JP2020193765A - Dry room for gas replacement - Google Patents

Abstract

To provide a gas replacement system capable of switching the environment in a drying chamber under an inert gas environment with a production device housed therein, to an atmospheric environment, or back to a low dew point and inert gas environment, in a relatively short period of time.SOLUTION: The gas replacing system for a booth, the inside of which needs to be kept clean under a low dew point and inert gas environment, is structured to introduce dry air thereinto in one pass to discharge moisture outside the device when maintenance work is being carried out, while independently carrying out a circulation operation by closing all of inert gas circulation lines with valves and the like, whereby a down time caused by an atmospheric break can greatly be reduced even when a plurality of booths are present. By connecting a low dew point gas supply device and an inert gas purification device to form an integral body, the cost of the system and an installation space therefor can be reduced.SELECTED DRAWING: Figure 1

Description

The present invention provides a drying chamber and chamber having an inert gas concentration (hereinafter, a gas whose active gas concentration is as close to 0 ppm as possible is referred to as "inert gas") such as a booth in which an organic EL display manufacturing apparatus is installed. , Dehumidification that can switch to a low dew point environment (hereinafter, a dew point temperature of 0 degrees or less is called "low dew point") in a relatively short time for maintenance and adjustment of manufacturing equipment at the booth. It relates to a gas replacement system including an apparatus and a gas purifier.

Conventionally, organic EL elements used in organic EL display devices, which are expected as next-generation flat panel displays to replace liquid crystal display devices, are promising for use as solid-state light-emitting inexpensive large-area full-color display devices and writing light source arrays. It has been actively researched and developed. However, organic substances such as organic light emitting materials used for organic EL devices and electrodes are vulnerable to moisture, and the performance and characteristics are rapidly deteriorated by the moisture in the air. Therefore, it is necessary to carry out manufacturing and experiments in a booth where air is purged with air with an extremely low dew point or an inert gas such as nitrogen gas vaporized from liquid nitrogen during the experiments associated with these developments. ..

At present, in the production of organic EL displays (OLEDs), printing technology such as inkjet technology is used to make a liquid organic EL material into a uniform thin film on a substrate to create an element with improved production efficiency and performance. Technology is being developed. In order to develop such a manufacturing technology, the booth is filled with an inert gas such as nitrogen gas in order to make the ambient environment of the manufacturing equipment an inert gas concentration at a low dew point such as moisture of 1 ppm or less and oxygen of 1 ppm or less. ing. However, when performing maintenance or adjustment of manufacturing equipment in the booth, it is necessary to return the inert gas environment with a low dew point to the atmospheric environment (hereinafter referred to as "atmospheric break").

At this time, if the inert gas environment is replaced with a normal atmosphere, various parts of the internal device adsorb water, and when returning to the inert gas environment again, it takes a very long time for the parts to desorb the adsorbed water. It takes.

Patent Document 1 as a technique for minimizing the internal volume of a gas enclosure assembly in order to minimize the amount of inert gas for returning from an atmospheric break to an inert gas environment and to minimize the downtime of the device. There is one described in.

Patent Document 2 discloses a glove box with an inert gas circulation purification device. According to this, in order to keep the atmosphere of the inert gas in the glove box constant and efficiently remove oxygen and water, a metal catalyst filling part filled with a metal catalyst that removes oxygen in the gas and a water content in the gas. The gas in the glove box is sucked out by the circulation pump, which is configured to supply the circulating gas from which oxygen and water have been removed by the adsorption tower composed of the desiccant filling part filled with the desiccant of the molecular sieve. , Oxygen and water are removed while passing through the adsorption tower and returned to the glove box to perform gas circulation.

Patent No. 6153539 Patent No. 5676521 JP-A-2019-52835

What is disclosed in Patent Document 1 is to frame the gas enclosure and make the internal volume as small as possible to minimize the amount of inert gas in the gas enclosure and minimize the downtime due to maintenance and the like. The work space can be optimized to accommodate the installation area of the OLED manufacturing apparatus. However, since the gas refining system that simultaneously purifies the inert gas and removes water is also stopped during the suspension, there is a problem that it takes too much time to return the booth to the inert gas environment at low humidity again. there were. In addition, since the gas purification device and the dehumidifying device are in the same mechanism, the purification rate differs between oxygen and water, and it takes a very long time to remove water compared to the removal of oxygen, so it is difficult to remove them at the same time. There is also.

Even in a conventional system such as Patent Document 2, since oxygen removal and water removal are performed by a series column, equipment selection has been performed with a rate-determining water removal capacity. As described above, in the conventional technique, it takes a long time to return to the inert gas environment after the atmospheric break, and it takes time to set up the manufacturing equipment line accordingly.

Therefore, as in Patent Document 3, a gas replacement dry room has been developed in which the time required to reach a predetermined water concentration is significantly shortened by removing water using a desiccant rotor and supplying a low dew point gas. .. Compared with the pellet-shaped molecular sieve used for removing water in Patent Document 2, the advantages of using a desiccant rotor for removing water are that the honeycomb shape has a large surface area, low pressure loss, and the honeycomb wall is very large. Since it is thin and the adsorbed water diffuses quickly, the entire honeycomb element is instantly absorbed and detached.

The gas replacement dry room of Patent Document 3 is provided with an airtight container for storing the manufacturing device used for OLED manufacturing and research and development inside the drying room in which the dry air from the dry air supply device is circulated. It is designed to supply an inert gas and a low dew point gas. In addition, an inert gas purification device and a low dew point gas supply device are arranged in series in the circulation path of the airtight container, and a circulation path separated from the circulation path is provided separately to control each other independently, so that water can be removed. Performance and oxygen removal performance can be adjusted individually. Further, by circulating the circulation path separately provided during the atmospheric break, the time required to return the airtight container from the atmospheric environment to the inert gas environment after the atmospheric break can be significantly shortened. Since the supply of the low dew point gas can be maintained while the supply of the inert gas is stopped, the dew point in the airtight booth quickly reaches a low state even after the atmospheric break.

In the present invention, the dry air supply device for supplying and circulating dry air to the drying chamber covering the airtight container and the inside of the drying chamber described in Patent Document 3 is omitted, and a low dew point gas purification device and an inert gas purification device are connected. The purpose of this is to simplify the device, save space, and simplify the operation method as compared with the dry room for gas replacement of Patent Document 3.

In order to solve the above problems, the present invention provides an airtight booth for storing the manufacturing equipment used for the manufacture and research and development of OLED, and supplies the low dew point gas and the inert gas to the airtight booth to be inert. Since the gas purification device and the low dew point gas supply device are connected and integrated, and if necessary, a switching means for passing through the bypass path is provided so that the gas that has passed through the low dew point gas supply device does not pass through the inert gas purification device. , When a person enters the airtight booth due to adjustment during an atmospheric break, the inert gas can be separated from the supply to the airtight booth and maintained in a closed loop circulation while supplying dry air to the airtight booth, and it is paused due to the atmospheric break. The time can be greatly reduced. Alternatively, the amount of dry air supplied can be reduced by operating the low dew point gas supply device during an atmospheric break without closed-loop circulation. Water molecules are polar substances, and if the atmosphere is introduced as it is into an airtight booth that needs to be maintained at a low dew point, water molecules will adhere to the walls of the airtight booth and inside the filter. In order to discharge the attached water molecules, it is necessary to supply low dew point air for a long time, but in the case of the present invention, since the dry air is supplied with the supply of the inert gas stopped, the atmosphere. Even after a break, the dew point in the airtight booth can be quickly reached to a low state.

Further, whether it is nitrogen gas contained in a cylinder as an inert gas, nitrogen gas obtained by vaporizing liquefied nitrogen, or oxygen from air by deep cold separation, pressure swing adsorption (PSA), membrane separation method, etc. Even with nitrogen gas from which the gas has been removed, the price of the gas is high, and the cost will increase unless the time for the atmospheric break and the time for returning to the inert gas environment after the atmospheric break are shortened. On the other hand, the cost can be reduced by producing a low dew point gas with a desiccant rotor, stopping the supply of the inert gas while maintaining the supply of the low dew point gas, and performing maintenance.

Moisture removal is performed by the desiccant dehumidifier, and the water removal time is greatly shortened. At the same time, a part of the low dew point gas is introduced into the inert gas purification device to remove oxygen. By adjusting the amount of gas introduced into the inert gas purification device, a dry room with an inert gas concentration can be created under optimum operating conditions.

Since the dry room for gas replacement of the present invention is configured as described above, it does not circulate from an air purification filter such as a HEPA filter or ULPA filter installed in the upper part of the container even during an atmospheric break, and is unidirectional (hereinafter, "one pass"). By supplying dry air with (), maintenance, maintenance, setup change, etc. are carried out so that the filter that most easily retains moisture does not retain moisture. In addition, an inert gas purification device was connected after the desiccant dehumidifier and integrated, and a circulation path provided separately was circulated during the atmospheric break to prevent the circulating air from approaching the atmospheric environment. By doing so, it is possible to significantly shorten the recovery time from the atmospheric environment after the air break in the airtight booth to the low dew point and inert gas environment. Further, by adjusting the flow rate of the gas flowing from the dehumidifier to the inert gas purification device, it is possible to easily create a dry room that can be optimized for a low dew point and an inert gas environment in a short time.

FIG. 1 is a flow chart of the dry room of the present invention according to the first embodiment. FIG. 2 is a flow chart of the dry room of the present invention in Example 2.

Hereinafter, embodiments for carrying out the present invention will be described with reference to the drawings. The present invention is not limited to the following examples.

In the present embodiment, as a gas replacement dehumidifier for a container whose inside needs to be kept clean with a low dew point and an inert gas, and as a gas replacement method, an organic EL display (OLED) using a printing technique such as an inkjet technique is manufactured or The booth of the research and development equipment will be described as an example. The present invention is not limited to OLED manufacturing or R & D equipment, but is a glove box used for the development of lithium-ion battery materials and semiconductor fields in which it is necessary to keep the storage space clean in a low dew point, inert gas environment. It can also be used for storage containers or closed spaces.

Hereinafter, Example 1 of the gas replacement dry room of the present invention will be described in detail with reference to FIG. The inside of the airtight booth 1 is kept clean with a low dew point and an inert gas. The airtight booth 1 may be a glove box, a dry room, or the like. The airtight booth 1 houses a manufacturing device 2 used for manufacturing OLEDs and research and development, and when cleanliness is required, air such as a HEPA filter or ULPA filter is stored in the air supply portion in the upper part of the airtight booth 1. It is configured to have a purification filter 3. The air purification filter 3 may be a plurality of fan filter units. Nitrogen gas or dry air as a utility is supplied to the container 1 through the pipe a.

In the desiccant dehumidifier 16, the honeycomb rotor 5 is divided into a processing zone 6, a purge zone 7, and a regeneration zone 8. The honeycomb rotor 5 can continuously absorb and desorb moisture while being rotated by a rotor drive motor 9 such as a geared motor. The gas to be processed is cooled and supplied to the processing zone 6 of the honeycomb rotor 5 by the precooler 11 through the blower 10. A part of the gas to be processed is branched in front of the processing zone 6, passes through the purge zone 7, is heated by the regeneration heater 14, and is sent to the regeneration zone 8. The gas that has passed through the regeneration zone 8 is cooled by the cooler 15, and the moisture in the recycled gas desorbed from the honeycomb is removed as a drain of condensed water and returned to the front of the blower 10. The gas to be processed that has passed through the honeycomb in the processing zone 6 is heated by the afterheater 12 as needed and is supplied to the airtight booth 1 as supply air SA. In this embodiment, the honeycomb rotor 5 having the purge zone 7 is used, but the present invention is not limited to this, and a configuration may use a honeycomb rotor divided into a processing zone and a regeneration zone.

In the nitrogen purifier 23, the catalyst containers 18 and 19 for purifying nitrogen contain metal catalysts such as a copper catalyst and a platinum catalyst, and are composed of two towers. When the catalyst breaks, the temperature is raised by the heaters 20 and 21 while flowing nitrogen gas and hydrogen gas to regenerate the catalyst. In this embodiment, the present invention is not limited to a copper catalyst, a platinum catalyst, or the like, and a catalyst containing copper and / or platinum as a main component or another metal catalyst used for removing oxygen may be used. Good. In addition to pellets, the metal catalyst may be granular, powdery, supported on a carrier, or the like. In this embodiment, the catalyst container is of the two-tower type, but the present invention is not limited to this, and one-tower type or a plurality of towers may be provided.

If the nitrogen gas supply facility has spare capacity, install a desiccant dehumidifier and a nitrogen purifier in an airtight room to supply nitrogen gas to the room, and invade the active gas from the desiccant dehumidifier 16. It may be configured to suppress.

First, the operation of the gas replacement dry room of the present invention having the above configuration will be described with respect to an atmospheric break for performing maintenance, setup change, adjustment, and the like of the airtight booth 1.

(Atmospheric break)
By closing the valves 26, 29, 30 and opening the valves 27, 28 and introducing the dry air from the dry air supply device (not shown) from the pipe a from the upper part of the airtight booth 1, the nitrogen gas is introduced into the dry air. Replace with. By providing dry air with a low dew point from the upper part of the airtight booth 1 in one pass, a large amount of air can be safely supplied at one time, so that the replacement speed of nitrogen and air can be significantly shortened. By supplying dry air in one pass from the upper part of the air purification filter 3 which is the easiest to retain the moisture in the airtight booth 1 without circulating the inside of the airtight booth 1, the moisture content even if a person works inside. Is discharged to the outside without remaining in the container 1.

During the atmospheric break, there are the following cases (1) and (2).

(1) On the other hand, in the inert gas circulation line, the valves 29 and 30 are closed during the atmospheric break, so that the inert gas circulates in the desiccant dehumidifier 16 and the nitrogen purifier 23. At this time, by operating the valve, the optimum operating environment can be prepared by changing the flow rate and the number of circulations of the gas flowing through each device. The valve is not limited to this, and an air volume adjusting device such as a damper or VAV (Variable Air Volume) may be used.

(2) Further, when there is one airtight booth as shown in FIG. 1, the inside of the airtight booth 1 can be dehumidified by the desiccant dehumidifier 16 during the atmospheric break. In this case, the valves 29, 30 and 31 are opened and the valves 33 and 34 are closed. The return air RA from the airtight booth 1 is mixed with the return gas from the regeneration zone 8 of the desiccant dehumidifier 16 through the pipe b, cooled by the precooler 11 by the blower 10, and processed zone 6 of the honeycomb rotor 5 as the gas to be processed. Is supplied to. Further, a part of the gas to be treated is branched in front of the treatment zone 6, passes through the purge zone 7, is heated by the regeneration heater 14, and is sent to the regeneration zone 8. The low dew point gas that has passed through the treatment zone 6 is supplied to the airtight booth 1 through the pipe c as an air supply SA. By performing the circulation operation in this way, it is possible to reduce the supply amount of dry air as a utility while maintaining the low dew point environment of the airtight booth 1.

Next, nitrogen substitution and circulation operation of the airtight booth 1 will be described.

(Nitrogen replacement operation)
After the atmospheric break, the inside of the airtight booth 1 is replaced with nitrogen to reduce the oxygen concentration to a specified concentration such as 100 ppm or less. Depending on the cases (1) and (2) of the atmospheric break, the nitrogen substitution operation is as follows.

(1) First, the valve 27 is closed and the valve 26 is opened. Nitrogen gas from a nitrogen cylinder, a nitrogen gas supply device (not shown), or the like is supplied to the airtight booth 1 through the pipe a. The return air RA from the airtight booth 1 opens the valve 28 by the pipe b and exhausts the air. By making the nitrogen gas supplied from the upper part of the airtight booth 1 in one pass, a large amount of gas can be supplied at one time. Therefore, the air remaining in the airtight booth is replaced with nitrogen gas at once, and the replacement speed of nitrogen and air is increased. Can be significantly shortened. Continue until the oxygen concentration in the airtight booth 1 drops to 100 ppm.

(2) Perform the same operation as in (1). The nitrogen gas supplied into the airtight booth 1 is exhausted through the valve 28, but the remaining gas passes through the regeneration zone 8 of the honeycomb rotor, is mixed with the gas cooled by the cooler 15, and is a honeycomb as a gas to be processed. It is introduced into the processing zone 6 of the rotor 5. A part of the gas to be processed is branched in front of the processing zone 6, passes through the purge zone 7, is heated by the regeneration heater 14, and is sent to the regeneration zone 8. At this time, since the valve 31 is open and the valves 33 and 34 are closed, the active gas such as oxygen does not flow into the nitrogen refiner 23. The gas to be processed that has passed through the honeycomb in the processing zone 6 is heated by the afterheater 12 as needed, and is supplied to the airtight booth 1 as supply air SA through the pipe c. In this way, nitrogen gas is supplied to replace the gas in the airtight booth 1, and the water accumulated in the airtight booth 1 after the atmospheric break is dehumidified to dehumidify the water concentration and the oxygen concentration in the airtight booth 1. Gradually decreases. This circulation operation is performed until the oxygen concentration in the airtight booth 1 becomes 100 ppm or less, and the inside of the airtight booth 1 is replaced with nitrogen gas.

(Oxygen removal / nitrogen purification operation)
After the oxygen concentration in the airtight booth 1 drops to a specified concentration such as 100 ppm or less, the valves 28 and 31 are closed and the valves 33, 34, 35 and 36 are opened. At this time, the other valves of the nitrogen purifier 23 are left closed. As a result, the gas that has passed through the purge zone 7 of the honeycomb rotor 5 is introduced into the catalyst container 18 of the nitrogen purifier 23, and oxygen removal is started by the metal catalyst in the catalyst container 18. Further, by narrowing the valve 26, the supply flow rate of nitrogen passing through the pipe a is reduced, and the positive pressure in the airtight booth 1 is maintained while supplying nitrogen gas. The return air RA from the airtight booth 1 is supplied to the honeycomb rotor 5 as a gas to be processed through the pipe b.

The gas flow in the desiccant dehumidifier 16 is as described above. The gas that has passed through the purge zone 7 is heated by the heat of adsorption of the honeycomb. On the other hand, since the metal catalyst easily reacts with oxygen under relatively high temperature conditions, it is convenient to supply the high temperature gas that has passed through the purge zone to the catalyst container. Assuming that copper is contained in the metal catalyst, for example, oxygen is removed by reacting with oxygen and oxidizing the copper to become copper oxide as shown in the following equation.
2Cu + O ₂ → 2CuO

The gas that has passed through the nitrogen refiner 23 is heated by the heater 14 and introduced into the regeneration zone 8 of the honeycomb rotor 5. The gas that has passed through the regeneration zone 8 passes through the processing zone 6 again and is supplied to the airtight booth 1 as an air supply SA. By performing the circulation operation in this way, the oxygen concentration and / or the water concentration gradually decreases. For example, the circulation operation is performed until a specified concentration such as a water concentration of 10 ppm and an oxygen concentration of 1 ppm or less is reached. After that, the operation of the manufacturing apparatus 2 is started, and experiments for manufacturing OLED and research and development are started. In this embodiment, the gas flows through the catalyst container 18, but the gas may flow through the catalyst container 19. That is, two catalyst containers are installed in parallel (two-tower type), and while the catalyst in one catalyst container is being regenerated, nitrogen purification treatment is performed in the other catalyst container. In addition, the present invention is not limited to this, and may be composed of one or a plurality of nitrogen purifiers composed of one or a plurality of catalyst containers.

In the first embodiment, the gas that has passed through the purge zone is sent to the nitrogen purifier, but the gas that has passed through the treatment zone or the gas that has passed through the purge zone and the gas that has passed through the treatment zone are mixed and supplied. It may be. Alternatively, a utility that supplies nitrogen gas used for nitrogen substitution may be connected to a nitrogen refiner to supply nitrogen gas to an airtight booth. Since the low dew point gas dehumidified by the honeycomb rotor flows through the catalyst container, it is difficult for water to accumulate.

(Catalyst regeneration operation)
When the catalyst ruptures and the gas passing through the catalyst container exceeds a specified concentration such as an oxygen concentration of 1 ppm, the catalyst regeneration operation is started. For example, when the catalyst in the catalyst container 18 breaks, the valves 35 and 36 are closed, the valves 37 and 38 are opened, and the gas that has passed through the purge zone 7 is switched to flow into the catalyst container 19. Next, the valves 39, 40, 43, 44 are opened, and the nitrogen gas containing hydrogen gas adjusted to a predetermined concentration is injected into the catalyst container 18 from a nitrogen gas supply device containing hydrogen gas, a nitrogen gas supply device (not shown), or the like. Supply to. At the same time, it is heated by the heater 20. For example, when copper is contained in the metal catalyst, for example, copper oxide reacts with hydrogen to be reduced as shown in the following equation, and oxygen is removed by becoming copper, the catalyst is regenerated, and the vacuum pump 22 vacuums. It is pulled and exhausted.
CuO + H ₂ → Cu + H ₂ O
The water discharged by the reaction is discharged as a drain by opening the valve 46.

With the above configuration, it is possible to make a space-saving gas replacement system, and it is possible to suppress the initial cost required for piping and installation work.

FIG. 2 shows a flow chart of the dry room of the present invention in Example 2. In the first embodiment, one airtight booth is used, but in the second embodiment, a plurality of airtight booths are configured. In FIG. 2, the configuration is composed of three airtight booths 1A, 1B, and 1C, but the present invention is not limited to this, and two or four or more may be provided. Since the apparatus configuration of the second embodiment is almost the same as that of the first embodiment, a duplicate description will be omitted.

When there are a plurality of airtight booths, even if some of the airtight booths have an atmospheric break, the inert gas can be circulated in another airtight booth to maintain the oxygen removal / nitrogen purification operation. Therefore, it is possible to significantly shorten the recovery time from the atmospheric environment after the atmospheric break to the environment with a low dew point and an inert gas concentration. In addition, since one desiccant dehumidifier and a nitrogen refiner can cover the gas supply of each airtight booth, the cost can be suppressed. The system of the present invention has a feature that the larger the line, the greater the cost merit.
In Example 2, one desiccant dehumidifier and a nitrogen purifier were used to supply the gas, but a plurality of desiccant dehumidifiers and / or nitrogen purifiers were used to supply the inert gas to the airtight booth. It may be configured.

In the following description of Example 2, the airtight booth 1A performs an atmospheric break from the inert gas environment, and after the atmospheric break, returns from the atmospheric environment to the low dew point / inert gas environment to perform oxygen removal / nitrogen purification operation. To do. During this period, the airtight booths 1B and 1C will continue to perform oxygen removal and purification operations.

(Atmospheric break)
A case where the airtight booth 1A is returned to the atmospheric environment by an atmospheric break will be described. By closing the valves 26, 47B, 47C, 48A, 51A and opening the valves 27, 47A, 50A and introducing the dry air from the upper part of the airtight booth 1A through the pipe a, the nitrogen gas is replaced with the dry air. By providing dry air with a low dew point from the upper part of the airtight booth 1A in one pass, a large amount of air can be safely supplied at one time, so that the replacement speed of nitrogen and air can be significantly shortened. In the case of an atmospheric break in all airtight booths, by closing all valves 48 and opening valves 49, the desiccant dehumidifier and nitrogen purifier can be circulated independently of the airtight booth. Since the inert gas can be maintained, the recovery time from the atmospheric break to the inert gas circulation operation is shortened.

(Nitrogen replacement operation)
After the atmospheric break, the inside of the airtight booth 1A is replaced with nitrogen gas to reduce the oxygen concentration to a predetermined concentration or less. First, the valve 27 is closed, the valve 26 and the valve 47A are opened, and nitrogen gas is supplied to the airtight booth 1A through the pipe a. When nitrogen gas is supplied through the pipe a in each airtight booth, the flow rate of the supplied gas can be adjusted by the flow meter 24 and the valve 47. The return air RA from the airtight booth opens the valve 50A and exhausts. In this way, the nitrogen replacement operation is performed in one pass until the oxygen concentration in the airtight booth 1 becomes equal to or lower than the specified concentration, and the inside of the airtight booth 1 is replaced with nitrogen gas. On the other hand, since the airtight booths 1B and 1C are in the oxygen removal / nitrogen refining operation, the valves 50B and 50C are closed and the valves 51B and 51C are open, the inert gas is sent to the desiccant dehumidifier 16 by the pipe b in the return air RA. be introduced. Here, since the valve 48A is closed, oxygen gas flows into the desiccant dehumidifier 16 and the nitrogen purifier 23 and has no effect. Further, the flow rate can be adjusted by opening the valve 49 and bypassing the pipe d.

RA from the airtight booths 1B and 1C and the inert gas bypassed through the pipe d are mixed, and the gas that has passed through the regeneration zone 8 of the honeycomb rotor 5 is further mixed, and the processing zone 6 of the honeycomb rotor 5 is mixed as the gas to be processed. Introduce to. Here, the valve 31 is closed, and the gas that has passed through the purge zone 7 is introduced into the nitrogen purifier 23, and the oxygen removal / nitrogen purification operation is performed as in the first embodiment.

When all the airtight booths are operated to replace nitrogen from the state of atmospheric break, the valves 31 are opened, the valves 33 and 34 are closed, and the active gas does not flow into the nitrogen refiner 23. Drive in the same way.

(Oxygen removal / nitrogen purification operation)
After the oxygen concentration in the airtight booth 1A drops below the specified concentration, the valve 50A is closed and the valve 51A is opened. Further, the valve 26 is throttled to reduce the supply flow rate of nitrogen gas passing through the pipe a, and the positive pressure in the airtight booth 1 is maintained while supplying nitrogen gas. The return air RA from the airtight booth 1 is supplied to the honeycomb rotor 5 as a gas to be processed through the pipe b. The gas that has passed through the purge zone 7 of the honeycomb rotor 5 is introduced into the nitrogen refiner 23 by the blower 17. The inert gas that has passed through the nitrogen purifier 23 is heated by the regeneration heater 14 and introduced into the regeneration zone 8 of the honeycomb rotor 5. The gas that has passed through the regeneration zone 8 passes through the processing zone 6 again and is supplied to the airtight booth 1 as an air supply SA. By performing the circulation operation in this way, the oxygen concentration and / or the water concentration gradually decreases. When the specified concentration is reached, the operation of the manufacturing apparatus 2 is started, and experiments for manufacturing OLED and research and development are started. In FIG. 2, the catalyst container is a two-tower type, but the present invention is not limited to this as in the first embodiment.

By connecting a desiccant dehumidifier and a nitrogen refiner to form an integrated device, it is possible to create a gas replacement system that saves space compared to Patent Document 3, and reduces the initial cost for piping and installation work. It becomes possible to suppress it.

From the above, it is possible to shorten the recovery time from the air environment after the air break of the airtight booth 1 to the return to a clean environment with a low dew point and an inert gas to 1/5 to 1/10 of the conventional technique. it can. Further, it is possible to realize a gas replacement system in which the inside of the airtight booth 1 can be easily optimized for an inert gas environment at a low dew point.

The present invention can also be used for storage containers such as glove boxes and dry rooms used for developing lithium-ion battery materials that need to keep the storage space clean with low dew point and low active gas concentration. it can.

1 Airtight booth 2 Manufacturing equipment 3 Air purification filter 4 Gas circulation path 5 Honeycomb rotor 6 Processing zone 7 Purge zone 8 Regeneration zone 9 Rotor drive motor 10, 17 Blower 11 Precooler 12 After heater 13 Air filter 14 Regeneration heater 15 Cooler 16 Desiccant Dehumidifier 18, 19 Catalyst vessel 20, 21 Heater 22 Pump 23 Nitrogen purifier 24, 25 Flow meter 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51 valves

Claims (7)

An airtight booth connecting a dry air supply device and an inert gas supply device is provided, and an inert gas purification device is connected after the low dew point gas supply device to integrate the gas, and the gas that has passed through the low dew point gas supply device is said to be the same. The low dew point gas that has passed through the inert gas purification device and has passed through the low dew point gas supply device is supplied to the airtight booth through a filter that removes foreign substances, and the gas inside the airtight booth is supplied to the low dew point. A dry room for gas replacement, characterized by having a pipeline that recirculates to the gas supply device. The gas replacement dry room according to claim 1, further comprising a switching means for bypassing the gas that has passed through the low dew point gas supply device to the airtight booth so that the gas has not passed through the inert gas purification device. The gas replacement dry room according to claim 1 and 2, wherein the airtight booth comprises one or more. The gas replacement dry room according to claim 1 to 3, wherein the foreign matter removing filter is a fan filter having a built-in HEPA filter and / or ULPA filter. The gas replacement dry room according to any one of claims 1 to 4, wherein the inert gas purifier is a nitrogen purifier containing a catalyst containing copper and / or platinum as a main component. The gas replacement dry room according to claim 1 to 5, wherein the low dew point gas supply device is a desiccant dehumidifier. The gas replacement dry room according to claim 6, wherein the air that has passed through the purge zone of the desiccant dehumidifier is supplied to the inert gas purifier.

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