CN111108069A - Particle management method for ultrapure water production system - Google Patents
Particle management method for ultrapure water production system Download PDFInfo
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- CN111108069A CN111108069A CN201880060242.6A CN201880060242A CN111108069A CN 111108069 A CN111108069 A CN 111108069A CN 201880060242 A CN201880060242 A CN 201880060242A CN 111108069 A CN111108069 A CN 111108069A
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- ultrapure water
- fine particles
- bed ion
- regenerative mixed
- mixed bed
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- 229910021642 ultra pure water Inorganic materials 0.000 title claims abstract description 84
- 239000012498 ultrapure water Substances 0.000 title claims abstract description 82
- 239000002245 particle Substances 0.000 title claims abstract description 81
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 238000007726 management method Methods 0.000 title description 20
- 239000012528 membrane Substances 0.000 claims abstract description 88
- 239000010419 fine particle Substances 0.000 claims abstract description 87
- 230000001172 regenerating effect Effects 0.000 claims abstract description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000000926 separation method Methods 0.000 claims abstract description 39
- 238000005342 ion exchange Methods 0.000 claims abstract description 38
- 230000003647 oxidation Effects 0.000 claims abstract description 16
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 16
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 230000007246 mechanism Effects 0.000 claims abstract description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 238000007872 degassing Methods 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000008119 colloidal silica Substances 0.000 description 7
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- 239000011859 microparticle Substances 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000010534 mechanism of action Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001070941 Castanea Species 0.000 description 1
- 235000014036 Castanea Nutrition 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241001089723 Metaphycus omega Species 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
- C02F1/325—Irradiation devices or lamp constructions
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/10—Investigating individual particles
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06M—COUNTING MECHANISMS; COUNTING OF OBJECTS NOT OTHERWISE PROVIDED FOR
- G06M11/00—Counting of objects distributed at random, e.g. on a surface
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
- C02F2103/04—Non-contaminated water, e.g. for industrial water supply for obtaining ultra-pure water
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Toxicology (AREA)
- Theoretical Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Removal Of Specific Substances (AREA)
- Physical Water Treatments (AREA)
Abstract
The subsystem (1) comprises: a sub-tank (2) for storing primary pure water (W), a pump (4) provided at the root end of a supply line (3) for the primary pure water (W) stored in the sub-tank (2), a heat exchanger (5) provided at the rear stage of the pump (4), a low-pressure Ultraviolet (UV) irradiation oxidation device (6), a non-regenerative mixed bed ion exchange device (7), and an ultrafiltration membrane (UF membrane) separation device (8) as a fine particle removal membrane device. A fine particle meter (PC) (9) is connected, which is a mechanism capable of switching between the outlet side of the UF membrane separation device (8) and the outlet side of the non-regenerative mixed bed ion exchange device (7) to measure the number of fine particles. According to the method for particle management in an ultrapure water production system, the number of particles in ultrapure water can be maintained in a reduced state.
Description
Technical Field
The present invention relates to a method for particle management in an ultrapure water production system, and more particularly to a method for particle management in an ultrapure water production system capable of maintaining the number of particles in ultrapure water in a reduced state.
Background
Apparatuses for producing ultrapure water used in the field of electronics industry are roughly classified into: a pretreatment apparatus for removing suspended matter and the like from water commonly used for industrial water, tap water and the like; a primary pure water unit for purifying the treated water of the pretreatment unit to produce pure water from which most of impurities have been removed; and a secondary pure water apparatus (subsystem) for producing ultrapure water from which impurities have been almost completely removed by further highly purifying the primary pure water.
Among them, the secondary water purification system (sub-system) basically comprises, as a base, a low-pressure Ultraviolet (UV) irradiation oxidation system for decomposing organic substances, a non-regenerative mixed bed ion exchange system packed with an ion exchange resin for adsorbing and removing ionic impurities, and an ultrafiltration membrane (UF membrane) separation system for completely removing fine particles, and further improves the purity of water to produce ultrapure water. In this case, the low pressure is passed through in a low-pressure UV radiation oxidation apparatusUltraviolet light emitted by the UV lamp at a wavelength of 185nm decomposes TOC to organic acids and further to CO2. Organic acid and CO generated by decomposition2Is removed by the ion exchange resin of the latter stage. In the UF membrane separation apparatus, fine particles such as particles flowing out of the ion exchange resin are removed. As described above, conventionally, the nano-sized particle removal treatment is performed by providing a particle removal film such as a UF film at the end of the subsystem, but in recent years, as semiconductor products have been advanced to higher performance and finer size, the management of particles has become stricter, and for example, in semiconductor factories, the management value is often set to be the one in many casesThe number of particles is 1/mL or less. Therefore, at present, the number of particles in ultrapure water is measured and managed at the outlet of the UF membrane separation apparatus of the subsystem.
A representative example of this subsystem is shown in fig. 5. In fig. 5, the subsystem 21 has: a sub-tank 22 for storing primary pure water W, a pump 24 provided at the root end of a supply line 23 for primary pure water W stored in the tank 22, a heat exchanger 25 provided at the subsequent stage of the pump 24, a low-pressure UV irradiation oxidation apparatus 26, a non-regenerative mixed bed ion exchange apparatus 27, and a UF membrane separation apparatus 28. Further, a particle meter (PC)29 as an off-line monitor is provided on the outlet side of the UF membrane separation device 28.
In the operation of the subsystem 21 described above, the pump 24 is operated to introduce the primary pure water W in the subtank 22 into the heat exchanger 25, the low-pressure UV irradiation oxidation apparatus 26, the non-regenerative mixed bed ion exchange apparatus 27, and the UF membrane separation apparatus 28 in this order, and the obtained ultrapure water W1 is sent to the water use point POU. On the other hand, the ultrapure water W1 unused at the water usage point POU is returned to the subtank 22 via the circulation line 23A and is treated again.
Disclosure of Invention
Problems to be solved by the invention
In the conventional subsystem 21 shown in fig. 5, the number of fine particles in the ultrapure water W1 is controlled by a fine particle meter 29 on the outlet side of the UF membrane separation unit 28, the particle load on the outlet side of the non-regenerative mixed bed ion exchanger 27 is measured by an electric conductivity meter, a specific resistance meter, or the like, and the non-regenerative mixed bed ion exchanger 27 is periodically replaced when the measurement result is larger than a predetermined value. However, even if such a management method is performed, there are the following problems: the particles leaked into the ultrapure water W1, and the number of particles in the ultrapure water W1 could not be maintained in a reduced state.
The present invention has been made in view of the above problems, and an object of the present invention is to provide a particle management method for an ultrapure water production system, which can maintain the number of particles in ultrapure water in a reduced state.
Means for solving the problems
In view of the above-mentioned object, the present invention provides a method for particle management in an ultrapure water production system, which comprises treating primary pure water produced in a primary pure water system with a sub-system, the sub-system is provided with a non-regenerative mixed bed ion exchange device and a fine particle removal membrane device in this order, and in the fine particle management method of the ultrapure water production system, monitoring is performed by measuring the number of particles in the ultrapure water at the outlet of the fine particle removal membrane apparatus by means of a fine particle number measuring means, while measuring the number of particles in the treated water of the non-regenerative mixed bed ion exchange apparatus by means of a fine particle number measuring means, when the number of fine particles in the treated water in the non-regenerative mixed bed ion exchanger exceeds a predetermined value, the non-regenerative mixed bed ion exchanger is replaced (invention 1).
According to the above invention (invention 1), the number of microparticles in the ultrapure water at the outlet of the microparticle removal membrane device can be stably reduced by measuring and managing the number of microparticles in the treated water of the non-regenerative mixed bed ion exchange device by the microparticle number measuring means. The reason is presumed as follows. That is, in the case where the particles in the ultrapure water are managed only on the outlet side of the particle removal film device, although the increase in the particles can be detected at the time point when the particles leak from the particle removal film device, it is not possible to prevent the occurrence of the case where the ultrapure water in which the number of particles is increased from the reference value is supplied at an early stage. Therefore, the present inventors examined the correlation between the number of particles in the treatment water of the non-regenerative mixed-bed ion exchange device and the number of particles in the ultrapure water treated by the particle removal membrane device, and as a result, found that when the number of particles in the treatment water of the non-regenerative mixed-bed ion exchange device increases, the particles are likely to leak into the ultrapure water at the outlet of the particle removal membrane device. Therefore, by managing the increase of the number of particles in the treatment water in the non-regenerative mixed bed ion exchange device and confirming the number of particles in the ultrapure water at the outlet of the particle removal membrane device, the treatment water can be stably supplied in a state in which the number of particles in the obtained ultrapure water has been reduced.
In the above invention (invention 1), the sub-system preferably includes a low-pressure Ultraviolet (UV) irradiation oxidation apparatus, a non-regenerative mixed bed ion exchange apparatus, and an ultrafiltration membrane (UF membrane) separation apparatus (invention 2) as the fine particle removal membrane apparatus in this order. In addition, in the above invention (invention 1), it is preferable that the subsystem comprises a low-pressure Ultraviolet (UV) irradiation oxidation device, a catalyst resin (hydrogen peroxide removal) device, a membrane degassing device, a non-regenerative mixed bed type ion exchange device, and an ultrafiltration membrane (UF membrane) separation device as the fine particle removal membrane device in this order (invention 3). Further, in the above invention (invention 1), it is preferable that the sub-system comprises a low-pressure Ultraviolet (UV) irradiation oxidation device, a non-regenerative mixed bed type ion exchange device, a membrane type degassing device, and an ultrafiltration membrane (UF membrane) separation device as the fine particle removal membrane device in this order (invention 4).
According to the above inventions (inventions 2 to 4), in the non-regenerative mixed bed ion exchanger disposed at the front stage of the ultrafiltration membrane (UF membrane) separation device, since fine particles such as colloidal silica are more likely to penetrate than sodium and chlorine plasma and the number of fine particles in ultrapure water increases as the fine particles flow out from the rupture portion of the ultrafiltration membrane (UF membrane) separation device, the number of fine particles in treated water in the non-regenerative mixed bed ion exchanger is managed, and when the number of fine particles is larger than a predetermined value, the non-regenerative mixed bed ion exchanger is replaced and the number of fine particles in ultrapure water at the outlet of the fine particle removal membrane device is confirmed, whereby the ultrapure water having an increased number of fine particles can be prevented from being supplied at an early stage.
In the above inventions (inventions 1 to 4), it is preferable that the number of fine particles measuring means is a fine particle meter, and the number of fine particles in the treated water of the non-regenerative mixed bed ion exchange device and the number of fine particles in the ultrapure water at the outlet of the fine particle removal membrane device are measured by switching one fine particle meter (invention 5).
According to the above invention (invention 5), the number of particles in the treatment water of the non-regenerative mixed bed ion exchanger and the number of particles in the ultrapure water at the outlet of the particle removal membrane device can be measured by one particle meter.
In the above inventions (inventions 1 to 4), it is preferable that the number of fine particles measuring means is a fine particle meter, the fine particle meter is provided on each of the outlet side of the non-regenerative mixed bed ion exchanger and the outlet side of the fine particle removal membrane device, and the number of fine particles in the treated water of the non-regenerative mixed bed ion exchanger and the number of fine particles in the ultrapure water at the outlet of the fine particle removal membrane device are measured (invention 6).
According to the above invention (invention 6), the number of particles in the treatment water of the non-regenerative mixed bed ion exchanger and the number of particles in the ultrapure water at the outlet of the particle removal membrane device can be measured independently of each other.
Effects of the invention
The present invention measures the number of particles in the treated water of a non-regenerative mixed bed ion exchanger, replaces the non-regenerative mixed bed ion exchanger when the number of particles exceeds a predetermined value, and confirms the number of particles in the ultrapure water at the outlet of a particle removal membrane device, thereby preventing the ultrapure water, the number of which increases, from being supplied at an early stage.
Drawings
FIG. 1 is a schematic view showing an ultrapure water production system to which a particle management method of an ultrapure water production system according to a first embodiment of the present invention can be applied.
FIG. 2 is a schematic view showing an ultrapure water production system to which a particle management method of an ultrapure water production system according to a second embodiment of the present invention can be applied.
FIG. 3 is a schematic diagram showing an ultrapure water production system to which a particle management method of an ultrapure water production system according to a third embodiment of the present invention can be applied.
FIG. 4 is a schematic diagram showing an ultrapure water production system to which a particle management method of an ultrapure water production system according to a fourth embodiment of the present invention can be applied.
FIG. 5 is a schematic diagram showing an ultrapure water production system to which a particle management method of a conventional ultrapure water production system can be applied.
Detailed Description
Hereinafter, a method for particle management in an ultrapure water production system according to a first embodiment of the present invention will be described in detail with reference to fig. 1.
The subsystem to which the particle management method of the ultrapure water production system of the present embodiment can be applied basically has the same configuration as that of the system shown in fig. 5. That is, in fig. 1, the subsystem 1 includes: a subtank 2 for storing primary pure water W, a pump 4 provided at the root end of a supply line 3 for the primary pure water W stored in the subtank 2, a heat exchanger 5 provided at the subsequent stage of the pump 4, a low-pressure UV irradiation oxidation apparatus 6, a non-regenerative mixed bed type ion exchange apparatus 7, and an ultrafiltration membrane (UF membrane) separation apparatus 8 as a fine particle removal membrane apparatus. A fine particle meter (PC)9, which is a mechanism capable of switching between the outlet side of the UF membrane separation apparatus 8 and the outlet side of the non-regenerative mixed bed ion exchange apparatus 7 to measure the number of fine particles, is connected. As the fine particle meter 9, "K-LAMIC" (trade name) manufactured by Nippon chestnut industries, Inc., and "UDI-50" (trade name) manufactured by PMS, Inc., can be used.
When the subsystem 1 described above is operated, the pump 4 is operated to introduce the primary pure water W in the subtank 2 into the heat exchanger 5, the low-pressure UV irradiation oxidation apparatus 6, and the non-regenerative mixed-bed ion exchange apparatus 7 in this order, and the treated water W2 in the non-regenerative mixed-bed ion exchange apparatus 7 is introduced into the UF membrane separation apparatus 8 to obtain ultrapure water W1. Then, the obtained ultrapure water W1 is supplied to the water consumption point POU. On the other hand, the ultrapure water W1 unused at the water usage point POU is returned to the subtank 2 via the circulation line 3A and is treated again.
As ultrapure water W1 in the present embodiment, water having a resistivity: 18.1 M.OMEGA.cm or more, fine particles: viable bacteria with a particle size of 50nm to 1000/L: less than 1/L, TOC (Total organic carbon): 1 μ g/L of total silicon: 0.1. mu.g/L of the following metals: 1ng/L of ions below: hydrogen peroxide with the concentration of 10ng/L or less: 30 μ g/L below, water temperature: 25 +/-2 ℃.
Next, a method of particle management in the ultrapure water production system will be described.
[ operation in the usual case ]
In the above-described ultrapure water production process, the number of fine particles of ultrapure water W1 on the outlet side of the UF membrane separation device 8 and the number of fine particles of treated water W2 in the non-regenerative mixed bed ion exchange device 7 were measured by appropriately switching the fine particle meter 9 to the outlet side of the UF membrane separation device 8 and the outlet side of the non-regenerative mixed bed ion exchange device 7 at predetermined timings, respectively. Then, as long as the number of particles of the ultrapure water W1 is 1/mL or less and the number of particles of the treated water W2 of the non-regenerative mixed bed ion exchange device 7 is 10/mL or less, the operation of the subsystem 1 can be continued and the ultrapure water W1 can be supplied to the water consumption point POU.
[ management operation of the number of particles ]
On the other hand, when the number of fine particles of ultrapure water W1 on the outlet side of the UF membrane separation apparatus 8 measured by the fine particle meter 9 as an off-line monitor is 1/mL or less and the number of fine particles of treated water W2 of the non-regenerative mixed bed ion exchange apparatus 7 exceeds 10/mL, the operation of the subsystem 1 is temporarily stopped and the non-regenerative mixed bed ion exchange apparatus 7 is replaced. This makes it possible to keep the number of fine particles of the ultrapure water W1 on the outlet side of the UF membrane separation device 8 at 1/mL or less, and to prevent the ultrapure water W1 having a number of fine particles exceeding the reference value from being supplied to the water consumption point POU. When the number of fine particles of the ultrapure water W1 on the outlet side of the UF membrane separation device 8 is still more than 1/mL after the above management, it is determined that the UF membrane separation device 8 has broken, and the UF membrane separation device 8 and the like may be replaced.
< mechanism of action >
The above effects can be obtained based on the following mechanism of action. Namely, it is reported that: in general, in ion exchange devices, soluble silica is very easy to remove, while colloidal silica is very difficult to remove (easy to penetrate) compared to boron ("UPW Micro 2017, UPW IRDS and SEMI update" slave Libman, etc.). In addition, the boron is more than sodium ion (Na) contained in the primary pure water W+) Chloride ion (Cl)-) Or carbonate ion (HCO)3 -) Very difficult to remove (easy to penetrate). That is, colloidal silica is far more specific than sodium ion (Na)+) Chloride ion (Cl)-) Carbonate ion (HCO)3 -) Easier to penetrate.
Therefore, the results of the investigation by the present inventors have clarified that the increase in the number of fine particles on the outlet side of the non-regenerative mixed-bed ion exchange device 7, that is, on the inlet side of the UF membrane separation device 8 is mainly caused by the colloidal silica particles. Conventionally, although a means for measuring an ion load, such as a conductivity meter or a specific resistance meter, is provided on the outlet side of the non-regenerative mixed bed ion exchanger 7 to measure the ion load, and the non-regenerative mixed bed ion exchanger 7 is periodically replaced when the measured value is larger than a predetermined value, the colloidal silica fine particles flow into the UF membrane separator 8. In contrast, by managing the number of particles of the treated water in the non-regenerative mixed-bed ion exchanger 7 from the viewpoint as in the present embodiment, the non-regenerative mixed-bed ion exchanger 7 can be replaced before the particles reach the outlet of the UF membrane separator 8, and therefore, it is possible to hopefully stabilize the number of particles of the ultrapure water W1 at the outlet of the UF membrane separator 8. Then, it is sufficient to measure and confirm by the particle meter 9 that the number of particles of the ultrapure water W1 does not increase.
The first embodiment of the present invention has been described above with reference to the drawings, but the present invention is not limited to the above embodiment and various modifications can be made. For example, it is also possible to provide a configuration in which a first particle meter 9A is provided on the outlet side of the UF membrane separation device 8 and a second particle meter 9B is provided on the outlet side of the non-regenerative mixed-bed ion exchange device 7, and the number of particles of the treated water W2 in the non-regenerative mixed-bed ion exchange device 7 and the number of particles of the ultrapure water W1 at the outlet of the UF membrane separation device 8 are measured independently from each other, as shown in fig. 2. In addition, the particle meter 9 and the like may be an on-line monitor using a centrifugal filtration method instead of an off-line monitor as the means for measuring the number of particles.
The subsystem 1 is not limited to the configurations of the first and second embodiments described above, and may be applied to various subsystems. For example, as shown in fig. 3, a system may be applied in which a catalyst resin (hydrogen peroxide removal) device 10 filled with an ion exchange resin loaded with a platinum group metal or the like and a membrane degassing device 11 are provided at a later stage of the low-pressure Ultraviolet (UV) irradiation oxidation device 6, and the latter stage is provided with a non-regenerative mixed bed type ion exchange device 7 and an ultrafiltration membrane (UF membrane) separation device 8 in this order. The subsystem 1 can also be applied to a subsystem in which a membrane type degassing device 12 is provided between a non-regenerative mixed bed type ion exchange device 7 and an ultrafiltration membrane (UF membrane) separation device 8, for example, as shown in fig. 4. In this case, the means for measuring the number of fine particles such as the fine particle meter 9 may be provided with another module such as the membrane type deaerator 12 as long as it is located on the outlet side of the non-regenerative mixed bed type ion exchanger 7 and before the UF membrane separation unit 8, and in this case, the number of fine particles may be measured on the outlet side of the other module or may be measured immediately after the non-regenerative mixed bed type ion exchanger 7.
Examples
The present invention will be described in more detail below with reference to specific examples.
[ Experimental example 1]
Ultrapure water was produced from city water as raw water by the ultrapure water production system shown in fig. 1. The low-pressure UV irradiation oxidation apparatus 6 constituting the subsystem 1 was manufactured by photoscience japan corp., japan フォトサイエンス, the non-regenerative mixed bed ion exchange apparatus 7 was manufactured by KR-FM (trade name) manufactured by kutakaki corporation, the UF membrane separation apparatus 8 was manufactured by KU corporation, KU-1510-HP-H (trade name), and the particle meter 9 was manufactured by kutakaki corporation, K-LAMIC (trade name).
In the ultrapure water production process in the ultrapure water production system described above, the treated water W2 of the non-regenerative mixed bed ion exchanger 7 and the ultrapure water W1 at the outlet of the UF membrane separation unit 8 were monitored for the number of fine particles, and when the treated water W2 of the non-regenerative mixed bed ion exchanger 7 exceeded 10 particles/mL, the non-regenerative mixed bed ion exchanger 7 was replaced and the above operations were repeated, with the result that the number of fine particles of the ultrapure water W1 at the outlet of the UF membrane separation unit 8 did not exceed 1 particle/mL. This is considered to be because the number of fine particles due to colloidal silica or the like in the treated water W2 flowing into the UF membrane separation apparatus 8 can be suppressed.
Comparative example 1
In example 1, the number of fine particles in the treated water W2 of the non-regenerative mixed bed ion exchanger 7 was not measured, but a specific resistance value was measured by a specific resistance meter, an ion load was determined from the specific resistance value, the non-regenerative mixed bed ion exchanger 7 was replaced when the ion load exceeded a predetermined value, and the above operations were repeated, showing that the number of fine particles in the ultrapure water W1 at the outlet of the UF membrane separator 8 tended to exceed 1/mL with time. The reason for this is considered to be that colloidal silica leaks due to partial cracking caused by the time-dependent deterioration of the UF membrane separation apparatus 8.
Description of reference numerals
1, a subsystem;
2, a sub-tank;
3 supply lines;
3A circulating line;
4, a pump;
5, a heat exchanger;
6 low pressure Ultraviolet (UV) irradiation oxidation device;
7 a non-regenerative mixed bed ion exchanger;
8 ultrafiltration membrane (UF membrane) separation means (particulate removal membrane means);
9. 9A, 9B particle meter (particle number measuring means);
water consumption points of the POU;
w primary pure water;
w1 ultrapure water;
w2 treated water of a non-regenerative mixed bed ion exchanger.
Claims (6)
1. A method for managing fine particles in an ultrapure water production system, which comprises treating primary pure water produced in a primary pure water system with a subsystem comprising a non-regenerative mixed-bed ion exchange device and a fine particle removal membrane device in this order,
monitoring is performed by measuring the number of particles in the ultrapure water at the outlet of the particle removal membrane device by a particle number measuring mechanism,
on the other hand, the number of fine particles in the treated water of the non-regenerative mixed bed ion exchanger is measured by fine particle number measuring means, and when the number of fine particles in the treated water of the non-regenerative mixed bed ion exchanger exceeds a predetermined value, the non-regenerative mixed bed ion exchanger is replaced.
2. The method for managing fine particles in an ultrapure water production system according to claim 1, wherein said sub-system comprises a low-pressure ultraviolet irradiation oxidation apparatus, a non-regenerative mixed bed ion exchange apparatus and an ultrafiltration membrane separation apparatus as said fine particle removal membrane apparatus in this order.
3. The method for managing fine particles in an ultrapure water production system according to claim 1, wherein the subsystem comprises a low-pressure ultraviolet irradiation oxidation apparatus, a catalyst resin apparatus, a membrane degassing apparatus, a non-regenerative mixed bed ion exchange apparatus, and an ultrafiltration membrane separation apparatus as the fine particle removal membrane apparatus in this order, and the catalyst resin apparatus is a hydrogen peroxide removal apparatus.
4. The method for managing fine particles in an ultrapure water production system according to claim 1, wherein said sub-system comprises a low-pressure ultraviolet irradiation oxidation apparatus, a non-regenerative mixed bed ion exchange apparatus, a membrane type degassing apparatus and an ultrafiltration membrane separation apparatus as said fine particle removal membrane apparatus in this order.
5. The method for managing fine particles in an ultrapure water production system according to any one of claims 1 to 4, wherein the means for measuring the number of fine particles is a fine particle meter, and the number of fine particles in the treated water in the non-regenerative mixed bed ion exchange device and the number of fine particles in the ultrapure water at the outlet of the fine particle removal membrane device are measured by switching one fine particle meter.
6. The method for managing fine particles in an ultrapure water production system according to any one of claims 1 to 4, wherein the means for measuring the number of fine particles is a fine particle meter, and the fine particle meter is provided on each of the outlet side of the non-regenerative mixed bed ion exchange device and the outlet side of the fine particle removal membrane device so as to measure the number of fine particles in the treated water of the non-regenerative mixed bed ion exchange device and the number of fine particles in the ultrapure water at the outlet of the fine particle removal membrane device.
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JP2018019853A JP7143595B2 (en) | 2018-02-07 | 2018-02-07 | Particle control method for ultrapure water production system |
PCT/JP2018/034111 WO2019155672A1 (en) | 2018-02-07 | 2018-09-14 | Fine particle management method for ultrapure water production system |
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KR (1) | KR102613112B1 (en) |
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JPH0929251A (en) * | 1995-07-17 | 1997-02-04 | Kurita Water Ind Ltd | Ultrapure water preparing apparatus |
JP2010227886A (en) | 2009-03-27 | 2010-10-14 | Kurita Water Ind Ltd | Apparatus for producing pure water |
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2018
- 2018-02-07 JP JP2018019853A patent/JP7143595B2/en active Active
- 2018-09-14 WO PCT/JP2018/034111 patent/WO2019155672A1/en active Application Filing
- 2018-09-14 KR KR1020207007350A patent/KR102613112B1/en active IP Right Grant
- 2018-09-14 CN CN201880060242.6A patent/CN111108069A/en active Pending
- 2018-09-18 TW TW107132793A patent/TW201936513A/en unknown
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JP2004223425A (en) * | 2003-01-23 | 2004-08-12 | Kurita Water Ind Ltd | Ion exchange resin for producing ultrapure water, and method for producing ultrapure water using the same |
US20080245738A1 (en) * | 2007-04-03 | 2008-10-09 | Siemens Water Technologies Corp. | Method and system for providing ultrapure water |
JP2010069460A (en) * | 2008-09-22 | 2010-04-02 | Japan Organo Co Ltd | Method for reducing hydrogen peroxide, device for reducing the same, device for manufacturing ultrapure water and cleaning method |
CN103359850A (en) * | 2012-04-09 | 2013-10-23 | 野村微科学股份有限公司 | Ultrapure water manufacturing apparatus |
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WO2019155672A1 (en) | 2019-08-15 |
JP7143595B2 (en) | 2022-09-29 |
TW201936513A (en) | 2019-09-16 |
KR20200117972A (en) | 2020-10-14 |
JP2019136628A (en) | 2019-08-22 |
KR102613112B1 (en) | 2023-12-12 |
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