KR20200137961A - Dry room for gas replacement - Google Patents

Abstract

There is provided a gas replacement system capable of performing switching of an atmosphere environment, a low dew point, and an inert gas environment in a relatively short time in a drying room having an inert gas concentration in which a manufacturing device is contained.
It is a gas replacement system for booths that need to keep the inside clean with a low dew point and inert gas concentration.During maintenance or repair, dry air is put in the booth in one pass and moisture is discharged to the outside of the device. All circulation lines are closed with valves or the like and independently circulated, so that even when there are a plurality of booths, the idle time by the standby brake can be greatly shortened. By connecting the low dew point gas supply device and the inert gas purification device to form an integral type, space is saved and the cost is reduced.

Description

Dry room for gas replacement {DRY ROOM FOR GAS REPLACEMENT}

The present invention relates to a drying chamber, a chamber, and a booth having a concentration of an inert gas (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 equipped with an organic EL display manufacturing device. For maintenance or adjustment of the system, a dehumidification device capable of switching to an environment with a low dew point (hereinafter, referred to as "low dew point" when the dew point temperature is 0 degrees or less) in a relatively short time, relates to a gas replacement system including a gas purifier. will be.

BACKGROUND ART Conventionally, organic EL elements used in organic EL displays and the like expected as next-generation flat panel displays instead of liquid crystal displays are promising for use as solid-state light-emitting type inexpensive large-area full-color display elements and write light source arrays. Active research and development has been in progress. However, organic materials such as organic light emitting materials used in organic EL devices, electrodes, and the like are weak to moisture, and their performance and characteristics are rapidly deteriorated due to moisture in the air. Therefore, even at the time of experiments according to these developments, it is necessary to carry out production or experiments in a booth purged with air with an inert gas such as air having a very low dew point or nitrogen gas obtained by vaporizing liquid nitrogen.

In addition, currently, in the manufacture of organic EL displays (OLEDs), using printing techniques such as inkjet technology, a liquid organic EL material is formed into a uniform thin film on a substrate, thereby manufacturing a device with improved production efficiency and performance. Development is taking place. In order to develop such a manufacturing technology, the inside of the booth is filled with an inert gas such as nitrogen gas in order to achieve an inert gas concentration at a low dew point such as 1 ppm of moisture or less and 1 ppm of oxygen or the like around the manufacturing apparatus. However, in the case of performing maintenance or adjustment of the manufacturing apparatus in the booth, it is necessary to return the low dew point inert gas environment to the atmospheric environment (hereinafter, referred to as "atmospheric brake").

At this time, when the inert gas environment is replaced in the normal atmosphere, various parts of the device inside the device adsorb moisture, and when it is returned to the inert gas environment, it takes a very long time to desorb the moisture adsorbed by the parts.

In order to minimize the amount of inert gas for returning back to the inert gas environment from the atmospheric environment after the atmospheric break, and to minimize the idle time of the apparatus, there is a technique described in Patent Document 1 for minimizing the internal volume of the gas enclosure assembly.

Patent Document 2 discloses a glove box equipped with an inert gas circulation purification device. According to this, in order to maintain a constant atmosphere of the inert gas in the glove box, and to efficiently remove oxygen and moisture, a metal catalyst charging unit filled with a metal catalyst that removes oxygen from the gas, and a metal catalyst charging unit that adsorbs and removes moisture in the gas. By an adsorption tower composed of a desiccant filling part filled with a desiccant of a molar sieve, it is configured to supply a circulating gas from which oxygen and moisture are removed, and the gas in the glove box is sucked out by a circulation pump, and oxygen and moisture are removed while passing through the adsorption tower. It is removed and returned back to the glove box, and gas circulation is performed.

Japanese Patent Publication No. 6153539 Japanese Patent Publication No. 5676521 Japanese Unexamined Patent Publication No. 2019-52835

Patent Document 1 discloses that the gas enclosure is framed and the internal volume is made as small as possible, thereby minimizing the amount of inert gas in the gas enclosure, minimizing the downtime due to maintenance, etc., and in the installation area of various OLED manufacturing apparatuses. You can optimize your workspace to adapt. However, there is a problem that it takes too much time to return the inside of the booth to an inert gas environment with low humidity again, since the gas purification system that accompanies during rest and simultaneously performs inert gas purification and moisture removal is also stopped. In addition, the gas purification device and the dehumidifying device are in the same mechanism, and the purification rate is different between oxygen and moisture, and there is a problem that it is difficult to remove the moisture at the same time because it takes a very long time to remove the moisture compared to the removal of oxygen.

Even in the conventional system as in Patent Document 2, since oxygen removal and water removal are performed in a series column, equipment selection has been performed in accordance with the water removal capacity rate. As described above, in the prior art, the recovery time from the standby brake to the return to the inert gas environment becomes longer, and thus it takes time to start the line of the manufacturing apparatus.

Accordingly, as in Patent Document 3, a dry room for gas replacement has been developed in which moisture is removed using a desiccant rotor and a low dew point gas is supplied, so that the time to reach a predetermined moisture concentration is significantly shortened. Compared with the pellet-shaped molecular sieve used for moisture removal in Patent Document 2, the advantage of using a desiccant rotor for moisture removal is that it has a large surface area, low pressure loss, and a very thin honeycomb wall because it is in a honeycomb shape. Since the adsorption moisture diffuses quickly, adsorption and desorption is performed in an instant in the whole honeycomb element.

In the dry room for gas replacement of Patent Document 3, an airtight container for storing a manufacturing device used for manufacturing or research and development of OLEDs is provided inside the drying chamber in which dry air from the dry air supply device is circulated. Inert gas and low dew point gas are supplied to the hermetic container. In addition, the inert gas purification device and the 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 to control each other independently. Can be adjusted with Further, by circulating the circulation path provided separately during the atmospheric brake, the return time for returning from the atmospheric environment after the atmospheric brake of the airtight container to the inert gas environment can be greatly 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 hermetic booth quickly reaches a low state even after the standby brake.

In the present invention, the drying chamber covering the airtight container described in Patent Document 3 and the drying air supply device for supplying and circulating dry air into the drying chamber are omitted, and a low dew point gas purification device and an inert gas purification device are connected to each other to form an integral structure. , Compared with the dry room for gas replacement of Patent Document 3, it aims at simplifying the apparatus, saving space, and simplifying the operation method.

In order to solve the above problems, the present invention provides an airtight booth for storing a manufacturing device used for manufacturing or research and development of OLEDs, and supplying low dew point gas and inert gas to the airtight booth, and an inert gas purification device And the low dew point gas supply device are connected and integrated, and if necessary, a switching means for passing the bypass path so that the gas that has passed the low dew point gas supply device does not pass through the inert gas purification device is provided. When a person enters the booth, dry air is supplied to the airtight booth, while the inert gas is separated from the supply to the airtight booth and can be maintained in closed loop circulation, so that the downtime due to the standby brake can be greatly shortened. . Alternatively, the supply amount of dry air can be reduced by operating the low dew point gas supply device during the atmospheric brake without closed loop circulation. Water molecules are polar substances, and when air is introduced into an airtight booth that needs to be kept at a low dew point, moisture will adhere to the walls of the airtight booth or inside the filter. In order to discharge the adhering moisture, it is necessary to supply low dew point air for a long time, but in the case of the present invention, since dry air is supplied with the supply of inert gas stopped, it is quickly inside the airtight booth even after the atmospheric brake. The dew point can reach a low state.

In addition, even if it is nitrogen gas contained in a cylinder as an inert gas, nitrogen gas obtained by evaporating liquefied nitrogen, or nitrogen gas obtained by removing oxygen from air by deep cooling separation or pressure swing adsorption (PSA), membrane separation method, etc. It is high, and the cost increases if the time of the standby brake or the return time to return to the inert gas environment after the standby brake is not shortened. On the other hand, cost can be reduced by making the low dew point gas into a desiccant rotor and stopping the supply of the inert gas while maintaining the supply of the low dew point gas to perform maintenance or the like.

Moisture removal is performed with a desiccant dehumidifier to significantly shorten the moisture removal time, and at the same time, a part of the low dew point gas is introduced into the inert gas purification device to remove oxygen.Therefore, the amount of gas treated with the desiccant dehumidifier and the inert gas By adjusting the amount of gas to be introduced into the refining device, a dry room with an inert gas concentration can be created under optimal operating conditions.

Since the dry room for gas replacement of the present invention is configured as described above, it is not circulated from the air purification filter such as HEPA filter or ULPA filter installed on the upper part of the container even during the atmospheric brake, but in one direction (hereinafter referred to as "one pass"). By supplying dry air to the filter, the filter that is most likely to retain moisture is prevented from retaining moisture, and maintenance, repair, and switching are performed. Further, an inert gas purification device was connected behind the desiccant dehumidifier to be integrated, and the circulation path provided separately during the atmospheric brake was circulated to prevent the circulating air from approaching the atmosphere. By doing in this way, the return time for returning to the low dew point and inert gas environment from the atmospheric environment after the atmospheric brake of the airtight booth can be greatly shortened. In addition, by adjusting the flow rate of the gas flowing from the dehumidifying device to the inert gas purification device, it is possible to obtain a dry room that has a low dew point in a short time and can be optimized for an inert gas environment.

1 is a flow diagram in the first embodiment of the dry room of the present invention.
Fig. 2 is a flow diagram in Example 2 of the dry room of the present invention.

EMBODIMENT OF THE INVENTION Below, the form for carrying out this invention is demonstrated using drawing. In addition, the present invention is not limited to the following examples.

In this embodiment, as a gas replacement dehumidification device and gas replacement method for a container that needs to be kept clean with a low dew point and inert gas, the production or research and development of an organic EL display (OLED) using a printing technology such as inkjet technology. The booth of the device will be described as an example. In addition, the present invention is not limited to OLED manufacturing or research and development equipment, and it is necessary to keep the storage space clean in a low dew point, inert gas environment, such as a glove box used for the development of lithium ion battery materials or semiconductor fields. It can also be used for a storage container or a closed space.

Example 1

Hereinafter, a first embodiment of a dry room for gas replacement of the present invention will be described in detail with reference to FIG. 1. The airtight booth 1 keeps the inside clean with a low dew point and an inert gas. The airtight booth 1 may be a glove box or a dry room. In the airtight booth 1, a manufacturing apparatus 2 used for manufacturing or research and development of OLEDs is stored, and when cleanliness is required, a HEPA filter or a ULPA filter, etc. It is configured with an air purification filter (3). Moreover, about the air purification filter 3, it is good also as a plurality of fan filter units. The airtight booth 1 is supplied with nitrogen gas or dry air as a utility through a 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 rotating 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 in a cooler 15, and the moisture in the regeneration gas desorbed from the honeycomb is removed as a drain of condensed water, and is 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 after-heater 12 as necessary, and is supplied to the hermetic booth 1 as air supply SA. In this embodiment, the honeycomb rotor 5 having the purge zone 7 is used, but the present invention is not limited thereto, and a honeycomb rotor divided into two into a processing zone and a regeneration zone may be used.

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 constituted by two towers. When the catalyst breaks through, nitrogen gas and hydrogen gas are flowed and the temperature is raised by the heaters 20 and 21 to regenerate the catalyst. In addition, in this embodiment, it is not limited to a copper catalyst, a platinum catalyst, etc., A catalyst containing copper and/or platinum as a main component, or another metal catalyst used for the purpose of removing oxygen may be used. In addition to pellets, the metal catalyst may be granular, powdery, or supported on a carrier. In the present embodiment, the catalyst container is a two-column type, but it is not limited thereto, and a single-column type or a plurality of columns may be provided.

When the nitrogen gas supply facility has sufficient capacity, a desiccant dehumidifier and a nitrogen purifier are installed in an airtight room, and nitrogen gas is supplied to the room to suppress the intrusion of active gas from the desiccant dehumidifier 16. It may be configured.

The operation of the dry room for gas replacement of the present invention having the above-described configuration is first described with respect to a standby brake for performing maintenance, switching, adjustment, etc. of the hermetic booth 1.

(Standby brake)

By closing the valves 26, 29, 30, opening the valves 27, 28 to introduce dry air from a dry air supply device (not shown), etc., from the top of the airtight booth 1 from the pipe a , Nitrogen gas is replaced with dry air. By allowing the low dew point dry air to be supplied from the top of the airtight booth 1 in one pass, since a large amount of air can be safely supplied at a time, the rate of substitution of nitrogen and air can be greatly shortened. Among the airtight booths (1), dry air is supplied from the top of the air purification filter (3), which is the easiest to keep moisture, in one pass without circulating the inside of the airtight booth (1). It does not remain in the booth 1 and is discharged outside.

Among the standby brakes, there are the following cases (1) and (2).

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

(2) In addition, 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 standby brake. In this case, the valves 29, 30, 31 are opened, and the valves 33, 34 are closed. Ventilation (RA) from the airtight booth (1) is mixed with the return gas from the regeneration zone (8) of the desiccant dehumidifier (16) through a pipe (b), and is free by the blower (10). It is cooled by the cooler 11 and supplied to the processing zone 6 of the honeycomb rotor 5 as a target gas. In addition, 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 low dew point gas that has passed through the treatment zone 6 is supplied to the airtight booth 1 through a pipe c as a supply air SA. In this way, by circulating operation, the supply amount of dry air as a utility can be reduced while maintaining the low dew point environment of the hermetic booth 1.

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

(Nitrogen substitution operation)

After the atmospheric brake, the inside of the airtight booth 1 is replaced with nitrogen so that the oxygen concentration is less than or equal to the specified concentration such as 100 ppm or less. According to the case (1) and (2) of the standby brake, 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 or a nitrogen gas supply device (not shown) is supplied to the hermetic booth 1 through the pipe (a). Ventilation (RA) from the airtight booth (1) is exhausted by opening the valve (28) by the pipe (b). Since nitrogen gas is supplied in one pass from the top of the hermetic booth 1, a large amount of gas can be supplied at a time, so that the air remaining in the hermetic booth is replaced with nitrogen gas at once, and the rate of substitution of nitrogen and air Can be greatly shortened. It continues until the oxygen concentration in the hermetic booth 1 decreases to 100 ppm.

(2) Perform the same operation as in (1). The nitrogen gas supplied in the airtight booth 1 is exhausted through the valve 28, but the remaining gas passes through the regeneration zone 8 of the honeycomb rotor 5 and is mixed with the gas cooled by the cooler 15. As a result, it is introduced into the processing zone 6 of the honeycomb rotor 5 as a target gas. 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. Further, at this time, since the valve 31 is open and the valves 33 and 34 are closed, an active gas such as oxygen does not flow into the nitrogen purifier 23. The gas to be treated, which has passed through the honeycomb in the treatment zone 6, is heated by the after heater 12 as necessary, and is supplied as a supply air SA to the hermetic booth 1 through the pipe c. In this way, by supplying nitrogen gas to displace the gas in the hermetic booth 1 and dehumidifying the moisture stored in the hermetic booth 1 after the atmospheric brake, the moisture concentration and the oxygen concentration in the hermetic booth 1 gradually decrease. do. This circulation operation is performed until the oxygen concentration in the hermetic booth 1 becomes 100 ppm or less, and the inside of the hermetic booth 1 is replaced with nitrogen gas.

(Oxygen removal and nitrogen purification operation)

After the oxygen concentration in the hermetic booth 1 has decreased 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 valve of the nitrogen purifier 23 is left closed. Thereby, 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 tightening the valve 26, the supply flow rate of nitrogen passing through the pipe a is reduced, and a positive pressure in the airtight booth 1 is maintained while supplying nitrogen gas. Ventilation RA from the hermetic booth 1 is a gas to be processed and is supplied to the honeycomb rotor 5 through a pipe b.

The flow of gas 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 appropriate to supply a high-temperature gas that has passed through the purge zone to the catalyst container. Assuming that the metal catalyst contains copper, for example, copper reacts with oxygen and oxidizes as shown in the following equation, and oxygen is removed by becoming copper oxide.

2Cu+O ₂ →2CuO

The 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 is again supplied to the hermetic booth 1 as a supply air SA through the processing zone 6. By performing the circulation operation in this way, the oxygen concentration and/or the moisture concentration gradually decrease. For example, circulation operation is performed until a specified concentration such as 10 ppm of water concentration and 1 ppm of oxygen concentration is reached. After that, operation of the manufacturing apparatus 2 is started, and an experiment for OLED manufacturing and research and development is started. In addition, in the present embodiment, the gas flows through the catalyst container 18, but the gas flow through the catalyst container 19 may be used. That is, two catalyst vessels are installed in parallel (two-column type), and while the catalyst in one catalyst vessel is being regenerated, nitrogen purification treatment is performed in another catalyst vessel. Further, the present invention is not limited thereto, and may be constituted by one or more nitrogen purifiers comprising one or more catalyst containers.

In Example 1, 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 may be mixed and supplied. Alternatively, a utility for supplying nitrogen gas used at the time of nitrogen replacement may be connected to a nitrogen purifier to supply nitrogen gas to an airtight booth. Further, since the low dew point gas dehumidified by the honeycomb rotor circulates through the catalyst container, moisture is difficult to be stored.

(Catalyst regeneration operation)

When the catalyst breaks through and the gas that has passed through the catalyst container exceeds a specified concentration such as an oxygen concentration of 1 ppm, the regeneration operation of the catalyst is started. For example, when the catalyst in the catalyst container 18 breaks through, 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 transferred to the catalyst container 19. ) To flow. Next, by opening the valves 39, 40, 43, 44, nitrogen gas containing hydrogen gas adjusted to a predetermined concentration from a nitrogen gas supply device containing hydrogen gas or a nitrogen gas supply device (not shown), etc. Is supplied to the catalyst vessel 18. At the same time, it is heated by the heater 20. For example, if the metal catalyst contains copper, for example, copper oxide is reduced by reacting with hydrogen as shown in the following equation, and oxygen is removed by becoming copper, and the catalyst is regenerated, and the vacuum pump 22 It is sucked in by vacuum and exhausted.

CuO+H ₂ →Cu+H ₂ O

In addition, water discharged by the reaction is discharged as a drain by opening the valve 46.

With the above configuration, it becomes possible to provide a space-saving gas replacement system, and it becomes possible to suppress the initial cost incurred in piping or installation work.

Example 2

Fig. 2 shows a flow diagram in Example 2 of the dry room of the present invention. In Example 1, one airtight booth was used, but in Example 2, it was constituted by a plurality of airtight booths. In addition, in FIG. 2, although it was made into the structure which consists of three airtight booths 1A, 1B, and 1C, it is not limited to this, You may provide 2 or 4 or more. In the second embodiment, since the configuration of the device in the first embodiment is substantially the same, redundant descriptions are omitted.

When there are a plurality of hermetic booths, even if some hermetic booths are in the air brake, inert gas is circulated in the other hermetic booths to maintain the oxygen removal and nitrogen purification operation. For this reason, the return time for returning from the atmospheric environment after the atmospheric brake to the environment with a low dew point and an inert gas concentration can be greatly shortened. In addition, since one desiccant dehumidifier and nitrogen purifier can supply gas to each hermetic booth, cost can be suppressed. The system of the present invention is characterized in that the larger the line, the greater the cost merit.

Further, in Example 2, it was configured to supply from one desiccant dehumidifier and nitrogen purifier, but may be configured to supply an inert gas to an airtight booth from a plurality of desiccant dehumidifiers and/or nitrogen purifiers.

In the description of Example 2 below, the airtight booth 1A performs an atmospheric brake from an inert gas environment, and after the atmospheric brake, returns from the atmospheric environment to a low dew point/inert gas environment to perform oxygen removal and nitrogen purification operation. do. In the meantime, it is assumed that the airtight booths 1B and 1C continue to perform oxygen removal and purification operations.

(Standby brake)

A case in which the airtight booth 1A is returned to the atmospheric environment by the atmospheric brake will be described. By closing the valves 26, 47B, 47C, 48A, 51A, opening the valves 27, 47A, 50A to introduce dry air from the top of the hermetic booth 1A through the pipe (a), nitrogen gas is introduced. Replace with dry air. By allowing the low dew point dry air to be supplied from the top of the airtight booth 1A in one pass, since a large amount of air can be safely supplied at a time, the rate of substitution of nitrogen and air can be greatly shortened. In addition, in the case of a standby brake in the entire hermetic booth, by circulating the desiccant dehumidifier and the nitrogen purifier independently from the hermetic booth by closing all the valves 48 and opening the valve 49 Since the inert gas can be held, the return time from the standby brake to the inert gas circulation operation is shortened.

(Nitrogen substitution operation)

After the atmospheric brake, the inside of the airtight booth 1A is replaced with nitrogen gas to make the oxygen concentration less than or equal to a predetermined concentration. First, the valve 27 is closed, the valve 26 and the valve 47A are opened, and nitrogen gas is supplied to the hermetic booth 1A through the pipe a. In each hermetic booth, when nitrogen gas is supplied through the pipe (a), the flow rate of the gas to be supplied can be adjusted by the flow meter 24 and the valve 47, respectively. Ventilation RA from the airtight booth opens the valve 50A to exhaust air. In this way, nitrogen replacement operation is performed in one pass until the oxygen concentration in the hermetic booth 1 becomes equal to or less than the specified concentration, and the inside of the hermetic booth 1 is replaced with nitrogen gas. Meanwhile, in the airtight booths 1B and 1C, during the oxygen removal/nitrogen purification operation, the valves 50B and 50C are closed and the valves 51B and 51C are open, so that the ventilation RA is performed by the pipe b. An inert gas is introduced into the desiccant dehumidifier 16. 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 performing bypass operation through the pipe d.

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

In addition, when the entire airtight booth is subjected to nitrogen substitution operation from the atmospheric brake state, the valve 31 is opened and the valves 33 and 34 are closed so that no active gas flows into the nitrogen purifier 23. Operate the same as in Example 1.

(Oxygen removal and nitrogen purification operation)

After the oxygen concentration in the hermetic booth 1A is lowered to the specified concentration or less, the valve 50A is closed and the valve 51A is opened. Further, the valve 26 is tightened to reduce the supply flow rate of the nitrogen gas passing through the pipe (a), and while supplying the nitrogen gas, the positive pressure in the airtight booth 1 is maintained. Ventilation RA from the hermetic booth 1 is a gas to be processed and is supplied to the honeycomb rotor 5 through a pipe b. The gas that has passed through the purge zone 7 of the honeycomb rotor 5 is introduced into the nitrogen purifier 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 is again supplied to the hermetic booth 1 as a supply air SA through the processing zone 6. By circulating in this way, the oxygen concentration and/or the moisture concentration decrease more gradually. When the specified concentration is reached, operation of the manufacturing apparatus 2 is started, and an experiment for manufacturing or research and development of OLEDs is started. In addition, in FIG. 2, although the catalyst container was made into a two-column type, as in Example 1, it is not limited to this.

By connecting the desiccant dehumidifier and the nitrogen purifier to form an integrated device, it becomes possible to obtain a gas displacement system that saves space compared to Patent Document 3, and it becomes possible to suppress the initial cost incurred for piping or installation work.

As described above, the return time from the atmospheric environment after the atmospheric brake of the airtight booth 1 to the clean environment with a low dew point and inert gas can be shortened to 1/5 to 1/10 of the prior art. Further, it is possible to realize a gas replacement system capable of easily optimizing the interior of the hermetic booth 1 to a low dew point and inert gas environment.

The present invention can also be utilized for storage containers such as glove boxes and dry rooms used to develop lithium ion battery materials and the like, which need to keep the storage space clean at a low dew point and inert gas concentration.

1 confidential booth
2 manufacturing device
3 air purification filter
4 gas circuit
5 Honeycomb rotor
6 treatment zone
7 purge zone
8 playing zone
9 rotor drive motor
10, 17 blowers
11 precooler
12 after heater
13 air filter
14 regenerative 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 valve

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 behind the low dew point gas supply device to form an integral body, and the gas passing through the low dew point gas supply device is the inert gas. Passing through a purification device, supplying the low dew point gas that has passed through the low dew point gas supply device through a filter for removing foreign matter to the hermetic booth, and recirculating the gas inside the hermetic booth to the low dew point gas supply device Dry room for gas replacement, characterized in that provided with a pipe. The method according to claim 1,
And a switching means for bypassing the gas tight booth so that the gas that has passed through the low dew point gas supply device does not pass through the inert gas purification device. The method according to claim 1 or 2,
A dry room for gas replacement comprising one or more airtight booths. The method according to any one of claims 1 to 3,
A dry room for gas replacement, characterized in that the foreign matter removal filter is a fan filter incorporating a HEPA filter and/or a ULPA filter. The method according to any one of claims 1 to 4,
The dry room for gas replacement, wherein the inert gas purification device is a nitrogen purifier incorporating a catalyst containing copper and/or platinum as a main component. The method according to any one of claims 1 to 5,
The dry room for gas replacement wherein the low dew point gas supply device is a desiccant dehumidifier. The method of claim 6,
A dry room for gas replacement, characterized in that air that has passed through the purge zone of the desiccant dehumidifier is supplied to the inert gas purification device.

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