TWI816980B - Drying room for gas replacement - Google Patents

Abstract

[Problem] The present invention provides a gas replacement system that can switch between an atmospheric environment or a low dew point and inert gas environment in a relatively short period of time in a drying chamber that stores an inert gas concentration in a manufacturing device. [Solution] A gas replacement system that requires a low dew point and an inert gas concentration to keep the interior of the chamber clean. In this gas replacement system, the gas replacement system is configured to provide a one-way flow of gas during maintenance or maintenance. Dry air is introduced into the room and moisture is discharged to the outside of the device. In addition, the inert gas circulation lines are closed by valves, etc. and circulate independently. Even when there are multiple chambers, the downtime due to atmospheric replacement can be greatly shortened. By connecting the low dew point gas supply device and the inert gas purification device to form an integrated model, it becomes space-saving and low-cost.

Description

Drying room for gas replacement

The present invention relates to a gas replacement system including a drying chamber with an inert gas concentration (hereinafter, a gas having an active gas concentration as close as possible to 0 ppm will be referred to as "inert gas") in a room in which an organic EL display manufacturing device is installed. Dehumidification in chambers and chambers that can be switched to a low dew point (hereinafter, a dew point temperature below 0 degrees is referred to as "low dew point") environment in a short period of time for maintenance or adjustment of manufacturing equipment, etc. Devices and gas purifiers.

Conventionally, organic EL elements used in organic EL display devices, etc., which are expected to be next-generation flat panel displays to replace liquid crystal display devices, have been widely used as solid-state light-emitting type inexpensive large-area full-color display elements or writing light source arrays. prospects, thereby conducting active research and development. However, organic substances and electrodes such as organic light-emitting materials used in organic EL elements have weak resistance to moisture, and their performance or characteristics are rapidly deteriorated by moisture in the air. Therefore, when conducting experiments related to such development, it is also necessary to perform manufacturing or experiments in a chamber that purifies the air using air with an extremely low dew point or an inert gas such as nitrogen obtained by vaporizing liquid nitrogen.

In addition, in the current manufacturing of organic EL displays (OLEDs), printing technologies such as inkjet technology are used to form a uniform thin film of liquid organic EL materials on a substrate to produce elements that improve production efficiency or performance. technology development. For the development of this manufacturing technology, the room is filled with inert gases such as nitrogen so that the surrounding environment of the manufacturing equipment has a low dew point such as 1 ppm or less of moisture and 1 ppm or less of oxygen and an inert gas concentration. However, when maintenance or adjustment of manufacturing equipment is performed indoors, it is necessary to return the low dew point inert gas environment to the atmospheric environment (hereinafter referred to as "atmosphere replacement").

At this time, if the inert gas environment is replaced with normal atmosphere, various components of the device located inside will absorb moisture. When returning to the inert gas environment again, the moisture adsorbed by the desorption components will be very time-consuming.

There is a technique described in Patent Document 1 as a technique for minimizing the amount of inert gas required to return to the inert gas environment from the atmospheric environment where the atmosphere is replaced and minimizing the downtime of the device. The internal volume of the enclosure members is minimized.

Patent Document 2 discloses a glove box equipped with an inert gas circulation purification device. Accordingly, in order to keep the inert gas atmosphere in the glove box constant and to effectively remove oxygen and moisture, a metal catalyst filling portion is filled with a metal catalyst that removes oxygen in the gas, and a metal catalyst filling portion is filled with a metal catalyst that adsorbs and removes the gas. The adsorption tower is composed of a desiccant filling part of molecular sieve (molecular sieve) and a desiccant filling part. It supplies circulating gas to remove oxygen and moisture, and uses a circulation pump to suck out the gas in the glove box and remove oxygen when passing through the adsorption tower. and moisture before returning to the glove box for gas circulation. [Prior technical literature] [Patent Document]

[Patent Document 1] Japanese Patent No. 6153539 [Patent Document 2] Japanese Patent No. 5676521 [Patent Document 3] Japanese Patent Publication No. 2019-52835

What is disclosed in Patent Document 1 is that by framing the gas enclosure and minimizing the internal volume, the downtime for maintenance and the like can be minimized with the smallest amount of inert gas in the gas enclosure, and can The work space is optimized to fit within the installation area of various OLED manufacturing equipment. However, as the device is stopped, the gas purification system that simultaneously performs inert gas purification and moisture removal is also stopped. Therefore, there is a problem that excessive time is spent to return the room to a low humidity and inert gas environment again. In addition, there is the following problem: the gas purification device and the dehumidification device are located in the same mechanism, and the purification speeds of oxygen and moisture are different. Removing moisture is very time-consuming compared with removing oxygen, so it is difficult to remove them at the same time.

In a conventional system such as Patent Document 2, oxygen removal and moisture removal are also performed using tandem columns, so the machine is selected with constant moisture removal capability. In this way, in the conventional technology, the recovery time until the atmosphere is replaced and returned to the inert gas environment becomes longer, and at the same time, it also takes time to start up the pipeline of the manufacturing equipment.

Therefore, as in Patent Document 3, a drying chamber for gas replacement is developed that uses a desiccant rotor to remove moisture and supply low dew point gas, thereby significantly shortening the time to reach a predetermined moisture concentration. Compared with the granular molecular sieve used for removing moisture in Patent Document 2, the advantages of using a desiccant rotor to remove moisture are as follows. That is, because it is honeycomb-shaped, the surface area is large and the pressure loss is low, and the walls of the honeycomb are very thin. The diffusion speed of adsorbed water is fast, so it is instantly adsorbed and desorbed throughout the honeycomb element.

In the gas replacement drying chamber of Patent Document 3, an airtight container is provided inside the drying chamber that circulates dry air from a dry air supply device, and an inert gas and a low dew point gas are supplied into the airtight container. Airtight containers store manufacturing equipment used for OLED manufacturing or research and development. In addition, the inert gas purification device and the low dew point gas supply device are arranged in series on the circulation path of the airtight container, and a circulation path is provided separately from the circulation path and controlled independently of each other. Therefore, the moisture removal can be adjusted independently. performance and oxygen removal performance. Furthermore, by circulating the circulation path provided separately in the atmosphere replacement, the recovery time of the airtight container from the atmospheric environment to the inert gas environment after the atmosphere replacement can be greatly shortened. Since the supply of low dew point gas can be maintained even when the supply of inert gas is stopped, the dew point in the airtight chamber quickly reaches a low state even after the atmosphere is replaced.

The present invention omits the drying chamber covering the airtight container described in Patent Document 3 and the dry air supply device for supplying and circulating dry air inside the drying chamber, and connects a low dew point gas purification device and an inert gas purification device. Compared with the gas replacement drying chamber of Patent Document 3, the integrated type is intended to simplify the device, save space, and simplify the operation method.

In order to solve the above problems, the present invention provides an airtight chamber that stores a manufacturing device used in the production or development of OLED, supplies a low dew point gas and an inert gas to the airtight chamber, and connects the inert gas purification device and the low dew point gas. The gas supply device is integrated, and a switching mechanism is provided as necessary so that the gas passing through the low dew point gas supply device passes through the bypass path and does not pass through the inert gas purification device. Therefore, people enter the airtight chamber during adjustments due to atmospheric replacement, etc. In the internal case, dry air can be supplied to the airtight chamber while the supply of inert gas to the airtight chamber can be divided to maintain a closed loop, thereby significantly shortening the downtime due to atmospheric replacement. Alternatively, the supply amount of dry air can be reduced by operating the low dew point gas supply device during atmospheric replacement without performing a closed loop cycle. Water molecules are polar substances. If the atmosphere is directly introduced into an airtight room that needs to be maintained at a low dew point, water molecules will adhere to the walls of the airtight room or inside the filter. In order to discharge the water molecules adhered in this way, it is necessary to supply low dew point air for a long time. However, in the case of the present invention, dry air is supplied in a state where the supply of inert gas is stopped. Therefore, even after the atmosphere is replaced, the air in the airtight chamber can be maintained. The dew point quickly reaches a lower state.

Furthermore, whether it is nitrogen entering the bottle as an inert gas, nitrogen gas produced by vaporizing liquefied nitrogen, or removing oxygen from the air through low-temperature separation, pressure swing adsorption (PSA: pressure swing adsorption), membrane separation, etc. Nitrogen is expensive. If the time for atmospheric replacement or the recovery time for returning to an inert gas environment after atmospheric replacement is not shortened, the cost will increase. On the other hand, the desiccant rotor is used to produce low dew point gas, and by maintaining the supply of low dew point gas while stopping the supply of inert gas for maintenance, etc., costs can be reduced.

The desiccant dehumidifier is used to remove moisture to greatly shorten the moisture removal time. At the same time, a part of the low dew point gas is introduced into the inert gas purification device to remove oxygen. Therefore, by adjusting the amount and introduction of the gas processed by the desiccant dehumidifier The amount of gas sent to the inert gas purification device can be used to create a drying chamber with an inert gas concentration under optimal operating conditions. [Effects of the invention]

The drying chamber for gas replacement of the present invention is configured as described above. Therefore, even during air replacement, the air is replaced by a high-efficiency particulate air (HEPA) filter or an ultra-low penetration air (ULPA) installed in the upper part of the container. Air purification filters such as Ultra Low Penetration Air filters supply dry air in one direction (hereinafter referred to as "one-way") without circulating it, thereby making it easier for the filter to retain moisture. This enables repairs or maintenance, configuration changes, etc. to be carried out. Furthermore, an inert gas purification device is connected and integrated after the desiccant dehumidifier, and a separately provided circulation path is circulated during atmospheric replacement, so that the circulating air does not come close to the atmospheric environment. By doing this, the recovery time from the atmospheric environment of the airtight chamber to a low dew point and inert gas environment can be significantly shortened. Furthermore, by adjusting the flow rate of the gas flowing from the dehumidification device to the inert gas purification device, it is possible to provide a drying chamber that can be easily optimized to a low dew point and inert gas environment in a short time.

Modes for implementing the present invention will be described below using the drawings. In addition, the present invention is not limited to the following examples.

In this embodiment, as a gas replacement dehumidification device and a gas replacement method of a container that requires low dew point and inert gas to keep the interior clean, it is used as a room for manufacturing or developing equipment for organic EL displays (OLED) using printing technology such as inkjet technology. Take an example to illustrate. In addition, the present invention is not limited to OLED manufacturing or R&D equipment. It can also be used for storage containers or closures such as glove boxes used in the development of lithium-ion battery materials or semiconductor fields that require a low dew point and inert gas environment to keep the storage space clean. space for use. [Example 1]

Hereinafter, Example 1 of the gas replacement drying chamber of the present invention will be described in detail based on FIG. 1 . Airtight chamber 1 uses low dew point and inert gas to keep the interior clean. The airtight room 1 can be a glove box or a drying room. The airtight chamber 1 stores manufacturing equipment 2 for OLED manufacturing or research and development. When cleanliness is required, the upper air supply part of the airtight chamber 1 is equipped with a high-efficiency particulate air filter or ultra-low penetration. Composition of air purifying filter 3 such as air filter. In addition, the air purification filter 3 may be provided as a plurality of fan filter units. Nitrogen gas or dry air as a utility is supplied to the airtight chamber 1 through the pipe a.

In the desiccant dehumidifier 16 , the honeycomb rotor 5 is divided into a processing area 6 , a purification area 7 , and a regeneration area 8 . The honeycomb rotor 5 can continuously adsorb and desorb moisture while rotating the rotor drive motor 9 such as a geared motor. The gas to be processed passes through the air blower 10 and is cooled by the precooler 11 and supplied to the processing area 6 of the honeycomb rotor 5 . A part of the gas to be processed is branched before the processing area 6 and passes through the purification area 7 . Then, it is heated by the regeneration heater 14 and sent to the regeneration area 8 . The gas passing through the regeneration area 8 is cooled by the cooler 15 , and the water condensed from the moisture in the regeneration gas desorbed from the honeycomb is removed as drainage water and returned to the front of the blower 10 . The gas to be processed passing through the honeycomb in the processing area 6 is heated by the post-heater 12 as needed, and is supplied to the airtight chamber 1 as supply air SA. In this embodiment, the honeycomb rotor 5 having the purification area 7 is used. However, the structure is not limited to this, and a honeycomb rotor divided into two areas: a processing area and a regeneration area may be used.

In the nitrogen purifier 23, the catalyst containers 18 and 19 for nitrogen purification contain a metal catalyst such as a copper catalyst or a platinum catalyst and are configured as twin towers. If the catalyst fails, the heaters 20 and 21 are used to increase the temperature while flowing nitrogen and hydrogen to regenerate the catalyst. In addition, in this embodiment, the catalyst is not limited to a copper catalyst or a platinum catalyst, and a catalyst mainly composed of copper and/or platinum or other metal catalysts used for the purpose of removing oxygen may be used. structure. In addition to the granular form, the metal catalyst can also be used in the form of granules, powders, or those loaded on a carrier. In this embodiment, the catalyst container is a double-tower type, but it is not limited to this, and it may be a single-tower type or a plurality of towers.

It can also be configured so that when there is still enough capacity in the nitrogen supply equipment, the desiccant dehumidifier and the nitrogen purifier are installed in an airtight room and nitrogen is supplied to the room, thereby suppressing the flow of nitrogen from the desiccant dehumidifier. 16 reactive gas intrusion.

With reference to the operation of the gas replacement drying chamber of the present invention configured as above, the atmosphere replacement for performing maintenance, installation change, adjustment, etc. of the airtight chamber 1 will be described.

(atmospheric replacement) By closing the valves 26, 29, and 30 and opening the valves 27 and 28, dry air from a dry air supply device (not shown) or the like is introduced from the upper part of the airtight chamber 1 through the pipe a, thereby replacing nitrogen with dry air. Since dry air with a low dew point is supplied in a unidirectional manner from the upper part of the airtight chamber 1, a large amount of air can be safely supplied at one time, so the replacement speed of nitrogen and air can be significantly shortened. By supplying dry air in a one-way manner from the upper part of the air purification filter 3 where moisture is most easily retained in the airtight chamber 1 without causing it to circulate inside the airtight chamber 1, even if people are working inside, moisture will not It will remain in the airtight chamber 1 and be discharged to the outside.

The following situations (1) and (2) exist in atmospheric replacement.

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

(2) Furthermore, as shown in FIG. 1 , when there is one airtight chamber, the airtight chamber 1 can also be dehumidified by the desiccant dehumidifier 16 during air replacement. In this case, valves 29, 30, 31 are opened and valves 33, 34 are closed. The return air RA from the airtight chamber 1 is mixed with the return air from the regeneration area 8 of the desiccant dehumidifier 16 through the pipe b, and is cooled by the precooler 11 via the air blower 10 and supplied to the honeycomb rotor 5 as the gas to be processed. In area 6. Then, a part of the gas to be processed is branched before the processing area 6 and passes through the purification area 7 . Then, it is heated by the regeneration heater 14 and sent to the regeneration area 8 . The low dew point gas passing through the processing area 6 is supplied as supply air SA into the airtight chamber 1 through the pipe c. In this way, by circulating operation, the low dew point environment of the airtight chamber 1 can be maintained, and the supply amount of dry air as a public facility can be reduced.

Next, the nitrogen replacement and circulation operation of the airtight chamber 1 will be described.

(Nitrogen replacement operation)

After the atmosphere is replaced, the inside of the airtight chamber 1 is replaced with nitrogen, and the oxygen concentration is set to a predetermined concentration such as 100 ppm or less. Depending on the conditions (1) and (2) of atmospheric replacement, the nitrogen replacement operation is as follows.

(1) First, the valve 27 is closed and the valve 26 is opened. Nitrogen gas from a nitrogen gas bottle, a nitrogen gas supply device (not shown), etc. is supplied to the airtight chamber 1 through the pipe a. The valve 28 is opened, and the return air RA from the airtight chamber 1 is exhausted (EA) through the pipe b. By configuring nitrogen to be supplied in one direction from the upper part of the airtight chamber 1, a large amount of gas can be supplied at once. Therefore, the air remaining in the airtight chamber can be quickly replaced with nitrogen, and the replacement speed of nitrogen and air can be greatly shortened. Continue until the oxygen concentration in the airtight chamber 1 decreases to 100 ppm.

(2) Perform the same operation as (1). The nitrogen gas supplied into the airtight chamber 1 is exhausted (EA) through the valve 28, but the remaining gas passes through the regeneration area 8 of the honeycomb rotor 5 and is mixed with the gas cooled by the cooler 15, and is introduced as the gas to be processed. into the treatment area 6 of the honeycomb rotor 5 . A part of the gas to be processed is branched before the processing area 6 and passes through the purification area 7 . Then, it is heated by the regeneration heater 14 and sent to the regeneration area 8 . In addition, at this time, the valve 31 is in an open state and the valves 33 and 34 are in a closed state, so active gases such as oxygen do not flow into the nitrogen purifier 23 . The gas to be processed passing through the honeycomb in the processing area 6 is heated by the post-heater 12 as needed, and is supplied as supply air SA into the airtight chamber 1 through the pipe c. In this way, nitrogen gas is supplied to replace the gas in the airtight chamber 1 and dehumidify the moisture remaining in the airtight chamber 1 after the atmospheric replacement, thereby slowly reducing the moisture concentration and oxygen concentration in the airtight chamber 1 . This cycle operation is performed until the oxygen concentration in the airtight chamber 1 becomes 100 ppm or less, and the inside of the airtight chamber 1 is replaced with nitrogen.

(Oxygen removal and nitrogen purification operation) After the oxygen concentration in the airtight chamber 1 drops to a predetermined 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 maintained in a closed state. Thereby, the gas passing through the purification area 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. Furthermore, by narrowing the valve 26, the supply flow rate of the nitrogen gas through the pipe a is reduced and the nitrogen gas is supplied, while maintaining the positive pressure in the airtight chamber 1. The return gas RA from the airtight chamber 1 is supplied to the honeycomb rotor 5 through the pipe b as the gas to be processed.

The flow of gas in the desiccant dehumidifier 16 is as described above. The gas passing through the purification area 7 is heated by the adsorption heat of the honeycomb. On the other hand, metal catalysts easily react with oxygen under higher temperature conditions, so it is better to supply high-temperature gas that passes through the purification area into the catalyst container. If the metal catalyst contains, for example, copper, copper reacts with oxygen and is oxidized according to the following formula, and becomes copper oxide, thereby removing oxygen. 2Cu+O ₂ →2CuO

The gas passing through the nitrogen purifier 23 is heated by the regeneration heater 14 and introduced into the regeneration area 8 of the honeycomb rotor 5 . The gas that has passed through the regeneration area 8 passes through the processing area 6 again and is supplied into the airtight chamber 1 as supply air SA. By performing the cyclic operation in this manner, the oxygen concentration and/or moisture concentration is gradually reduced. For example, the circulation operation is performed until the water concentration reaches a predetermined concentration of 10 ppm and the oxygen concentration reaches a predetermined concentration of 1 ppm or less. After that, the operation of the manufacturing device 2 is started, and experiments for manufacturing or developing OLEDs are started. In addition, in this embodiment, the gas flows in the catalyst container 18 . However, the gas may also flow in the catalyst container 19 . That is, two catalyst containers (double-tower type) are installed in parallel, and while the catalyst in one catalyst container is being regenerated, the other catalyst container is used to perform nitrogen purification processing. In addition, it is not limited to this, and may also be composed of one or a plurality of nitrogen purifiers composed of one or a plurality of catalyst containers.

In Embodiment 1, the gas passing through the purification area is sent to the nitrogen purifier, but the gas passing through the treatment area or the gas passing through the purification area and the gas passing through the treatment area may be mixed and supplied. Alternatively, a structure may be adopted in which a utility supplying nitrogen gas used in nitrogen replacement is connected to a nitrogen purifier to supply nitrogen gas to the airtight chamber. In addition, the low dew point gas dehumidified by the honeycomb rotor circulates in the catalyst container, so moisture is difficult to retain.

(catalyst regeneration operation)

When the catalyst fails and the gas passing through the catalyst container exceeds a predetermined concentration such as oxygen concentration 1 ppm, the catalyst regeneration operation is started. For example, when the catalyst in the catalyst container 18 fails, the valves 35 and 36 are closed and the valves 37 and 38 are opened so that the gas passing through the purification area 7 flows into the catalyst container 19 . Next, the valves 39, 40, 43, and 44 are opened, and nitrogen gas containing hydrogen gas adjusted to a predetermined concentration is supplied to the catalyst container 18 from a nitrogen gas supply device containing hydrogen gas or a nitrogen gas supply device (not shown) or the like. middle. At the same time, the heater 20 is used for heating. For example, when the metal catalyst contains copper, as shown in the following formula, copper oxide reacts with hydrogen and is reduced, and oxygen is removed by converting it into copper, the catalyst is regenerated, and the vacuum pump 22 performs vacuum extraction and discharge. Air (EA).

CuO+H ₂ →Cu+H ₂ O

In addition, by opening the valve 46, the water reacted and discharged is discharged as drainage water.

With the above structure, a space-saving gas replacement system can be set up, and production costs incurred in piping and installation work can be suppressed.

[Example 2]

FIG. 2 shows a flow path diagram in Example 2 of the drying chamber of the present invention. In Example 1, one airtight chamber is used, but in Example 2, a plurality of airtight chambers are used. In addition, in FIG. 2 , the structure is configured to include three airtight chambers 1A, 1B, and 1C. However, the structure is not limited to this, and two or four or more airtight chambers may be provided. The device structure of Embodiment 2 is almost the same as that of Embodiment 1, so repeated description is omitted.

When there are a plurality of airtight chambers, even if a part of the airtight chamber is being replaced by the atmosphere, inert gas can be circulated in another airtight chamber to maintain oxygen removal. Nitrogen purification operation. Therefore, the recovery time from the atmospheric environment after atmospheric replacement to an environment with a low dew point and an inert gas concentration can be significantly shortened. In addition, one desiccant dehumidifier and nitrogen purifier can be used to supply gas to each airtight chamber, so costs can be suppressed. The system of the present invention has the following characteristics, that is, the larger the pipeline scale, the greater the cost advantage.

In addition, in Example 2, one desiccant dehumidifier and a nitrogen purifier are used to supply the inert gas. However, a plurality of desiccant dehumidifiers and/or nitrogen purifiers may be used to supply the inert gas to the airtight chamber.

In the following description of Example 2, the airtight chamber 1A is set to perform atmospheric replacement from the inert gas environment, and then return from the atmospheric environment to a low dew point after the atmospheric replacement. , inert gas environment and perform oxygen removal and nitrogen purification operations. During this period, the airtight chambers 1B and 1C are set to continue oxygen removal and nitrogen purification operations.

(atmospheric replacement)

The case where the airtight chamber 1A returns to the atmospheric environment by atmospheric replacement will be described. By closing the valves 26, 47B, 47C, 48A, and 51A and opening the valves 27, 47A, and 50A, dry air is introduced from the upper part of the airtight chamber 1A through the pipe a, thereby replacing the nitrogen gas with the dry air. Since dry air with a low dew point is supplied in a unidirectional manner from the upper part of the airtight chamber 1A, a large amount of air can be safely supplied at once, and therefore the replacement speed of nitrogen and air can be significantly shortened. In addition, in all the airtight chambers, when the atmosphere is replaced, by closing all the valves 48 and opening the valve 49, the desiccant dehumidifier and the nitrogen purifier are circulated independently of the airtight chamber, thereby maintaining inertness. gas, so the recovery time from atmospheric replacement to inert gas circulation operation becomes shorter.

(Nitrogen replacement operation) After the atmosphere is replaced, the inside of the airtight chamber 1A is replaced with nitrogen, and the oxygen concentration is set 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 into the airtight chamber 1A through the pipe a. When nitrogen gas is supplied to each airtight chamber through the pipe a, the flow rate of the supplied gas can be adjusted by the flow meter 24 and the valve 47 respectively. The return air RA from the airtight chamber opens the valve 50A and is discharged. In this way, the nitrogen replacement operation is performed in a one-way manner until the oxygen concentration in the airtight chamber 1 becomes a predetermined concentration or less, and the interior of the airtight chamber 1 is replaced with nitrogen. On the other hand, in the airtight chambers 1B and 1C, during the oxygen removal and nitrogen purification operation, the valves 50B and 50C are in the closed state and the valves 51B and 51C are in the open state. Therefore, the return air RA passes through the pipe b and the inert gas is introduced to the desiccant dehumidification. Machine 16 hits. Among them, the valve 48A is in a closed state, so oxygen flows into the desiccant dehumidifier 16 and the nitrogen purifier 23 without causing any influence. Furthermore, the flow rate can be adjusted by opening the valve 49 and performing a bypass operation through the pipe d.

The return gas RA from the airtight chambers 1B and 1C is mixed with the inert gas in the bypass operation through the pipe d, and then the gas passing through the regeneration area 8 of the honeycomb rotor 5 is mixed, and is introduced into the processing area 6 of the honeycomb rotor 5 as the gas to be processed. middle. Among them, the valve 31 is in a closed state, and similarly to Embodiment 1, the gas passing through the purification area 7 is introduced into the nitrogen purifier 23 to perform oxygen removal and nitrogen purification operations.

In addition, when all the airtight chambers are replaced with nitrogen from the atmosphere, the valve 31 is opened and the valves 33 and 34 are closed so that the active gas does not flow into the nitrogen purifier 23, and the same configuration as in Example 1 is performed. Works the same way.

(Oxygen removal, nitrogen purification operation) After the oxygen concentration in the airtight chamber 1A drops below a predetermined concentration, the valve 50A is closed and the valve 51A is opened. Then, the valve 26 is narrowed to reduce the supply flow rate of the nitrogen gas through the pipe a, thereby supplying the nitrogen gas while maintaining the positive pressure in the airtight chamber 1 . The return gas RA from the airtight chamber 1 is supplied to the honeycomb rotor 5 through the pipe b as the gas to be processed. The gas passing through the purification area 7 of the honeycomb rotor 5 is introduced into the nitrogen purifier 23 through the air blower 17 . The inert gas passing through the nitrogen purifier 23 is heated by the regeneration heater 14 and introduced into the regeneration area 8 of the honeycomb rotor 5 . The gas that has passed through the regeneration area 8 passes through the processing area 6 again and is supplied into the airtight chamber 1 as supply air SA. By performing the cyclic operation in this manner, the oxygen concentration and/or the moisture concentration are further gradually reduced. After reaching the predetermined concentration, the operation of the manufacturing device 2 is started, and experiments for manufacturing or developing OLEDs are started. In addition, in FIG. 2 , the catalyst container is a double tower type, but like Example 1, it is not limited to this.

By connecting a desiccant dehumidifier and a nitrogen purifier to form an integrated device, compared to Patent Document 3, a space-saving gas replacement system can be set up, and production costs such as piping and installation work can be suppressed. .

By the above, the recovery time until the atmospheric environment of the airtight chamber 1 is returned to an environment where the inside is cleaned with low dew point and inert gas can be shortened to 1/5 to 1/10 of the conventional technology. Furthermore, a gas replacement system can be realized in which the inside of the airtight chamber 1 can be easily optimized to a low dew point and inert gas environment. [Industrial availability]

The present invention can also be used in storage containers such as glove boxes or drying rooms for developing lithium-ion battery materials that require low dew point and inert gas concentration to keep the storage space clean.

1,1A,1B,1C: Airtight room 2,2A,2B,2C: Manufacturing equipment 3,3A,3B,3C: Air purification filter 4: Gas circulation path 5: Honeycomb rotor 6: Processing area 7:Purification area 8: Regeneration area 9: Rotor drive motor 10,17: Blower 11: Precooler 12:Rear heater 13:Air filter 14: Regenerative heater 15:Cooler 16: Desiccant dehumidifier 18,19:Catalyst container 20,21: heater 22:Pump 23:Nitrogen purifier 24,24A,24B,24C,25,25A,25B,25C: flow meter 26,27,28,29,30,31,32,33,34,35,36,37,38,39,40,41,42,43,44,45,46,47,47A,47B,47C, 48,48A,48B,48C,49,50,50A,50B,50C,51,51A,51B,51C: valve a:Piping b:Piping c:Piping d:Piping

Figure 1 is a flow path diagram in Embodiment 1 of the drying chamber of the present invention. Figure 2 is a flow path diagram in Example 2 of the drying chamber of the present invention.

1: Airtight room

2: Manufacturing device

3: Air purification filter

4: Gas circulation path

5: Honeycomb rotor

6: Processing area

7:Purification area

8: Regeneration area

9: Rotor drive motor

10: Blower

11: Precooler

12:Rear heater

13:Air filter

14: Regenerative heater

15:Cooler

16: Desiccant dehumidifier

17: Blower

18:Catalyst container

19:Catalyst container

20:Heater

21:Heater

22:Pump

23:Nitrogen purifier

24:Flow meter

25:Flowmeter

26,27,28,29,30,31,32,33,34,35,36,37,38,39,40,41,42,43,44,45,46: valve

a:Piping

b:Piping

c:Piping

RA: Be angry

SA: air supply

Claims (6)

A drying chamber for gas replacement, characterized in that an airtight chamber connected to a pipe for supplying dry air and/or an inert gas is provided, and a nitrogen gas as an inert gas purification device is connected after a desiccant dehumidifier as a low dew point gas supply device. The purifier is formed into an integrated type. During the operation of oxygen removal and nitrogen purification, the gas passing through the desiccant dehumidifier passes through the nitrogen purifier. The desiccant dehumidifier is configured to have at least a processing area and a regeneration area, and will pass through the nitrogen. The gas of the purifier is introduced into the regeneration area, and the gas passing through the regeneration area is introduced into the processing area. The airtight chamber is set up to supply the low dew point gas passing through the processing area through a filter that removes foreign matter. The gas is replaced by drying The chamber includes a pipeline for mixing the return gas from the airtight chamber with the gas passing through the regeneration zone and recirculating it to the processing zone. The drying chamber for gas replacement as described in item 1 of the patent scope, wherein a pipeline is provided to connect the gas passing through the desiccant dehumidifier to the nitrogen purifier and the gas passing through the nitrogen purifier is sent to the In the bypass line of the pipeline in the regeneration area, valves are provided in each pipeline. By opening and closing these valves, the gas passing through the desiccant dehumidifier is bypassed during the atmospheric replacement and/or nitrogen replacement operation. The nitrogen purifier. The drying chamber for gas replacement described in item 1 of the patent application, wherein the airtight chamber is composed of one or a plurality of airtight chambers. The drying room for gas replacement as described in item 1 of the patent application, wherein the filter for removing foreign matter is a fan with a built-in high-efficiency particulate air (HEPA) filter and/or an ultra-low penetration air (ULPA) filter. filter. For example, the drying chamber for gas replacement described in item 1 of the patent application, wherein the nitrogen purifier is a nitrogen purifier with a built-in catalyst containing copper and/or platinum as the main component. The drying room for gas replacement as described in item 1 of the patent application, wherein a purification area is further provided between the processing area and the regeneration area of the desiccant dehumidifier, and the purification area passes through the purification area. The nitrogen gas is supplied to the nitrogen purifier.

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