JP2009254935A - Gas dissolving membrane device and method of manufacturing gas-dissolved solution - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a gas dissolving membrane device which can be stably operated continuously for a long time and a method of manufacturing a gas-dissolved solution. <P>SOLUTION: A first valve 31 is opened during operation of manufacturing a gas-dissolved water, and a condensate water obtained by condensing process in a gas phase chamber 13 is stored in a reservoir 34 passing through a first valve 31 (a process for reserving condensate water). Next, when the amount of the condensate water measured by a condensate water detection means 35 exceeds a predetermined value, the first valve 31 is closed, and a second valve 32, a third valve 33 and a valve 42 are opened. Further, a sweep gas is supplied to upstream of the reservoir 34 through piping 41, and the condensate water is drained from an outflow part of the reservoir 34 (a process for draining condensate water). After that, the valve 42 and the third valve 33 are closed and a valve 53 is opened by actuating an exhaust device 52, and then the interior of the reservoir 34 is evacuated until the readings of a manometer 54 are equal to the pressure levels measured by the manometer 54 (a process for adjusting pressure). Then, the operation returns to the process of reserving condensate water. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a gas-dissolving membrane device and a method for producing a gas-dissolving solution. Specifically, the gas-dissolving membrane module includes a gas-permeable membrane module that is partitioned into a liquid phase chamber and a gas phase chamber by a gas-permeable membrane. Water is supplied to the chamber, gas is supplied to the gas phase chamber, and the gas in the gas phase chamber is dissolved in the water in the liquid phase chamber via the gas permeable membrane to produce gas-dissolved water The present invention relates to a gas dissolution membrane device and a method for producing a gas solution.

  Conventionally, cleaning of a silicon substrate for a semiconductor, a glass substrate for a liquid crystal, etc., mainly includes a mixed solution of hydrogen peroxide solution and sulfuric acid, a mixed solution of hydrogen peroxide solution, hydrochloric acid and water, hydrogen peroxide solution, ammonia solution and water. This is performed by a so-called RCA cleaning method in which a concentrated chemical solution based on hydrogen peroxide, such as a mixed solution, is washed at a high temperature and then rinsed with ultrapure water. However, this RCA cleaning method uses a large amount of hydrogen peroxide water, high-concentration acid, alkali, etc., so the cost of the chemical solution is high. In addition, the cost of rinsing ultrapure water, the cost of waste liquid treatment, and chemical vapor are exhausted. However, a large cost is required, such as an air conditioning cost for newly preparing clean air.

  On the other hand, various efforts have been made to reduce costs in the cleaning process and reduce the burden on the environment. A typical example is a technique for cleaning an object to be processed by ultrasonic cleaning or the like using gas-dissolved water in which a specific gas is dissolved. As this specific gas, oxygen gas, ozone, carbon dioxide gas, rare gas, inert gas, hydrogen gas, or the like is used.

  As a method for producing such gas-dissolved water, a method using a membrane module incorporating a gas-permeable membrane is known. In this method, water is supplied to the liquid phase side of the gas permeable membrane, a specific gas is supplied to the gas phase side, and the gas on the gas phase side is dissolved in the water on the liquid phase side through the gas permeable membrane. Manufacturing gas-dissolved water.

  For example, Japanese Patent Application Laid-Open No. 11-077023 describes that after degassing ultrapure water to lower the saturation of dissolved gas, hydrogen gas is dissolved in this ultrapure water.

  FIG. 4 is a process flow diagram of the publication. The ultrapure water is sent to the deaeration membrane module 2 via the flow meter 1. In the degassing membrane module 2, the gas phase in contact with the ultrapure water through the gas permeable membrane is kept in a reduced pressure state by the vacuum pump 3, and the gas dissolved in the ultrapure water is degassed. The ultrapure water from which the dissolved gas has been degassed is then sent to the hydrogen gas dissolving membrane module 4. In the hydrogen gas dissolving membrane module 4, the hydrogen gas supplied from the hydrogen gas supplier 5 is sent to the gas phase side and supplied to ultrapure water through the gas permeable membrane. A chemical solution such as ammonia water is added from the chemical solution storage tank 6 to the ultrapure water in which the dissolved hydrogen gas concentration has reached a predetermined value by the chemical injection pump 7 and adjusted to a predetermined pH value. The hydrogen-containing ultrapure water that has become alkaline due to the dissolution of hydrogen gas is finally sent to the microfiltration device 8 and fine particles are removed by an MF filter or the like.

The dissolved gas measurement sensors 9 installed at the inlet and outlet of the degassing membrane module 2 measure the amount of gas in the ultrapure water to determine the saturation, and send a signal to the vacuum pump to determine the saturation and the desired purity of the ultrapure water. The amount of deaeration is adjusted by comparing with the degree of saturation. The deaeration amount is adjusted, for example, by adjusting the degree of vacuum by the vacuum pump by adjusting the degree of opening of the vacuum degree adjusting valve. The gas saturation of the ultrapure water after deaeration is measured by the dissolved gas measuring sensor 9, and the hydrogen gas concentration in the hydrogen-containing ultrapure water flowing out from the hydrogen gas dissolving membrane module is measured by the dissolved hydrogen measuring sensor 9A. These measurement signals are sent to the hydrogen gas supply device, and the supply amount of the hydrogen gas is controlled by adjusting, for example, the opening degree of a valve provided in the hydrogen gas supply path.
JP-A-11-077023

  In the above-mentioned Japanese Patent Application Laid-Open No. 11-077023, the gas permeable membrane of the hydrogen gas dissolving membrane module 4 has a characteristic of transmitting only gas and not transmitting liquid, but transmits water vapor. For this reason, water vapor diffuses from the liquid phase chamber to the gas phase chamber through the gas permeable membrane. Thus, the water vapor that has passed through the gas permeable membrane from the liquid phase chamber to the gas phase chamber is condensed in the gas phase chamber to become condensed water, and is accumulated in the gas phase chamber.

  When the amount of the condensed water is small, the influence on the performance of the hydrogen gas dissolving membrane module 4 is slight. However, when the amount of condensed water is large, the gas permeable membrane covered with the condensed water is on the gas phase chamber side. As a result, the effective area of the gas permeable membrane contributing to gas permeation decreases. Thereby, the performance of the hydrogen gas-dissolving membrane module 4 is lowered, and the hydrogen gas cannot be sufficiently dissolved in the ultrapure water.

  For this reason, when condensed water accumulates in the gas phase chamber of the hydrogen gas dissolving membrane module 4, it is necessary to stop the operation and discharge the condensed water from the gas phase chamber.

  As a method of discharging the condensed water accumulated in the gas phase chamber of the hydrogen gas dissolving membrane module during operation, an exhaust device such as a vacuum pump is connected to the gas phase chamber, and when the condensed water accumulates in the gas phase chamber. It is conceivable that the condensed water is sucked and discharged by the vacuum pump. However, when liquid water is sucked into the vacuum pump, the pump drive section is significantly deteriorated, causing problems such as a reduction in suction performance and an increase in failure. As a result, it is necessary to stop the operation and perform maintenance or replacement of the pump. In addition, when the condensed water in the gas phase chamber is sucked with a vacuum pump or the like, the pressure in the gas phase chamber decreases, so the amount of gas supplied from the gas phase chamber to the ultrapure water in the liquid phase chamber through the gas permeable membrane Decreases and the gas concentration of the gas-dissolved water decreases.

  An object of the present invention is to solve the above-mentioned problems and to provide a gas-dissolving membrane device and a method for producing a gas-dissolving solution that can be operated continuously and stably for a long period of time.

  The apparatus for producing gas-dissolved water of the present invention (Claim 1) is for discharging a gas-dissolved membrane module partitioned into a gas phase chamber and a liquid phase chamber by a gas permeable membrane, and condensed water condensed in the gas phase chamber. In the gas dissolution membrane device having the condensate discharge device, the condensate discharge device includes a storage portion into which the condensed water discharged from the gas phase chamber flows and a discharge portion having a water outflow portion from the storage portion. A first valve that communicates and shuts off the passage, the gas phase chamber and the reservoir, and supplies pressurized gas into the reservoir with the first valve closed to condense in the reservoir And a gas supply means for discharging water from the outflow portion.

  The gas dissolution membrane device according to claim 2 is the gas dissolution membrane device according to claim 1, wherein a second valve is provided in the outflow portion, and the first valve and the second valve are closed in the storage portion. It has a pressure adjusting means for adjusting the pressure.

  According to a third aspect of the present invention, there is provided the gas-dissolving membrane device according to the second aspect, wherein the pressure adjusting means includes an exhaust device that sucks and exhausts the gas in the exhaust passage.

  A method for producing a gas solution according to the present invention (Claim 4) is a method for producing a gas solution using the gas dissolution membrane device according to any one of Claims 1 to 3, wherein the gas solution is provided in the liquid phase chamber. A gas solution for passing a liquid and supplying a gas to the gas phase chamber, and allowing the gas in the gas phase chamber to pass through the gas permeable membrane and dissolve in the liquid in the liquid phase chamber to obtain a gas solution. During the execution of the manufacturing operation, the first valve is opened, the condensed water storage step for receiving the condensed water condensed in the gas phase chamber into the storage section, the first valve is closed and the gas is closed. A pressurized gas is supplied from the supply means into the storage section, and a condensed water discharge step for discharging condensed water in the storage section from the outflow section is sequentially performed.

  According to a fifth aspect of the present invention, there is provided the method for producing a gas solution according to the fourth aspect, wherein the condensate drainage device is the condensate drainage device according to the second or third aspect. A condensed water storage step of opening the valve and closing the second valve to receive condensed water condensed in the gas phase chamber into the storage unit; and closing the first valve and the second valve; A condensate discharge step of supplying pressurized gas from the gas supply means into the reservoir and discharging condensed water in the reservoir from the outflow portion, the first valve and the first valve A pressure adjusting step of sequentially opening the first valve after closing the valve 2 and adjusting the pressure in the reservoir to be the same as the pressure in the gas phase chamber by the pressure adjusting means. It is characterized by that.

  In the gas-dissolving membrane device of the present invention (Claims 1 to 3) and the method for producing a gas-dissolving liquid (Claims 4 and 5), the condensed water condensed in the gas phase chamber is opened. Is received in the storage unit, it is prevented that the condensed water accumulates in the gas phase chamber during the manufacturing operation of the gas solution and the manufacturing efficiency decreases. Further, when condensed water accumulates in the reservoir, the first valve is closed and pressurized gas is supplied from the gas supply means into the reservoir, thereby discharging the condensed water in the reservoir from the outflow portion. Can be made. At this time, since the first valve is closed, the pressure in the gas phase chamber does not change, and the production of the gas solution is stably continued. In the present invention, since the gas supply means is used for discharging the condensed water in the storage portion as described above and no vacuum pump is used, the deterioration of the pump driving portion due to the condensed water being sucked into the vacuum pump, and the suction performance There will be no problems such as a decrease or an increase in failure.

  As described in claim 2, the second valve is provided in the outflow portion, and has pressure adjusting means for adjusting the pressure in the storage portion in a state in which the first valve and the second valve are closed. Also good.

  In this case, as in claim 5, the first valve is opened and the second valve is closed, and the condensed water storage step for receiving the condensed water condensed in the gas phase chamber in the storage portion; A condensed water discharge step of closing the valve and opening the second valve, supplying pressurized gas from the gas supply means into the storage section, and discharging condensed water in the storage section from the outflow section; The first valve and the second valve are closed, and the pressure in the reservoir is adjusted by the pressure adjusting means to be the same as the pressure in the gas phase chamber, and then the first valve is opened. It is preferable to sequentially perform the adjustment step. Since the second valve and the third valve are closed in the condensate storage step, it is possible to prevent gas and impurities from flowing back to the storage unit from outside the system. Since the pressure in the storage section is made the same as the pressure in the gas phase chamber in the pressure adjustment process and then returned to the condensed water storage process, the gas in the storage section flows back into the gas phase chamber or the pressure in the gas phase chamber fluctuates at the time of return. The production of the gas solution is stably continued. Since the condensed water in the reservoir is discharged from the reservoir in the condensed water discharge process, the pressure regulator does not suck in the condensed water in the subsequent pressure adjustment process, and the pressure regulator is deteriorated due to the suction of the condensed water. No problems such as performance degradation or failure occur.

  Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 to FIG. 3 are system diagrams for explaining a gas dissolution membrane device and a method for producing a gas solution according to the embodiment. FIG. 1 is a system diagram illustrating a condensed water storage process, FIG. 2 is a system diagram illustrating a condensed water discharge process, and FIG. 3 is a system diagram illustrating a pressure adjustment process.

  In this embodiment, gas dissolved water is generated by the gas permeable membrane module 10, and condensed water in the gas phase chamber 13 of the gas permeable membrane module 10 is discharged by the condensed water discharge device 60.

  The gas dissolution membrane module 10 is partitioned into a liquid phase chamber 12 and a gas phase chamber 13 by a gas permeable membrane 11.

  The gas permeable membrane 10 is not particularly limited as long as it does not permeate water and permeates gas dissolved in water. For example, polypropylene, polydimethylsiloxane, polycarbonate-polydimethylsiloxane block copolymer, Examples thereof include a polymer film such as polyvinylphenol-polydimethylsiloxane-polysulfone block copolymer, poly (4-methylpentene-1), poly (2,6-dimethylphenylene oxide), and polytetrafluoroethylene.

  A raw water pipe 21 provided with an on-off valve 21 a is connected to the liquid phase chamber 12 of the gas dissolution membrane module 10. Further, a pipe 23 for extracting dissolved gas water is connected to the liquid phase chamber 12.

  The raw water supplied to the raw water pipe 21 is not particularly limited as long as it has a cleanliness that satisfies the application used at the point of use and does not contain substances that extremely deteriorate or alter the gas permeable membrane. Water, pure water, ultrapure water, etc. are used. Moreover, you may use the deaerated water deaerated by the deaeration membrane module 2 of FIG.

  A gas supply pipe 22 having a flow rate adjusting valve 22 a is connected to the gas phase chamber 13 of the gas dissolving membrane module 10.

  Examples of the specific gas supplied to the gas supply pipe 22 include hydrogen, oxygen, carbon dioxide, ozone, a rare gas such as argon and helium, an inert gas such as nitrogen, and a mixed gas of two or more of these gases. Is used.

  A condensed water discharge device 60 is connected to the gas phase chamber 13. Next, the condensed water discharge device 60 will be described.

  A tubular discharge passage 30 is connected to the gas phase chamber 13. One end of the discharge path 30 is connected to the gas phase chamber 13, and has a horizontal portion 30 a that extends horizontally and a hanging portion 30 b that hangs down from the other end of the horizontal portion. A first valve 31, a second valve 32, and a third valve 33 are provided on the hanging portion 30b in this order from the upper side to the lower side. A portion of the discharge path 30 between the first valve 31 and the second valve 32 is a storage portion 34, and a lower end side of the storage portion 34 is an outflow portion 34a. Condensed water detection means 35 is provided in the storage part 34.

  Although there is no restriction | limiting in the internal diameter of this discharge path 30, since it is difficult for condensed water to flow when an internal diameter is too small, it is preferable that an internal diameter is 3.96-25.4 mm, especially 6-23 mm.

  As the condensed water detection means 35, for example, a liquid level meter that detects the liquid level of the condensed water accumulated in the storage unit 34, a weight meter that measures the weight of the accumulated condensed water, or the like is used. Among these, since the structure is simple and accurate detection is possible, it is preferable to use a liquid level gauge. As the liquid level gauge, a liquid level gauge using light, ultrasonic waves, capacitance, or the like can be used.

  A gas supply pipe 41 for supplying sweep gas to the reservoir 34 is connected to the upper side of the reservoir 34. A valve 42 is provided in the gas supply pipe 41.

  Examples of the sweep gas include the same as the supply gas. For example, hydrogen gas, oxygen gas, carbon dioxide gas, ozone, rare gas such as argon or helium, inert gas such as nitrogen, etc. are exemplified.

  An exhaust pipe 51 including an exhaust device 52 for discharging the gas in the storage section 34 is connected to a position between the second valve 32 and the third valve 33 in the discharge path 30. The exhaust pipe 51 is provided with a valve 53 and a pressure gauge 54.

  As the exhaust device 52, an exhaust device having an ability to depressurize the inside of the storage section 34 to 15 kPa or less, particularly 10 kPa or less is suitably used. Examples of the exhaust device include a vacuum pump and an aspirator. When a vacuum pump is used, an oilless type is preferably used in order to prevent contamination on the vacuum side.

  A pressure gauge 36 is provided in the discharge passage 30 at a position closer to the gas phase chamber 13 than the first valve 31.

  Although not shown, the condensed water discharge device 60 has a control circuit. This control circuit receives a signal from the condensed water detection means 35, and controls opening and closing of the first valve 31, the second valve 32, the third valve 33, the valve 42 and the valve 53 based on the received signal. It is configured to be able to do. The control circuit receives signals from the pressure gauge 36 and the pressure gauge 54, and controls the operation of the exhaust device 52 and / or the opening degree of the valve 53 so that these pressures have the same value or approximate values. It is configured to be able to do.

  The valves (the first valve 31, the second valve 32, the third valve 33, the valve 42, and the valve 53) used in the condensed water discharge device 60 are oil-free to prevent contamination on the vacuum side. Is preferred.

  Next, an example of a method for producing gas-dissolved water using the gas-dissolving membrane device configured as described above will be described.

  In this example, the raw water is circulated in the liquid phase chamber 12 of the gas dissolving membrane module 10 and the gas is supplied to the gas phase chamber 13 to produce the gas dissolved water. The condensed water discharge device 60 is operated and discharged.

  Therefore, first, the process of producing the gas-dissolved water will be described, and then the operation process (condensate storage process, condensate discharge process, and pressure adjustment process) of the condensate discharge device 60 executed in the manufacture process will be described.

[Production operation of dissolved gas water]
The valves 21a and 22a are opened. Note that at least the first valve 31 (preferably all valves) of the condensed water discharge device 60 is closed.

  Thereby, raw water is supplied to the liquid phase chamber 12 of the gas dissolution membrane module 10 via the raw water pipe 21. Further, gas is supplied into the gas phase chamber 13 via the gas supply pipe 22. The gas supplied into the gas phase chamber 13 passes through the gas permeable membrane 11 and dissolves in the raw water in the liquid phase chamber 12. The gas dissolved water thus obtained is supplied to the use point via the gas dissolved water pipe 23.

  The pressure in the gas phase chamber 13 is determined by the dissolved gas concentration, but in the case of hydrogen, it is preferably about 60 to 100 kPa.

  In the process of producing the gas-dissolved water in this way, water vapor permeates through the gas permeable membrane 11 from the liquid phase chamber 12 and gradually diffuses into the gas phase chamber 13, and is condensed in the gas phase chamber 13 to become condensed water. . The condensed water in the gas phase chamber 13 is discharged as follows using the condensed water discharge device 60 described above.

[Condensate storage process (Fig. 1)]
During execution of the gas dissolved water production operation, the first valve 31 is opened while the second valve 32, the third valve 33, the valve 42, and the valve 53 of the condensed water discharge device 60 are closed. Valve (FIG. 1).

  Thereby, the condensed water condensed in the gas phase chamber 13 is stored in the storage unit 34 through the discharge path 30 and the first valve 31. The amount of condensed water stored in the storage unit 34 is measured by the condensed water detection means 35.

  Since the second valve 32 and the third valve 33 are closed when condensate is stored in the storage unit 34, gas and impurities are discharged from the outside of the system through the discharge passage 30, the third valve 33, and the second valve. Inflow into the storage part 34 through the valve 32 is prevented.

[Condensate draining process (Fig. 2)]
When the amount of condensed water measured by the condensed water detection means 35 exceeds a predetermined value, the first valve 31 is closed and the second valve 32, the third valve 33, and the valve 42 are opened (second valve). Figure).

  As a result, the sweep gas is supplied to the upper side in the storage portion 34 via the pipe 41. Condensed water in the storage unit 34 is pressed by the sweep gas and discharged from the outflow part 34a of the storage unit 34, and further discharged out of the system of the condensed water discharge device 60 through the discharge path 30.

  Thus, although the inside of the storage part 34 is pressurized by the supply of the sweep gas, the first valve 31 is closed, so that the sweep gas is introduced into the gas phase chamber 13 upstream of the first valve 31. Does not flow in or the pressure in the gas phase chamber 13 does not increase. For this reason, manufacture of gas dissolution water is continued stably.

  The closing of the first valve 31 and the opening of the valve 42 may be performed at the same time, but the first valve 31 is closed in order to reliably prevent the reverse flow of the sweep gas to the gas phase chamber 13. After that, the valve 42 may be opened.

  Further, the second valve 32 and the third valve 33 may be opened before, simultaneously with, or after the valve 42 is opened. First, the valve 42 is opened and the storage unit 34 is opened. It is preferable to pressurize the inside and then open the second valve 32 and the third valve 33. When the second valve 32 and the third valve 33 are opened after pressurizing the inside of the storage portion 34 in this way, air and foreign matters outside the system are discharged from the discharge passage 30, the third valve 33, and the second valve. Backflow into the reservoir 34 through 32 is prevented. In order to prevent this backflow, it is preferable to open the second valve 32 and the third valve 33 after setting the pressure in the reservoir 34 to 0.05 PMa or more.

  The second valve 32 and the third valve 33 may be opened simultaneously, or one of them may be opened first.

  In order to promote the discharge of the condensed water, the valve 42 may be opened and closed with the second valve 32 and the third valve 33 opened. Further, the valve 42 may be opened and closed while the second valve 32 and the third valve 33 are alternately opened. Further, the condensed water storage process, the condensed water discharge process, and the pressure adjustment process described later may be repeated to promote the discharge of the condensed water.

[Pressure adjustment process (Fig. 3)]
In the condensate discharge process, the downstream side of the first valve 31 is pressurized by the sweep gas, and therefore the first valve 31 is opened in this state and the process returns to the condensate storage process. The sweep gas may flow into the gas phase chamber 13 through the first valve 31. In order to prevent this, the following pressure adjustment process is performed.

  After performing the condensed water discharge step, the valve 42 and the third valve 33 are closed. Further, the exhaust device 52 is operated to open the valve 53 (FIG. 3).

  As a result, the gas in the portion downstream of the first valve 31 in the discharge passage 30 (the portion between the first valve 31 and the third valve 33) is exhausted, and the pressure decreases. In the exhaust by the exhaust device 52, the pressure in the portion downstream of the first valve 31 in the discharge passage 30 (pressure measured by the pressure gauge 54) is the pressure in the upstream portion (measured by the pressure gauge 54). Until the pressure becomes the same value or approximate value.

  The pressure may be adjusted by using a pressure adjusting valve as the valve 53 and adjusting the opening degree of the valve 53. As this pressure regulating valve, a type having a built-in pressure sensor may be used. In this case, the pressure gauge 54 can be omitted.

  Further, the pressure may be adjusted by adjusting the amount of bleed of the exhaust device 52. For example, when the exhaust device 52 is a vacuum pump, the frequency may be controlled, and when the exhaust device 52 is an aspirator, the pressure and flow rate of the driving fluid may be controlled.

  In this way, after the pressure in the downstream portion of the discharge passage 30 from the first valve 31 becomes the same as the pressure in the upstream portion, the valve 53 is closed and the exhaust device 52 is stopped. . In addition, the second valve 32 is closed and the first valve 31 is opened. Thereby, it returns to a condensed water storage process (FIG. 1).

  These three steps (condensed water storage step, condensed water discharge step, and pressure adjustment step) may be repeated until the amount of condensed water detected by the condensed water detection means 35 becomes a predetermined amount or less. Further, a timer and a counter may be provided in the condensed water discharge device 60, and these three steps may be repeated a predetermined number of times every predetermined time.

  Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples.

[Example 1]
Using the apparatus shown in FIG. 1, hydrogen-dissolved water is produced using ultrapure water sufficiently degassed as raw water passing through the liquid phase chamber 12 and using hydrogen gas as the specific gas supplied to the gas phase chamber 13. did. Ultrapure water was supplied to the liquid phase chamber 12 at 1 m ³ / h, and hydrogen gas was supplied to the gas phase chamber 13 at 1.2 g / h to perform continuous operation for 3 months.

  A liquid level gauge was used as the condensed water detection means 35, and a vacuum pump was used as the exhaust device 52.

  The condensed water in the storage part 34 was discharged once every 60 minutes.

Through continuous operation for three months, hydrogen gas-dissolved water having a dissolved hydrogen gas concentration of 1.2 mg / L could be produced at 1 m ³ / h.

[Comparative Example 1]
Using the apparatus in which the third valve 33 was closed except for the gas supply pipe 41 and the valve 53 from the apparatus of FIG.

  In the first comparative example, when the condensed water detecting means 35 detects the condensed water, the first valve 31 is closed and the second valve 32 is opened, and the condensed water in the reservoir 34 is opened by the vacuum pump 52. Was discharged out of the system.

For two months from the start of operation, hydrogen gas-dissolved water having a dissolved hydrogen gas concentration of 1.2 mg / L could be produced at 1 m ³ / h. However, the suction capability of the vacuum pump 52 dropped after two months, and the condensed water was no longer sucked. When the operation was further continued, the dissolved hydrogen gas concentration gradually decreased, and the dissolved hydrogen gas concentration decreased to 0.9 mg / L three months after the operation started. When the operation was stopped and the gas dissolving membrane module 10 was opened, about 3/4 of the gas phase chamber 13 was submerged with condensed water.

It is a systematic diagram explaining the condensed water storage process of the gas dissolving film apparatus which concerns on embodiment. It is a systematic diagram explaining the condensed water discharge process of the gas dissolution membrane apparatus concerning an embodiment. It is a systematic diagram explaining the pressure regulation process of the gas dissolution film apparatus concerning an embodiment. It is a manufacturing-process system diagram of the hydrogen-dissolved water which concerns on a prior art example.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 Gas melt | dissolution membrane module 11 Gas permeable membrane 12 Liquid phase chamber 13 Gas phase chamber 30 Discharge path 31 1st valve 32 2nd valve 33 3rd valve 34 Storage part 35 Condensed water detection means 41 Gas supply piping 52 Exhaust device

Claims (5)

In a gas dissolution membrane device having a gas dissolution membrane module partitioned into a gas phase chamber and a liquid phase chamber by a gas permeable membrane, and a condensed water discharge device for discharging condensed water condensed in the gas phase chamber,
The condensate drain device is
A storage section into which condensed water discharged from the gas phase chamber flows in, and a discharge path having an outflow section of water from the storage section;
A first valve that communicates and shuts off the gas phase chamber and the reservoir;
Gas supply means for supplying pressurized gas into the reservoir with the first valve closed to discharge condensed water in the reservoir from the outlet;
A gas-dissolving membrane device comprising:   2. The pressure adjusting means according to claim 1, wherein a second valve is provided in the outflow portion, and the pressure in the storage portion is adjusted with the first valve and the second valve closed. A gas-dissolving membrane device characterized by that.   3. The gas dissolution membrane device according to claim 2, wherein the pressure adjusting means includes an exhaust device that sucks and exhausts the gas in the exhaust passage. A method for producing a gas-dissolved solution using the gas-dissolving membrane device according to any one of claims 1 to 3,
A liquid is passed through the liquid phase chamber and gas is supplied to the gas phase chamber, and the gas in the gas phase chamber is allowed to pass through the gas permeable membrane and dissolved in the liquid in the liquid phase chamber. During the execution of the production operation of the obtained gas solution,
A condensed water storage step of opening the first valve and receiving condensed water condensed in the gas phase chamber into the storage unit;
A condensed water discharge step of closing the first valve and supplying pressurized gas from the gas supply means into the storage section, and discharging condensed water in the storage section from the outflow section;
Are sequentially performed. A method for producing a gas-dissolved solution. In Claim 4, the said condensed water discharge device is the condensed water discharge device of Claim 2 or 3,
During execution of the manufacturing operation,
A condensed water storage step of opening the first valve and closing the second valve, and receiving condensed water condensed in the gas phase chamber in the storage unit;
The first valve is closed and the second valve is opened, and pressurized gas is supplied from the gas supply means into the reservoir, and the condensed water in the reservoir is discharged from the outlet. A condensate draining process,
The first valve and the second valve are closed, and the pressure adjusting means adjusts the pressure in the reservoir to the same as the pressure in the gas phase chamber, and then opens the first valve. The adjustment process;
Are sequentially performed. A method for producing a gas-dissolved solution.

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