51 are sterilized.
- FIG. 4 is a flowchart showing the sterilization process in the supply unit of the sterile liquefied gas device according to the present embodiment.
- the sterilization method in the sterile liquefied gas device 10 is, as shown in FIG. 4, a connection step S11, a connection confirmation step S12, a vacuuming step S13, a no leak confirmation step S14, and a sterilization step S15.
- the connecting pipe 19 is connected to the piping 51 of the isolator 5 by the clamp 19 c of the sterile liquefied gas device 10 as the connecting step S11 shown in FIG.
- the connection pipe 19 is not connected to the connection pipe 18, the connection pipe 18 is connected to the connection pipe 18 by the clamp 19 d.
- connection step S11 first, the valve 18a, the valve 19g, the valve 19e and the valve 51a are closed, the vacuum pump 19f is stopped, and the sterilizer 16 is stopped. At this time, the source gas supply device 12 is stopped, the cooling device 13 is stopped, and the sterilizing gas removal device 17 is stopped.
- connection confirmation step S12 shown in FIG. 4 the connection state between the connection pipe 19 and the pipe 51 is detected by a sensor provided on the clamp 19 c of the connection pipe 19. Then, when the signal can not be detected, that is, when the connection between the intake pipe 19 and the pipe 51 can not be confirmed, it is set so as not to advance to the next step.
- the inside of the inlet pipe 19 is depressurized, and the gas inside the inlet pipe 19 is exhausted. This is because in the subsequent sterilization process S15, the supplied sterile gas is filled up to every corner of the interior of the mixing tube 19 to provide a sufficient sterilization atmosphere, and the water etc. inside the mixing tube 19 is externally In order to
- the valve 19e is opened, and the vacuum pump 19f connected to the connection pipe 19 is operated.
- the vacuum pump 19 f is operated as a pressure reducing and discharging device.
- the degree of vacuum inside the branch pipe 19b is measured by the measuring device 19h while the valve 19e is open, and the degree of vacuum inside the coupling pipe 19 becomes a predetermined value. Confirm that it has reached the status. As a result, it is confirmed that no leak has occurred in the inside of the joint pipe 19 and the sterilization area S, that is, connection of the joint, or closure by a valve is surely performed.
- a valve (not shown) is provided at a portion directly above the suction side of the vacuum pump 19f, and after performing the vacuum drawing step S13, the valve is closed.
- a space including the inside of the branch pipe 19b may be a closed space. If it is not a closed space, the differential pressure between the internal pressure of the branch pipe 19b and the atmospheric pressure is the cause, and the indicated value of the measuring device 19h indicates that the pressure gradually rises with the passage of time, and there is no leak Can be determined. Since such a leak detection method is an integral method rather than a dynamic confirmation method of confirming the ultimate pressure in a state where the vacuum pump 19f continues to operate, it is possible to perform the leakage determination with high accuracy. It is possible.
- the valve 19e is closed, and the vacuum pump 19f is stopped, thereby completing the no-leak check step S14.
- the sterilization area S is sterilized in the sterilization step S15 shown in FIG.
- the valve 18a is closed, the valve 51a is closed, the valve 19e is closed, and the valve 19g is opened.
- the sterilizer 16 is operated, and the sterilizing gas, which is hydrogen peroxide gas set to about 100 ° C. supplied from the sterilizing gas supply device, and the main pipe 19a of the intake pipe 19 through the valve 19g It supplies to the branch pipe 19b branched from the main pipe 19a.
- the sterilizing gas which is hydrogen peroxide gas set to about 100 ° C. supplied from the sterilizing gas supply device, and the main pipe 19a of the intake pipe 19 through the valve 19g It supplies to the branch pipe 19b branched from the main pipe 19a.
- the decompressed interior is filled with a sterilizing gas.
- the sterilizing gas comes in contact with the inner surface of the sterilizing region S, and the sterilizing process is performed on the inner surface of the sterilizing region S in contact with the sterilizing gas, thereby killing the bacteria from the inner surface of the sterilizing region S.
- the processing conditions in the sterilization step S15 can adopt the conditions of sterilization required in, for example, a lyophilizer for medicine, in order to obtain complete aseptic conditions. Under such processing conditions, the sterilization area S is exposed to hydrogen peroxide gas for about 30 to 45 minutes to maintain the exposed state, thereby killing the bacteria.
- a valve (not shown) is provided at a portion directly above the suction side of the vacuum pump 19f, and by closing this valve, a sterilizing gas is introduced to the sterilizing region S in a vacuum state, and a state where the sterilizing gas is stored. It is more desirable to keep
- the valve 19g is closed and the valve 19e is opened.
- the vacuum pump 19 f serving as a sterilizing gas discharging device is operated to discharge the sterilizing gas filled in the inside of the connecting pipe 19 to the outside.
- the atmosphere or the inert gas is filled (replaced) in the sterilization area S (the inside of the joint pipe 19), and the sterilizing gas remaining inside the joint pipe 19
- the concentration can be significantly reduced. For this reason, it is more preferable to provide the dilution gas introduction device in the sterile liquefied gas device 10 and to have the sterilization step include the dilution step.
- the vacuum pump 19f serving as a sterilizing gas discharge device is stopped, and the degree of vacuum inside the branch pipe 19b is measured by the measuring device 19h while the valve 19e is open. Based on the measurement result, it is confirmed that the degree of vacuum inside the intake pipe 19 has reached a predetermined value, whereby the sterilizing gas is discharged and removed in the interior of the intake pipe 19 and the sterilization area S. Check what happened.
- the sterilization area S it is confirmed that no leak has occurred, that is, connection of the joint, or blockade by a valve is surely performed.
- the degree of vacuum inside the intake pipe 19 is maintained at a predetermined value, it is set so as not to advance to the next step. Then, the valve 19g is closed, the valve 19e is closed, and the sterilization process for the connecting pipe 19 is finished.
- the valve 18a is opened and the valve 51a is opened in the liquid nitrogen supply step S18 shown in FIG. In this state, the sterile liquid nitrogen stored in the liquefied gas storage tank 11 is supplied to the piping 51 of the isolator 5 while maintaining and guaranteeing the aseptic condition.
- the sterile liquefied gas can be produced as in the first embodiment described above, and the produced sterile liquid nitrogen (liquefied gas) is stored in the liquefied gas storage tank 11.
- the sterilization process can be performed on the intermixing tube 19.
- the bacteria in the sterilization area S partitioned by the valve 18a, the valve 51a, the valve 19e, and the valve 19g are killed, and in this state, the liquid nitrogen supply step S18 can be started.
- the connecting pipe 19 and the connecting portion It is possible to perform the sterilization treatment of (1) without using other equipment, and to easily supply the aseptic liquefied gas to the liquefied gas supply target (the connection target).
- the steps S12, S14, and S17 for confirming each of the steps S11, S13, S15, and S16 in the sterilization process for the intake pipe 19 allow the intake pipe 19 to be processed. It is possible to automate sterilization processing. As a result, the operator can supply the liquefied gas to the liquefied gas supply target in the state where the sterilization processing is completed only by connecting the connecting pipe 19 to the pipe 51, and the liquefaction can be performed while maintaining and guaranteeing the aseptic condition. Supply of gas can be enabled.
- the isolator 5 to be supplied with liquefied gas does not need to be provided with a device for performing sterilization processing, aseptic liquid gas is supplied as needed to the objects to be supplied such as the plurality of isolators 5 etc. It becomes easy to do.
- a sterilizer 16 for performing gas sterilization in the production of liquefied gas is used as a device for supplying sterilizing gas to the intake pipe 19. That is, the sterilizer 16 has both the function of supplying the sterilizing gas to the sterilizing area S in the first embodiment and the function of supplying the sterilizing gas to the interlinking pipe 19.
- a configuration may be employed in which a sterilizer provided separately from the sterilizer 16 supplies sterilizing gas to the pipe 19.
- FIG. 5 is a schematic view showing a bacteria liquefied gas apparatus in the present embodiment
- FIG. 6 is a schematic diagram showing an example of a movement sensor in the bacteria liquefied gas apparatus according to the present embodiment.
- the present embodiment differs from the above-described first and second embodiments in terms of the portable device.
- symbol is attached
- the aseptic liquefied gas device 10 includes at least a carriage 15a, wheels 15b, an acceleration sensor, and the like as a moving device 15 (portable device) that makes at least the liquefied gas storage tank 11 portable. And a control unit 15u.
- the carriage 15a As shown in FIG. 5, the liquefied gas storage tank 11, the raw material gas supply device 12, the cooling device 13, the supply piping 14, the control unit 15u, the sterilization device 16, and the sterilization gas removal device 17, the liquefied gas supply unit 18 (connection pipe), and the connection pipe 19 are placed.
- the carriage 15a allows the members (apparatus, valves, piping, etc. described above) surrounded by the broken line to be moved integrally.
- bogie 15a is abbreviate
- a plurality of wheels 15b are provided under the carriage 15a, and the carriage 15a is movable. Each of the plurality of wheels 15b can be fixed and detached with respect to a stopper 15s provided on a floor or the like.
- the stopper 15s is a trolley so that the aseptic liquefied gas device 10 is disposed at a position where the liquefied gas is produced and a position where the intake pipe 19 can be connected to the isolator 5 to which the produced liquefied gas is supplied. 15a can be fixed. Thus, the carriage 15a is movable between the position where the liquefied gas production is performed and the position where the liquefied gas is supplied, and the liquefied gas production and the liquefied gas supply are enabled.
- the stopper 15s is provided with sensors connected to the control unit 15u.
- the operation of producing liquefied gas or the operation of delivering liquefied gas is enabled in the sterile liquefied gas device 10 by the detection signal output from the sensor only when the wheel 15b is located at the position corresponding to the stopper 15s.
- a proximity sensor, a weight detection sensor, a contact detection sensor, or the like can be employed as the sensor.
- the movement sensor 15g is provided integrally with the carriage 15a, and can detect a state in which the carriage 15a is moving.
- the configuration of the movement sensor 15g is not limited as long as the movement of the carriage 15a can be detected.
- a configuration may be employed in which a sphere 15g1 made of a conductor is disposed in a container 15g2 opened at the top made of a conductor.
- the control unit 15u a signal detected electrically when the ball 15g1 contacts the inner wall of the container 15g2.
- the movement sensor 15g is connected to the control unit 15u, and the operation for producing liquefied gas or the operation for supplying liquefied gas is enabled in the aseptic liquefied gas device 10 only when the movement sensor 15g does not detect movement. .
- the control unit 15u includes a pressure detection device and a temperature detection device connected to the internal state display device 11f of the liquefied gas storage tank 11, the raw material gas supply device 12, the cooling device 13, the supply pipe 14, and the valves 14a and 14b. , 14c, the sensor of the stopper 15s, the movement sensor 15g, the sterilizer 16, the sterilizing gas removing device 17, the valves 18a and 18c of the liquefied gas supply unit 18 (connection piping), and the valve 19e of the connecting pipe 19, It is connected to 19 g, a vacuum pump 19 f and a measuring device 19 h, and sensors of the clamps 19 c and 19 d.
- the control unit 15u controls the operation of these devices and members, or receives signals output from these members.
- control unit 15u operates as a power source serving as an uninterruptible power supply for supplying necessary power to the components of the aseptic liquefied gas device 10 and the isolator 5. It is considered one.
- control unit 15u is also connected to a power supply 13d for supplying power to the cooling device 13 and a connector 13e.
- the control unit 15u controls the operation of the cooling device 13, the power supply 13d, and the connector 13e, or receives signals output from these members.
- the power required for the operation of the cooling device 13 is much greater than the power required for the operation of the other configurations described above. For this reason, when the cooling device 13 is operated, power is supplied not from the power supply that is integrated with the control unit 15u as an uninterruptible power supply, but from the power supply 13d fixed to the facility and capable of large capacity power supply. .
- the liquefying operation is not performed during movement of the carriage 15 a by the above-described sensors, so that safety can be ensured.
- the structure required for the aseptic liquefied gas apparatus 10 is mounted in the trolley
- the sterile liquefied gas device 10 can be moved toward the plurality of isolators 5.
- the supply pipe 19 and the connection portion through which the liquefied gas flows can be sterilized before supplying the liquefied gas to the isolator 5 without using other facilities, and the supply of the aseptic liquefied gas can be easily performed. It can be done.
- space saving and weight reduction of the portable aseptic liquefied gas device 10 can be achieved.
- the aseptic liquefied gas device 10 can be easily used in a small scale facility such as a research facility in which a plurality of isolators 5 are installed in the same room. can do. In this case, there is no need to install a large-scale sterilized liquefied gas production apparatus. In addition, there is no need to connect a sterile liquefied gas production device to a supply target such as a non-movable production device via a long pipe. The supply of the aseptic liquefied gas can be easily made possible without performing a large-scale remodeling on the layout change of the facility such as the movement of the isolator 5.
- the aseptic liquefied gas device 10 can be moved toward the supply object to which aseptic liquefied gas is supplied by the carriage 15a, it is confirmed that the necessary sterilization processing is completed, and the sterilization as an arbitrary supply object is performed. Supply of sterile liquefied gas can be easily enabled while guaranteeing the condition.
- the sterile liquefied gas device 10 can be produced as in the first embodiment described above, and the sterile liquid nitrogen produced in the same manner as the second embodiment described above ( In a state in which the liquefied gas is stored in the liquefied gas storage tank 11, sterilization processing can be performed on the coupling pipe 19. Thereby, the bacteria in the sterilization area S can be killed, and in this state, the liquid nitrogen supply step S18 can be started.
- steps S11, S13, S15, and S16 are confirmed as in the second embodiment described above.
- S14 and S17 it is possible to automate the sterilization process for the interlinking tube 19.
- the operator can supply the liquefied gas to the liquefied gas supply target in a state where the sterilization processing is completed only by connecting the intake pipe 19 to the pipe 51, and the liquefaction can be performed while maintaining and guaranteeing the aseptic condition. Supply of gas can be enabled.
- the isolator 5 which is the liquid gas supply target does not need to be provided with a device for performing the sterilization process, it is necessary when supplying the plurality of isolators 5 etc. while maintaining safety. It is only possible to supply sterile liquefied gas.
- a sterilizer 16 for performing gas sterilization in the production of liquefied gas is used as a device for supplying sterilizing gas to the intake pipe 19. That is, the sterilizer 16 has both the function of supplying the sterilizing gas to the sterilizing area S in the first embodiment and the function of supplying the sterilizing gas to the interlinking pipe 19.
- a configuration may be employed in which a sterilizer provided separately from the sterilizer 16 supplies sterilizing gas to the pipe 19.
- power is supplied to the cooling device 13 from the fixed power supply 13 d.
- the present invention is not limited to this configuration, and the power supply 13d may be mounted on the carriage 15a. That is, a portable power source capable of supplying a large amount of power can be placed on the carriage 15a.
- FIG. 7 is a schematic view showing a bacteria liquefied gas device in the present embodiment.
- the present embodiment differs from the above-described first to third embodiments in terms of the configuration of the portable device.
- the same members as those in the first to third embodiments are given the same reference numerals, and the description thereof will be omitted or simplified.
- the raw material gas supply device 12 is disposed in a fixed state like the power supply 13d. Furthermore, in the supply piping 14, a valve 12a and a clamp 12b are provided between the source gas supply device 12 and the valve 14a.
- the clamp 12b As the configuration of the clamp 12b, the same configuration as that of the clamps 19c and 19d is adopted.
- the supply pipe 14 and the raw material gas supply device 12 can be connected and disconnected.
- the valve 12a As the configuration of the valve 12a, the same configuration as that of the valve 18a is adopted.
- the supply pipe 14 and the raw material gas supply device 12 can be connected and disconnected.
- the clamp 12b is provided with a connection sensor, which detects that it is in a connected state and can output the signal to the control unit 15u.
- the position near the clamp 12b is equivalent to that of the connection pipe 19.
- the sterilizable configuration of can also be arranged.
- liquefied gas production when liquefied gas production is performed, liquefied gas production is performed at a position (liquefied gas production position) in the vicinity of the source gas supply device 12 disposed in a fixed state.
- the aseptic liquefied gas device 10 When supplying the manufactured liquefied gas to the isolator 5 or the like, the aseptic liquefied gas device 10 is moved to a position near the isolator 5 (liquefied gas supply position), and the aseptic liquefied gas device 10 is connected to the isolator 5 be able to.
- the power supply 13d and the raw material gas supply device 12 are arranged in a fixed state and the power supply 13d and the raw material gas supply device 12 are not mounted on the carriage 15a, space saving of the portable aseptic liquefied gas device 10 is realized. It is possible to further reduce the weight.
- bogie 15a can be suitably selected for space saving of the portable aseptic liquefied gas apparatus 10, and weight reduction.
- the filter 14d is opened after a predetermined period regardless of whether the liquefied gas production process has been performed or not performed after the sterilization process is performed. , 18b periodically to maintain sterility.
- the description regarding the integrity test step S21 is not described, but it is preferable to appropriately carry out.
- sterile liquid nitrogen which can be used directly as a sterile pharmaceutical product or can be used directly in a sterile room, when there is a need to quench the product in the fields of biomedicine and regenerative medicine or lyophilizer It can mention mentioning.
- valve 18b ... filter 19 ... connection pipe (supply part) 19a: main pipe 19b: branch pipe 19c, 19d: clamp 19e, 19g: valve 19f: vacuum pump 19h: measuring device 19A: integrity testing device 19Aa to 19Ag, 19Av: valve 19B: integrity testing unit 5: isolator 51: piping 51a ... valve S ... sterilization area
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Abstract
Description
本願は、2017年11月7日に日本に出願された特願2017-214520号に基づき優先権を主張し、その内容をここに援用する。
特許文献2には、極低温耐性を有する材質のフィルタを用いて液体窒素を無菌化することが記載されている。
特許文献3には、無菌化したガスを冷却して液化すること、および、配管等を蒸気によって滅菌することが記載されている。
特許文献4に記載されるように、アイソレータにおいては、作業室内を滅菌状態に維持することが必要である。
特に、iPS細胞に関連した技術などにおいては、無菌の液体窒素の供給を実現することは急務である。
さらに、単一の施設内において、複数のアイソレータに対して無菌液体窒素を供給可能としたいという要求もあるが、同時に、液体窒素製造装置の大きさは大型化したくないという要求もあった。
しかも、作業手順をなるべく簡素化して、無菌状態を維持するとともに厳密な無菌状態を保証して、このような液体窒素の供給を可能とすることが要求されている。
本発明の第1態様に係る無菌液化ガス装置において、前記原料ガスを液化することによって得られる液化ガスが液体窒素とされてもよい。
本発明の第1態様に係る無菌液化ガス装置において、少なくとも前記液化ガス貯留タンクを可搬とする移動装置を備えてもよい。
本発明の第1態様に係る無菌液化ガス装置は、前記液化ガス貯留タンクに接続され、前記液化ガス貯留タンクの下流側に向けて、前記液化ガス貯留タンクに貯留した液化ガスを供給し、密閉可能な供給部と、前記供給部を滅菌する供給部滅菌装置と、を備えてもよい。
本発明の第1態様に係る無菌液化ガス装置において、前記供給部滅菌装置は、前記供給部が液化ガス供給対象に接続された際に前記液化ガスを無菌状態で前記液化ガス供給対象に供給可能であり、前記供給部滅菌装置は、供給部を無菌化する無菌化処理を行うことが可能とされてもよい。
本発明の第1態様に係る無菌液化ガス装置は、前記供給部が前記液化ガス供給対象に接続されたことを検出する接続センサを備え、前記接続センサにより、前記供給部と前記液化ガス供給対象との接続が確認された場合に、前記供給部滅菌装置が前記無菌化処理を開始可能とされてもよい。
本発明の第1態様に係る無菌液化ガス装置は、前記液化ガス貯留タンクが移動中であることを検出する移動センサを備え、前記移動センサにより、無菌液化ガス装置が移動中であることを検出した場合には液化処理が停止可能とされてもよい。
本発明の第2態様に係る無菌液化ガス装置の取り合い管は、液化ガス貯留タンクと液化ガス供給対象とに接続される取り合い管であって、前記液化ガス貯留タンクと、前記液化ガス供給対象とに接続可能な接続部と、密閉可能なバルブと、を有し、前記バルブにより前記取り合い管の内部を密閉した状態で前記取り合い管の内部の気体を排気可能な真空排気装置が接続されており、排気された状態にある前記取り合い管の内部に滅菌ガスを供給可能な滅菌装置が前記取り合い管に接続されている。
特に、大型のタンク設置など大規模な設備を設置することが不必要となる。
また、液化ガスとは、-50℃未満の標準沸点を有するガスであり、例えば、窒素、酸素、液体空気およびアルゴンを挙げることができる。
これにより、滅菌ガスを製造する無菌液化ガスと同一とすることで、滅菌ガスが仮に残留したとしても製造ガスの純度に悪影響を与えないため、好ましい。また、滅菌工程において、当初は大気を利用し、後に、大気から不活性ガスに切り替えて滅菌を行うという手順がコスト面で優れ、上記の悪影響を回避することができ、双方の利点を両立できるため、好ましい。同様に、不活性ガスの種類として、2種類のガスを用い、ガス供給を切り替えて滅菌を行うことも同様の効果を得ることができる。
なお、液化ガス製造時の原料ガス供給装置からの供給流量に比べて、滅菌ガス除去処理におけるガス供給流量は大きく設定されることが滅菌ガス除去処理の短時間化のために好ましい。なお、液化ガス貯留タンク等の滅菌領域を減圧することで、滅菌領域に供給する不活性ガス温度を100℃よりも低く設定することができる。例えば、30kpaまで減圧した場合に70℃程度に設定することができる。
ここで、サニタリ規格とは、食品、酪農、醸造、飲料、製菓、水産、医薬、化粧品、化学工業品、清涼飲料、ビール、酒、食肉加工、化学薬品液、半導体等の製造に用いられる規格を意味する。
図1は、本実施形態における無菌液化ガス装置を示す模式断面図であり、図において、符号10は、無菌液化ガス装置である。
液化ガス貯留タンク11には、図1に示すように、上端となる蓋部11aを貫通して供給配管14と接続配管18と冷却装置13とが設けられている。
本実施形態に係る原料ガス供給装置12としては、吸着剤を利用した窒素発生装置(PSA)を有しており、空気から効率よく酸素と窒素を分離し、99.99%までの窒素ガスを液化ガス貯留タンク11に供給可能である。なお、原料ガスを液化ガス貯留タンク11に供給可能であれば、原料ガス供給装置12の構成は、上記構成に限定されない。
なお、水冷部13cを設けないでコンプレッサ13bにより直接外部に廃熱する構成(空冷)を採用することもできる。液化ガス貯留タンク11の内部に突出した冷却部13aは、その表面がサニタリ仕様を満たすように構成されている。
滅菌フィルタ14dとしては、例えば、PALL社製の気体滅菌用疎水性PTFEメンブレンフィルターを採用することができる。
滅菌フィルタ14dには、滅菌フィルタ14dにおける無菌状態を維持可能な状態であることを確認・検査する完全性試験装置19Aを設けることができる。
本発明における「完全性試験」は、JISK3835の第3頁、6.3(1)(b)に記載されている通り、「JISK3832若しくはJISK3833または採用したフィルタの取扱説明書に基づき、無菌的に完全性試験を行い、試験フィルタの破損などの欠陥が無いことを確認する。」ことが重要である。
図1に示す無菌液化ガス装置10の構成においては、完全性試験機19Bが、無菌液化ガス装置10にビルトインされている。しかしながら、完全性試験は、「定期的な検査」という位置づけであることから、完全性試験機19Bは、無菌液化ガス装置10に常時必要な機器ではない。なお、フィルタ18bに接続されている配管及びこの配管に設けられているバルブの配置は、上述した滅菌フィルタ14dに接続されている配管及びこの配管に設けられているバルブの配置と同一であるため、説明を省略する。
ただし、完全性試験機19Bが無菌液化ガス装置10に常設された構成は、より安全である。このため、以下の説明では、完全性試験機19Bが無菌液化ガス装置10に常設された場合を説明している。
JISK3833に記載された「2.拡散流量試験」と段落0045以降の説明は、基本的に類似する。ゆえに、詳細については、JISK3833の記載を反映させることが好ましい。
JISK3833に記載された「7.1.(2)」の手順によりフィルタを全て湿らせた。手順としては、完全性試験器側から純水を投入、バルブ19Acを閉あるいは微小に開いた状態で、1次側を純水で満たすことにより、「7.1.(2)(e)」を達成させる。
その後、「7.2.(1)」を実施することにより、完全性試験とする。
完全性試験が終了した後は、当該装置は取り外しても構わない。完全性試験器側は、フランジ接続の状態なので、封止、ドレイン側のバルブ2個と上下の流路バルブ2個が残存する構成で終了となる。
バルブ14bを開とし、バルブ14a,バルブ14cを閉とし、滅菌装置16により滅菌ガスを無菌液化ガス装置10の内部に向けて供給することで、滅菌フィルタ14dより下流部分に位置する滅菌領域Sをガス滅菌することが可能となる。
この場合、滅菌領域S全体に滅菌ガスを行き渡らせるように、接続配管18の下流側、例えば、バルブ18aの下流位置、あるいは、バルブ18cの下流位置(外側位置)に真空ポンプ等の排気装置を設けること、または、この位置にポンプを接続可能とすることもできる。このように、滅菌領域S内を真空引きして、滅菌領域S内における残留物を滅菌ガスに置換することで、滅菌ガスの濃度を上昇させ、滅菌領域S内を万遍なく滅菌することが可能となる。
この場合、滅菌領域S全体から滅菌ガスを除去可能とするために、接続配管18の下流側、例えば、バルブ18aの下流位置、あるいは、バルブ18cの下流位置(外側位置)にポンプ等の排気装置を設けること、または、この位置にポンプを接続可能とすることもできる。
さらに、接続配管18の上流側端部は、貯溜凹部11dの最低位置となる中央部分に対してほぼ接触するように配置されることもできる。このように、接続配管18の上流側端部が配置されることで、滅菌時に貯溜凹部11dに溜まった水分等を外部に排出可能なドレインとして接続配管18を用いることもできる。
図2は、本実施形態に係る無菌液化ガス装置における液化ガス製造工程を示すフローチャートである。
滅菌工程S1においては、まず、バルブ14aとバルブ14cとを閉状態として、バルブ14bを開状態とし、冷却装置13を停止状態とし、原料ガス供給装置12を停止状態とし、バルブ18aを開状態とし、バルブ18cを開状態とする。
滅菌ガス除去装置17から供給された高温不活性ガスは、無菌状態となっている滅菌フィルタ14dを通過することによって、菌を死滅させた無菌状態で滅菌領域S内に供給される。
また、完全性試験工程S21は、滅菌工程S1より前に行うことが好ましい。これは、滅菌フィルタ14d,フィルタ18bの部分が湿ってしまうおそれがあるため、また、バルブ19Ad,19Ac(ドレイン弁)の開閉による外部からのコンタミネーションの混入を防止するためである。
必要に応じて、滅菌ガス除去装置17などにより液化ガス貯留タンク11内を加圧することにより、液化ガス貯留タンク11に貯留された無菌液化ガスは、開状態のバルブ18aを通じて、取出口から外部に供給することが可能となる。
あるいは、バルブ18aを閉状態とし、バルブ18cを開状態として液化冷却工程S4を開始した場合には、フィルタ18bが設けられていることにより、バルブ18cから菌が入り込むことがない。
さらに、原料ガスを供給せず液化ガス製造を行っていない状態で、液化ガスの液体が保管されている場合は、入熱による原料ガスの蒸発で液化ガス貯留タンク11内の圧力が上がる、このため、図示しない圧力検出装置とバルブ18cとを連動させることによって、液化ガス貯留タンク11の内圧を設定値まで下げるように制御されている。また、バルブ18cを安全バルブとして作動させる場合には、開状態を維持しておく。
図3は、本実施形態における無菌液化ガス装置を示す模式正面図である。本実施形態は、供給部に関する点で、上述した第1実施形態と異なる。図3において、第1実施形態と同一部材には同一符号を付して、その説明は省略または簡略化する。
なお、図3においては、完全性試験装置19Aの一部の図示が省略されている。図3に示す完全性試験装置19Aの構成としては、図1に示した構成と同等の構成が採用されている。
枝管19bには、また、バルブ19gを介して滅菌ガスを供給可能な装置、具体的には、滅菌装置16に接続されるとともに、枝管19bの内部の真空度を測定する測定装置19hが設けられている。測定装置19hに関し、滅菌装置に侵されない測定装置として、隔膜真空計を用いることが好ましい。
これら取り合い管19は、これらの表面または内面がサニタリ仕様を満たすように構成されている。
この場合、取り合い管19は、クランプ19dによって接続配管18に接続される。なお、無菌液化ガス装置10に取り合い管19を常設する構成とした場合には、クランプ19dを設けないこともできる。また、あらかじめ取り合い管19が無菌液化ガス装置10に接続された場合には、上述した液化ガス製造における滅菌工程S1により、取り合い管19内部を滅菌しておくことも可能である。
この状態で、供給する液化ガスの無菌状態を維持するために、取り合い管19、接続配管18、配管51を無菌化する処理を行う。
図4は、本実施形態に係る無菌液化ガス装置の供給部における無菌化工程を示すフローチャートである。
なお、取り合い管19が接続配管18に接続されていなかった場合には、クランプ19dによって、取り合い管19が接続配管18に接続される。
これにより、バルブ18a、バルブ51a、バルブ19gで仕切られた主管19aおよび枝管19bの内部が減圧される。この減圧された内部が、滅菌領域Sとなる。
取り合い管19の内部の真空度が所定値に到達した状態であることが確認できたら、バルブ19eを閉状態とするとともに、真空ポンプ19fを停止状態とし、無リーク確認工程S14を終了する。
滅菌工程S15においては、バルブ18aを閉状態、バルブ51aを閉状態、バルブ19eを閉状態として、バルブ19gを開状態とする。
この状態で、滅菌ガス排出装置となる真空ポンプ19fを作動させ、取り合い管19の内部に充填された滅菌ガスを外部に排出する。この際、図示しないが、滅菌装置16に代えて、大気あるいは不活性ガスを滅菌領域S(取り合い管19の内部)に満たす(置換する)ことで、取り合い管19の内部に残留する滅菌ガスの濃度を著しく下げることができる。このため、希釈ガス導入装置を無菌液化ガス装置10に設けるとともに、無菌化工程が希釈工程を備えることがより好ましい。
ここで、取り合い管19の内部の真空度が所定値に維持された状態であることが確認できない場合には、次のステップに進まないように設定されている。
次いで、バルブ19gを閉状態として、バルブ19eを閉状態とし、取り合い管19に対する滅菌処理を終了する。
図5は、本実施形態における菌液化ガス装置を示す模式図であり、図6は、本実施形態に係る菌液化ガス装置における移動センサの一例を示す模式図である。
本実施形態は、可搬装置に関する点で、上述した第1および第2実施形態と異なる。図5及び図6において、第1および第2実施形態と同一部材には同一符号を付して、その説明は省略または簡略化する。
具体的には、センサとしては、近接センサ、重量検出センサ、または、接触検知センサ等が採用できる。
図7は、本実施形態における菌液化ガス装置を示す模式図である。
本実施形態は、可搬装置の構成に関する点で、上述した第1~第3実施形態と異なる。図7において、第1~第3実施形態と同一部材には同一符号を付して、その説明は省略または簡略化する。
11…液化ガス貯留タンク
11d…貯溜凹部
11f…内部状態表示装置
12…原料ガス供給装置
13…冷却装置(機械式冷凍機システム)
13a…冷却部
13b…コンプレッサ
13c…水冷部
13d…電源
13e…コネクタ
14…供給配管
14a,14b,14bc…バルブ
14d…滅菌フィルタ
15…移動装置(可搬装置)
15a…台車
15b…車輪
15s…ストッパ
15g…移動センサ
15u…制御部(電源)
16…滅菌装置
17…滅菌ガス除去装置
18…接続配管(供給部)
18a,18c…バルブ
18b…フィルタ
19…取り合い管(供給部)
19a…主管
19b…枝管
19c,19d…クランプ
19e,19g…バルブ
19f…真空ポンプ
19h…測定装置
19A…完全性試験装置
19Aa~19Ag,19Av…バルブ
19B…完全性試験部
5…アイソレータ
51…配管
51a…バルブ
S…滅菌領域
Claims (8)
- 液化ガス貯留タンクと、
前記液化ガス貯留タンクに原料ガスを供給する原料ガス供給装置と、
前記液化ガス貯留タンク内を冷却して前記原料ガスを液化する冷却装置と、
前記原料ガス供給装置と前記液化ガス貯留タンクとを接続する供給配管と、
前記供給配管に設けられる滅菌フィルタと、
前記滅菌フィルタよりも下流部分に位置する滅菌領域を滅菌ガスにより滅菌する滅菌装置と、
滅菌後に前記滅菌ガスを除去する滅菌ガス除去装置と、を有する、
無菌液化ガス装置。 - 前記原料ガスを液化することによって得られる液化ガスが液体窒素とされる、
請求項1に記載の無菌液化ガス装置。 - 少なくとも前記液化ガス貯留タンクを可搬とする移動装置を備える、
請求項1又は請求項2に記載の無菌液化ガス装置。 - 前記液化ガス貯留タンクに接続され、前記液化ガス貯留タンクの下流側に向けて、前記液化ガス貯留タンクに貯留した液化ガスを供給し、密閉可能な供給部と、
前記供給部を滅菌する供給部滅菌装置と、を備える、
請求項1から請求項3のいずれか一項に記載の無菌液化ガス装置。 - 前記供給部滅菌装置は、前記供給部が液化ガス供給対象に接続された際に前記液化ガスを無菌状態で前記液化ガス供給対象に供給可能であり、
前記供給部滅菌装置は、供給部を無菌化する無菌化処理を行うことが可能とされている、
請求項4に記載の無菌液化ガス装置。 - 前記供給部が前記液化ガス供給対象に接続されたことを検出する接続センサを備え、
前記接続センサにより、前記供給部と前記液化ガス供給対象との接続が確認された場合に、前記供給部滅菌装置が前記無菌化処理を開始可能とされている、
請求項5に記載の無菌液化ガス装置。 - 前記液化ガス貯留タンクが移動中であることを検出する移動センサを備え、
前記移動センサにより、無菌液化ガス装置が移動中であることを検出した場合には液化処理が停止可能とされる、
請求項1から請求項6のいずれか一項に記載の無菌液化ガス装置。 - 液化ガス貯留タンクと液化ガス供給対象とに接続される取り合い管であって、
前記液化ガス貯留タンクと、前記液化ガス供給対象とに接続可能な接続部と、
密閉可能なバルブと、
を有し、
前記バルブにより前記取り合い管の内部を密閉した状態で前記取り合い管の内部の気体を排気可能な真空排気装置が接続されており、
排気された状態にある前記取り合い管の内部に滅菌ガスを供給可能な滅菌装置が前記取り合い管に接続されている、
無菌液化ガス装置の取り合い管。
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US16/759,232 US20200345881A1 (en) | 2017-11-07 | 2018-07-25 | Sterilized-liquefied gas apparatus and connectin pipe thereof |
CN201880069884.2A CN111278471A (zh) | 2017-11-07 | 2018-07-25 | 无菌液化气体装置及无菌液化气体装置的结合管 |
JP2018556958A JP6460558B1 (ja) | 2017-11-07 | 2018-07-25 | 無菌液化ガス装置 |
KR1020207012541A KR20200066660A (ko) | 2017-11-07 | 2018-07-25 | 무균 액화 가스 장치, 및 무균 액화 가스 장치의 취합관 |
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KR (1) | KR20200066660A (ja) |
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BRPI1002740B1 (pt) * | 2010-08-20 | 2020-12-29 | Flávio Camilotti | sistema compacto de envasamento de gás |
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- 2018-07-25 CN CN201880069884.2A patent/CN111278471A/zh active Pending
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- 2018-07-25 KR KR1020207012541A patent/KR20200066660A/ko not_active Application Discontinuation
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JP2000185710A (ja) * | 1998-10-14 | 2000-07-04 | Toyo Seikan Kaisha Ltd | 液化ガス除菌充填方法とその装置 |
JP2009120242A (ja) * | 2007-11-16 | 2009-06-04 | Daiwa Can Co Ltd | 液化ガス充填装置の殺菌方法 |
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