WO2019155672A1 - Fine particle management method for ultrapure water production system - Google Patents
Fine particle management method for ultrapure water production system Download PDFInfo
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- WO2019155672A1 WO2019155672A1 PCT/JP2018/034111 JP2018034111W WO2019155672A1 WO 2019155672 A1 WO2019155672 A1 WO 2019155672A1 JP 2018034111 W JP2018034111 W JP 2018034111W WO 2019155672 A1 WO2019155672 A1 WO 2019155672A1
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- WIPO (PCT)
- Prior art keywords
- ultrapure water
- membrane
- fine particle
- fine particles
- bed ion
- Prior art date
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- 239000010419 fine particle Substances 0.000 title claims abstract description 116
- 229910021642 ultra pure water Inorganic materials 0.000 title claims abstract description 82
- 239000012498 ultrapure water Substances 0.000 title claims abstract description 80
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 238000007726 management method Methods 0.000 title claims abstract description 21
- 239000012528 membrane Substances 0.000 claims abstract description 92
- 230000001172 regenerating effect Effects 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000005342 ion exchange Methods 0.000 claims abstract description 36
- 238000000926 separation method Methods 0.000 claims abstract description 28
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims description 42
- 239000007800 oxidant agent Substances 0.000 claims description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims 1
- 238000012544 monitoring process Methods 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group 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 6
- 239000000460 chlorine Substances 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
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- -1 chlorine ions Chemical class 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
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 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
- 150000001638 boron Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 239000008213 purified water Substances 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
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 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
Definitions
- the present invention relates to a particle management method for an ultrapure water production system, and more particularly, to a particle management method for an ultrapure water production system that can maintain a reduced number of particles in ultrapure water.
- the ultrapure water production equipment used in the electronics industry is largely divided into a pretreatment device that removes turbidity from normal water such as industrial water and tap water, and a large amount of purified water from the pretreatment device.
- a primary pure water device for producing pure water from which impurities are partially removed and a secondary pure water device (subsystem) for producing ultrapure water from which the primary pure water has been further refined to remove impurities completely. Consists of.
- the secondary pure water device is basically a low-pressure ultraviolet (UV) irradiation oxidizer that decomposes organic matter, and a non-regenerative mixed bed filled with an ion exchange resin that adsorbs and removes ionic impurities.
- a basic ion exchange device and an ultrafiltration membrane (UF membrane) separation device for completely removing fine particles are provided as basic components, and the purity of water is further increased to ultrapure water.
- TOC is decomposed into an organic acid and further to CO 2 by ultraviolet rays having a wavelength of 185 nm emitted from a low pressure UV lamp.
- the decomposed organic acid and CO 2 are removed by a subsequent ion exchange resin.
- fine particles such as outflow particles of the ion exchange resin are removed.
- nanometer-size fine particle removal processing has been performed by installing a fine particle removal film such as a UF membrane at the end of the subsystem.
- semiconductor products have become more sophisticated and refined. Accordingly, the management of fine particles is becoming stricter. For example, in a semiconductor factory, the control value is often set to 1 particle / mL or less of particles having a diameter of 50 nm or more. For this reason, the number of fine particles in ultrapure water is measured and managed at the outlet of the UF membrane separator of the subsystem.
- the sub-system 21 includes a sub tank 22 for storing the primary pure water W, a pump 24 provided at the base end portion of the supply line 23 of the primary pure water W stored in the tank 22, and the pump 24, a heat exchanger 25, a low-pressure UV irradiation oxidizer 26, a non-regenerative mixed bed ion exchanger 27, and a UF membrane separator 28 provided in the subsequent stage.
- a fine particle meter (PC) 29 as an off-line monitor is provided on the outlet side of the UF membrane separation device 28.
- PC fine particle meter
- the pump 24 is operated, and the primary pure water W in the sub-tank 22 is converted into the heat exchanger 25, the low-pressure UV irradiation oxidizer 26, and the non-regenerative mixed bed ion exchanger 27. And the UF membrane separator 28 are sequentially passed, and the obtained ultrapure water W1 is sent to the use point POU. On the other hand, the ultrapure water W1 that has not been used at the use point POU is returned to the sub tank 22 via the circulation line 23A and processed again.
- the number of fine particles in the ultrapure water W1 is managed by the fine particle meter 29 on the outlet side of the UF membrane separation device 28, while the non-regenerative mixed bed ion exchange device 27
- the ion load on the outlet side was measured with a conductivity meter, a specific resistance meter or the like, and was periodically exchanged when it became larger than a predetermined value.
- a conductivity meter, a specific resistance meter or the like was measured with a conductivity meter, a specific resistance meter or the like, and was periodically exchanged when it became larger than a predetermined value.
- the present invention has been made in view of the above problems, and an object thereof is to provide a method for managing fine particles of an ultrapure water production system capable of maintaining a state in which the number of fine particles in ultrapure water is reduced. To do.
- the present invention provides fine particles of an ultrapure water production system in which primary pure water produced by a primary pure water system is treated by a subsystem having a non-regenerative mixed bed ion exchange device and a fine particle removal membrane device in this order.
- a management method wherein the number of fine particles in ultrapure water at the outlet of the fine particle removal membrane device is monitored by measuring the number of fine particles, and the treated water fine particles of the non-regenerative mixed bed ion exchange device A non-regenerative mixed bed ion exchanger is replaced when the number of treated water particles in the non-regenerative mixed bed ion exchanger exceeds a predetermined value.
- a fine particle management method for a water production system is provided (Invention 1).
- invention 1 by measuring and managing the number of fine particles of the treated water of the non-regenerative type mixed bed ion exchange device by the fine particle number measuring means, ultrapure water at the outlet of the fine particle removal membrane device It is possible to stably reduce the number of fine particles. This is presumed to be due to the following reasons. That is, when the fine particles in ultrapure water are managed only on the outlet side of the fine particle removal membrane device, the increase in fine particles can be detected when the fine particle leaks from the fine particle removal membrane device. The supply of ultrapure water having an increased number of fine particles cannot be prevented in advance.
- the present inventors It was found that when the number of treated water particles in the mixed bed type ion exchanger increased, the particles easily leaked into the ultrapure water at the outlet of the particle removing membrane device. Therefore, by controlling the increase in the treated water particulates in this non-regenerative mixed bed ion exchange device, and confirming the number of particulates in the ultrapure water at the outlet of the particulate removal membrane device, Can be stably supplied with the number of fine particles reduced.
- the subsystem includes a low-pressure ultraviolet (UV) irradiation oxidizer, a non-regenerative mixed bed ion exchanger, and an ultrafiltration membrane (UF membrane) separator as the particulate removal membrane device. It is preferable to prepare in this order (Invention 2).
- the subsystem is a low-pressure ultraviolet (UV) irradiation oxidizer, a catalyst resin (hydrogen peroxide removal) device, a membrane deaerator, a non-regenerative mixed bed ion exchanger, and It is preferable to provide an ultrafiltration membrane (UF membrane) separation device as the fine particle removal membrane device in this order (Invention 3).
- the said subsystem is ultrafiltration as a low-pressure ultraviolet-ray (UV) irradiation oxidation apparatus, a non-regenerative mixed bed type ion exchange apparatus, a membrane-type deaeration apparatus, and the said fine particle removal membrane apparatus. It is preferable to provide a membrane (UF membrane) separation device in this order (Invention 4).
- the non-regenerative mixed bed type ion exchange device arranged in the front stage of the ultrafiltration membrane (UF membrane) separator is colloidal silica compared to ions such as sodium and chlorine. And so on, and the fine particles flow out from the ruptured part of the ultrafiltration membrane (UF membrane) separator and increase the number of fine particles in ultrapure water.
- 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 apparatus
- the particle number measuring means is a particle meter, and the number of treated water particles in the non-regenerative mixed bed ion exchanger and the ultrapure water at the outlet of the particle removal membrane device It is preferable to measure the number of particles inside by switching one particle meter (Invention 5).
- the number of treated water particles in the non-regenerative mixed bed ion exchanger and the number of particles in ultrapure water at the outlet of the particle removal membrane device are measured with one particle meter. be able to.
- the fine particle number measuring means is a fine particle meter, and a 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.
- a 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.
- the number of treated water particles in the non-regenerative mixed bed ion exchanger and the number of particles in ultrapure water at the outlet of the particle removing membrane device can be measured independently.
- the present invention measures the number of fine particles of treated water in a non-regenerative type mixed bed type ion exchange device, and when the number of fine particles exceeds a predetermined value, replaces the non-regenerative type mixed bed type ion exchange device to remove fine particles.
- the subsystem to which the particulate management method of the ultrapure water production system of the present embodiment can be applied has basically the same configuration as that shown in FIG. That is, in FIG. 1, the sub-system 1 includes a sub-tank 2 for storing the primary pure water W, a pump 4 provided at the base end portion of the supply line 3 of the primary pure water W stored in the sub-tank 2, A heat exchanger 5, a low-pressure UV irradiation oxidizer 6, a non-regenerative mixed bed ion exchanger 7, and an ultrafiltration membrane (UF membrane) separator 8 as a fine particle removal membrane device provided at the subsequent stage of the pump 4.
- UF membrane ultrafiltration membrane
- a fine particle meter (PC) 9 is connected 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 to measure the number of fine particles in a switchable manner.
- the fine particle counter 9 “K-LAMIC” (trade name) manufactured by Kurita Kogyo Co., Ltd., “UDI-50” (trade name) manufactured by PMS, etc. can be used.
- the pump 4 is operated and the primary pure water W in the sub-tank 2 is sequentially transferred to the heat exchanger 5, the low-pressure UV irradiation oxidizer 6, and the non-regenerative mixed bed ion exchanger 7.
- Water is passed through and the treated water W2 of the non-regenerative mixed bed ion exchange device 7 is passed through the UF membrane separation device 8 to obtain ultrapure water W1.
- the obtained ultrapure water W1 is supplied to the use point POU.
- the ultrapure water W1 that has not been used at the use point POU is returned to the sub tank 2 via the circulation line 3A and is processed again.
- ultrapure water W1 in the present embodiment resistivity: 18.1 M ⁇ ⁇ cm or more, fine particles: particle size of 50 nm or more and 1000 / L or less, viable bacteria: 1 / L or less, TOC (Total Organic Carbon ): 1 ⁇ g / L or less, Total silicon: 0.1 ⁇ g / L or less, Metals: 1 ng / L or less, Ions: 10 ng / L or less, Hydrogen peroxide: 30 ⁇ g / L or less, Water temperature: 25 ⁇ 2 ° C. Is preferred.
- the fine particle counter 9 is appropriately switched 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 at predetermined timings, The number of fine particles of the ultrapure water W1 on the outlet side of the UF membrane separation device 8 and the number of fine particles of the treated water W2 of the non-regenerative mixed bed ion exchange device 7 are measured.
- the operation of the sub-system 1 is performed. Continue to supply ultrapure water W1 to the use point POU.
- the number of fine particles of the ultrapure water W1 on the outlet side of the UF membrane separation device 8 can be maintained at 1 / mL or less, and the ultrapure water W1 with the number of fine particles exceeding the reference value is supplied to the use point POU. Can be prevented in advance. Even if such management is performed, if the number of fine particles of the ultrapure water W1 on the outlet side of the UF membrane separator 8 exceeds 1 / mL, it is determined that the UF membrane separator 8 has been broken. The UF membrane separation device 8 may be replaced.
- the increase in the number of fine particles on the outlet side of the non-regenerative mixed bed ion exchange device 7, that is, the inlet side of the UF membrane separation device 8 is mainly caused by colloidal silica particles.
- the non-regenerative mixed bed ion exchange apparatus 7 is provided with means for measuring an ion load such as a conductivity meter and a specific resistance meter on the outlet side thereof to measure the ion load, which becomes larger than a predetermined value.
- the colloidal silica particles flow into the UF membrane separation device 8.
- the non-regenerative mixed bed ion exchange device 7 by controlling the number of treated water fine particles in the non-regenerative mixed bed ion exchange device 7 as in the present embodiment, it is possible to control the fine particles before they reach the outlet of the UF membrane separation device 8. Since the regenerative mixed bed type ion exchange device 7 can be exchanged, the number of fine particles of the ultrapure water W1 at the outlet of the UF membrane separation device 8 can be stabilized. Then, it may be confirmed by measuring with the fine particle meter 9 that the number of fine particles of the ultrapure water W1 does not increase.
- the first particle counter 9A is provided on the outlet side of the UF membrane separation device 8 and the second particle counter 9B is provided on the outlet side of the non-regenerative mixed bed ion exchanger 7.
- a configuration may be employed in which the number of fine particles in the treated water W2 of the non-regenerative mixed bed ion exchange device 7 and the number of fine particles in the ultrapure water W1 at the outlet of the UF membrane separation device 8 are independently measured.
- the fine particle counter 9 and the like may be an online monitor using a centrifugal filtration method instead of an offline monitor.
- the subsystem 1 is not limited to those of the first and second embodiments described above, and can be applied to various subsystems.
- a non-regenerative mixed bed ion exchange device 7 and an ultrafiltration membrane (UF membrane) separation device 8 in this order can be suitably applied.
- the subsystem 1 for example, as shown in FIG.
- a membrane deaerator 12 is provided between a non-regenerative mixed bed ion exchanger 7 and an ultrafiltration membrane (UF membrane) separator 8 It can be suitably applied to.
- the particle number measuring means such as the particle counter 9 is in front of the UF membrane separation device 8 on the outlet side of the non-regenerative mixed bed ion exchange device 7, other elements such as the membrane deaeration device 12 are used. In such a case, the number of fine particles may be measured at the outlet side of another element, or may be measured immediately after the non-regenerative mixed bed ion exchange device 7.
- Example 1 The ultrapure water production system shown in FIG. 1 was used to produce ultrapure water using city water as raw water.
- the low pressure UV irradiation oxidizer 6 constituting the subsystem 1 is a product of Japan Photoscience
- the non-regenerative mixed bed ion exchanger 7 is “KR-FM” manufactured by Kurita Kogyo Co., Ltd.
- a UF membrane separator “KU-1510-HP-H” manufactured by Kurita Kogyo Co., Ltd. was used as 8
- K-LAMIC manufactured by Kurita Kogyo Co., Ltd. was used as the fine particle counter 9.
- the number of fine particles in the treated water W2 of the non-regenerative mixed bed ion exchange device 7 and the ultrapure water W1 at the outlet of the UF membrane separation device 8 is monitored.
- the number of fine particles of the treated water W2 of the non-regenerative type mixed bed ion exchanger 7 exceeds 10 / mL
- the result of repeating the operation of replacing the non-regenerative type mixed bed ion exchanger 7 is a result of the UF membrane separation device.
- the number of fine particles of the ultrapure water W1 at the outlet of 8 did not exceed 1 / mL. This is considered to be because the number of fine particles caused by colloidal silica or the like in the treated water W2 flowing into the UF membrane separation device 8 can be suppressed.
- Example 1 without measuring the number of fine particles of the treated water W2 of the non-regenerative mixed-bed ion exchanger 7, the specific resistance value is measured by a specific resistance meter, and the ion load is determined from the specific resistance value.
- the number of fine particles in the ultrapure water W1 at the outlet of the UF membrane separator 8 is one over time. The tendency which exceeded / mL was shown. This is presumably because the UF membrane separation device 8 was partially broken due to deterioration with time and colloidal silica leaked.
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- 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)
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
A sub-system 1 comprising: a sub-tank 2 for storing primary pure water W; a pump 4 provided at a base end portion of a supply line 3 for the primary pure water W stored in the tank 2; a heat exchanger 5 provided in the subsequent 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. In addition, a fine particle counter 9 which is a means for counting the number of fine particles is provided so as to be switchable 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. This fine particle management method for an ultrapure water production system can maintain the number of fine particles in ultrapure water to be reduced.
Description
本発明は、超純水製造システムの微粒子管理方法に関し、特に超純水中の微粒子数を低減化した状態に維持することの可能な超純水製造システムの微粒子管理方法に関する。
The present invention relates to a particle management method for an ultrapure water production system, and more particularly, to a particle management method for an ultrapure water production system that can maintain a reduced number of particles in ultrapure water.
電子産業分野で使用される超純水の製造装置は大きく分けて、工業用水や水道水など通常の水から濁質等を除去する前処理装置と、前処理装置の処理水を精製して大部分の不純物を除去した純水を製造する一次純水装置と、一次純水をさらに高度に精製して不純物をほぼ完全に除去した超純水を製造する二次純水装置（サブシステム）とからなる。
The ultrapure water production equipment used in the electronics industry is largely divided into a pretreatment device that removes turbidity from normal water such as industrial water and tap water, and a large amount of purified water from the pretreatment device. A primary pure water device for producing pure water from which impurities are partially removed, and a secondary pure water device (subsystem) for producing ultrapure water from which the primary pure water has been further refined to remove impurities completely. Consists of.
このうち、二次純水装置（サブシステム）は、基本的には有機物を分解する低圧紫外線（ＵＶ）照射酸化装置、イオン性不純物を吸着除去するイオン交換樹脂を充填した非再生型の混床式イオン交換装置及び微粒子を完全に除去するための限外濾過膜（ＵＦ膜）分離装置を基本構成として備え、水の純度をより一層高めて超純水にする。ここで、低圧ＵＶ照射酸化装置では、低圧ＵＶランプより出される波長１８５ｎｍの紫外線によりＴＯＣを有機酸さらにはＣＯ２にまで分解する。分解された有機酸及びＣＯ２は後段のイオン交換樹脂で除去される。ＵＦ膜分離装置では、イオン交換樹脂の流出粒子などの微小粒子が除去される。このように従来は、サブシステムの末端にＵＦ膜等の微粒子除去膜を設置することで、ナノメートルサイズの微粒子除去処理を行っていたが、近年、半導体製品の高性能化、微細化の進展に伴い、微粒子管理が厳しくなっており、例えば、半導体工場ではφ５０ｎｍ以上の粒子が１個／ｍＬ以下に管理値が設定されることも多い。このためサブシステムのＵＦ膜分離装置の出口で超純水中の微粒子数を測定し、管理することが行われている。
Of these, the secondary pure water device (subsystem) is basically a low-pressure ultraviolet (UV) irradiation oxidizer that decomposes organic matter, and a non-regenerative mixed bed filled with an ion exchange resin that adsorbs and removes ionic impurities. A basic ion exchange device and an ultrafiltration membrane (UF membrane) separation device for completely removing fine particles are provided as basic components, and the purity of water is further increased to ultrapure water. Here, in the low pressure UV irradiation oxidizer, TOC is decomposed into an organic acid and further to CO 2 by ultraviolet rays having a wavelength of 185 nm emitted from a low pressure UV lamp. The decomposed organic acid and CO 2 are removed by a subsequent ion exchange resin. In the UF membrane separator, fine particles such as outflow particles of the ion exchange resin are removed. Conventionally, nanometer-size fine particle removal processing has been performed by installing a fine particle removal film such as a UF membrane at the end of the subsystem. However, in recent years, semiconductor products have become more sophisticated and refined. Accordingly, the management of fine particles is becoming stricter. For example, in a semiconductor factory, the control value is often set to 1 particle / mL or less of particles having a diameter of 50 nm or more. For this reason, the number of fine particles in ultrapure water is measured and managed at the outlet of the UF membrane separator of the subsystem.
このサブシステムの代表的な例を図５に示す。図５において、サブシステム２１は、一次純水Ｗを貯留するためのサブタンク２２と、このタンク２２に貯留した一次純水Ｗの供給ライン２３の基端部に設けられたポンプ２４と、このポンプ２４の後段に設けられた熱交換器２５、低圧ＵＶ照射酸化装置２６、非再生型混床式イオン交換装置２７及びＵＦ膜分離装置２８とを有する。そして、ＵＦ膜分離装置２８の出口側にオフラインモニターとしての微粒子計（ＰＣ）２９が設けられている。
A typical example of this subsystem is shown in FIG. In FIG. 5, the sub-system 21 includes a sub tank 22 for storing the primary pure water W, a pump 24 provided at the base end portion of the supply line 23 of the primary pure water W stored in the tank 22, and the pump 24, a heat exchanger 25, a low-pressure UV irradiation oxidizer 26, a non-regenerative mixed bed ion exchanger 27, and a UF membrane separator 28 provided in the subsequent stage. A fine particle meter (PC) 29 as an off-line monitor is provided on the outlet side of the UF membrane separation device 28.
上述したようなサブシステム２１の運転中は、ポンプ２４を稼動して、サブタンク２２内の一次純水Ｗを熱交換器２５、低圧ＵＶ照射酸化装置２６、非再生型混床式イオン交換装置２７及びＵＦ膜分離装置２８に順次通水し、得られた超純水Ｗ１をユースポイントＰＯＵに送る。一方、ユースポイントＰＯＵで使用されなかった超純水Ｗ１は循環ライン２３Ａを経てサブタンク２２に返送され、再度処理される。
During the operation of the sub-system 21 as described above, the pump 24 is operated, and the primary pure water W in the sub-tank 22 is converted into the heat exchanger 25, the low-pressure UV irradiation oxidizer 26, and the non-regenerative mixed bed ion exchanger 27. And the UF membrane separator 28 are sequentially passed, and the obtained ultrapure water W1 is sent to the use point POU. On the other hand, the ultrapure water W1 that has not been used at the use point POU is returned to the sub tank 22 via the circulation line 23A and processed again.
従来の図５に示すようなサブシステム２１では、超純水Ｗ１中の微粒子数をＵＦ膜分離装置２８の出口側の微粒子計２９により管理する一方、非再生型混床式イオン交換装置２７は、その出口側のイオン負荷を導電率計や比抵抗計などにより計測し、これが所定の値よりも大きくなったら定期的に交換していた。しかしながら、このような管理方法によっても超純水Ｗ１中に微粒子がリークし、超純水Ｗ１中の微粒子数を低減化した状態に維持することができないことがある、という問題点があった。
In the conventional subsystem 21 as shown in FIG. 5, the number of fine particles in the ultrapure water W1 is managed by the fine particle meter 29 on the outlet side of the UF membrane separation device 28, while the non-regenerative mixed bed ion exchange device 27 The ion load on the outlet side was measured with a conductivity meter, a specific resistance meter or the like, and was periodically exchanged when it became larger than a predetermined value. However, even with such a management method, there is a problem that the fine particles leak into the ultrapure water W1 and the number of fine particles in the ultrapure water W1 may not be maintained.
本発明は上記問題点に鑑みてなされたものであり、超純水中の微粒子数を低減化した状態に維持することの可能な超純水製造システムの微粒子管理方法を提供することを目的とする。
The present invention has been made in view of the above problems, and an object thereof is to provide a method for managing fine particles of an ultrapure water production system capable of maintaining a state in which the number of fine particles in ultrapure water is reduced. To do.
上記目的に鑑み本発明は、一次純水システムで製造した一次純水を非再生型混床式イオン交換装置及び微粒子除去膜装置をこの順に備えたサブシステムで処理する超純水製造システムの微粒子管理方法であって、前記微粒子除去膜装置の出口の超純水中の微粒子数を微粒子数計測手段により計測することで監視する一方、前記非再生型混床式イオン交換装置の処理水の微粒子数を微粒子数計測手段により計測して、前記非再生型混床式イオン交換装置の処理水の微粒子数が所定の値を超えたら前記非再生型混床式イオン交換装置を交換する、超純水製造システムの微粒子管理方法を提供する（発明１）。
In view of the above-mentioned object, the present invention provides fine particles of an ultrapure water production system in which primary pure water produced by a primary pure water system is treated by a subsystem having a non-regenerative mixed bed ion exchange device and a fine particle removal membrane device in this order. A management method, wherein the number of fine particles in ultrapure water at the outlet of the fine particle removal membrane device is monitored by measuring the number of fine particles, and the treated water fine particles of the non-regenerative mixed bed ion exchange device A non-regenerative mixed bed ion exchanger is replaced when the number of treated water particles in the non-regenerative mixed bed ion exchanger exceeds a predetermined value. A fine particle management method for a water production system is provided (Invention 1).
かかる発明（発明１）によれば、非再生型混床式イオン交換装置の処理水の微粒子数を微粒子数計測手段により計測して管理することにより、微粒子除去膜装置の出口の超純水中の微粒子数を安定して低減化することが可能となる。これは以下のような理由によると推測される。すなわち、超純水中の微粒子を微粒子除去膜装置の出口側のみで管理した場合、微粒子除去膜装置から微粒子がリークした時点で微粒子の増加を検知することができるが、これでは基準値よりも微粒子数が増加した超純水が供給されるのを未然に防止することができない。そこで、本発明者らが非再生型混床式イオン交換装置の処理水の微粒子数と微粒子除去膜装置で処理して得られる超純水中の微粒子数の関連性を調査した結果、非再生型混床式イオン交換装置の処理水の微粒子数が増加すると、微粒子除去膜装置の出口の超純水に微粒子がリークしやすいことがわかった。そこで、この非再生型混床式イオン交換装置の処理水の微粒子の増加を管理するとともに、微粒子除去膜装置の出口の超純水中の微粒子数を確認することで、得られる超純水中の微粒子数を低減化した状態で安定して供給することができる。
According to this invention (Invention 1), by measuring and managing the number of fine particles of the treated water of the non-regenerative type mixed bed ion exchange device by the fine particle number measuring means, ultrapure water at the outlet of the fine particle removal membrane device It is possible to stably reduce the number of fine particles. This is presumed to be due to the following reasons. That is, when the fine particles in ultrapure water are managed only on the outlet side of the fine particle removal membrane device, the increase in fine particles can be detected when the fine particle leaks from the fine particle removal membrane device. The supply of ultrapure water having an increased number of fine particles cannot be prevented in advance. Therefore, as a result of investigating the relationship between the number of treated water particles in the non-regenerative mixed-bed ion exchanger and the number of particles in ultrapure water obtained by processing with the particle removal membrane device, the present inventors It was found that when the number of treated water particles in the mixed bed type ion exchanger increased, the particles easily leaked into the ultrapure water at the outlet of the particle removing membrane device. Therefore, by controlling the increase in the treated water particulates in this non-regenerative mixed bed ion exchange device, and confirming the number of particulates in the ultrapure water at the outlet of the particulate removal membrane device, Can be stably supplied with the number of fine particles reduced.
上記発明（発明１）においては、前記サブシステムが低圧紫外線（ＵＶ）照射酸化装置、非再生型混床式イオン交換装置及び前記微粒子除去膜装置としての限外濾過膜（ＵＦ膜）分離装置をこの順に備えることが好ましい（発明２）。また、上記発明（発明１）においては、前記サブシステムが低圧紫外線（ＵＶ）照射酸化装置、触媒樹脂（過酸化水素除去）装置、膜式脱気装置、非再生型混床式イオン交換装置及び前記微粒子除去膜装置としての限外濾過膜（ＵＦ膜）分離装置をこの順に備えることが好ましい（発明３）。さらに、上記発明（発明１）においては、前記サブシステムが低圧紫外線（ＵＶ）照射酸化装置、非再生型混床式イオン交換装置、膜式脱気装置及び前記微粒子除去膜装置としての限外濾過膜（ＵＦ膜）分離装置をこの順に備えることが好ましい（発明４）。
In the above invention (Invention 1), the subsystem includes a low-pressure ultraviolet (UV) irradiation oxidizer, a non-regenerative mixed bed ion exchanger, and an ultrafiltration membrane (UF membrane) separator as the particulate removal membrane device. It is preferable to prepare in this order (Invention 2). In the above invention (Invention 1), the subsystem is a low-pressure ultraviolet (UV) irradiation oxidizer, a catalyst resin (hydrogen peroxide removal) device, a membrane deaerator, a non-regenerative mixed bed ion exchanger, and It is preferable to provide an ultrafiltration membrane (UF membrane) separation device as the fine particle removal membrane device in this order (Invention 3). Furthermore, in the said invention (invention 1), the said subsystem is ultrafiltration as a low-pressure ultraviolet-ray (UV) irradiation oxidation apparatus, a non-regenerative mixed bed type ion exchange apparatus, a membrane-type deaeration apparatus, and the said fine particle removal membrane apparatus. It is preferable to provide a membrane (UF membrane) separation device in this order (Invention 4).
かかる発明（発明２～４）によれば、限外濾過膜（ＵＦ膜）分離装置の前段に配置された非再生型混床式イオン交換装置は、ナトリウムや塩素などのイオンに比べてコロイダルシリカなどの微粒子が破過しやすく、この微粒子が限外濾過膜（ＵＦ膜）分離装置の破断部分から流出して超純水中の微粒子数の増加をきたすので、非再生型混床式イオン交換装置の処理水の微粒子数を管理して該微粒子数が所定の値を上回ったら、非再生型混床式イオン交換装置を交換して、微粒子除去膜装置の出口の超純水中の微粒子数を確認することで、微粒子数が増加した超純水が供給されるのを未然に防止することができる。
According to such inventions (Inventions 2 to 4), the non-regenerative mixed bed type ion exchange device arranged in the front stage of the ultrafiltration membrane (UF membrane) separator is colloidal silica compared to ions such as sodium and chlorine. And so on, and the fine particles flow out from the ruptured part of the ultrafiltration membrane (UF membrane) separator and increase the number of fine particles in ultrapure water. When the number of fine particles in the treated water of the apparatus is controlled and the number of fine particles exceeds 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 apparatus By confirming the above, it is possible to prevent the ultrapure water having an increased number of fine particles from being supplied.
上記発明（発明１～４）においては、前記微粒子数計測手段が微粒子計であり、前記非再生型混床式イオン交換装置の処理水の微粒子数と前記微粒子除去膜装置の出口の超純水中の微粒子数とを１台の微粒子計を切り替えることで計測することが好ましい（発明５）。
In the above inventions (Inventions 1 to 4), the particle number measuring means is a particle meter, and the number of treated water particles in the non-regenerative mixed bed ion exchanger and the ultrapure water at the outlet of the particle removal membrane device It is preferable to measure the number of particles inside by switching one particle meter (Invention 5).
かかる発明（発明５）によれば、１台の微粒子計で非再生型混床式イオン交換装置の処理水の微粒子数と微粒子除去膜装置の出口の超純水中の微粒子数とを計測することができる。
According to this invention (Invention 5), the number of treated water particles in the non-regenerative mixed bed ion exchanger and the number of particles in ultrapure water at the outlet of the particle removal membrane device are measured with one particle meter. be able to.
上記発明（発明１～４）においては、前記微粒子数計測手段が微粒子計であり、前記非再生型混床式イオン交換装置の出口側及び前記微粒子除去膜装置の出口側にそれぞれ微粒子計を設けて、前記非再生型混床式イオン交換装置の処理水の微粒子数及び前記微粒子除去膜装置の出口の超純水中の微粒子数をそれぞれ計測することが好ましい（発明６）。
In the above inventions (Inventions 1 to 4), the fine particle number measuring means is a fine particle meter, and a 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. Thus, it is preferable to measure the number of treated water particles in the non-regenerative mixed bed ion exchanger and the number of particles in ultrapure water at the outlet of the particle removing membrane device (Invention 6).
かかる発明（発明６）によれば、非再生型混床式イオン交換装置の処理水の微粒子数と微粒子除去膜装置の出口の超純水中の微粒子数をそれぞれ独立して計測することができる。
According to this invention (Invention 6), the number of treated water particles in the non-regenerative mixed bed ion exchanger and the number of particles in ultrapure water at the outlet of the particle removing membrane device can be measured independently. .
本発明は、非再生型混床式イオン交換装置の処理水の微粒子数を計測して、該微粒子数が所定の値を超えたら非再生型混床式イオン交換装置を交換して、微粒子除去膜装置の出口の超純水中の微粒子数を確認することで、微粒子数が増加した超純水が供給されるのを未然に防止することができる。
The present invention measures the number of fine particles of treated water in a non-regenerative type mixed bed type ion exchange device, and when the number of fine particles exceeds a predetermined value, replaces the non-regenerative type mixed bed type ion exchange device to remove fine particles. By confirming the number of fine particles in the ultrapure water at the outlet of the membrane device, it is possible to prevent the supply of ultrapure water having an increased number of fine particles.
以下、本発明の第一の実施形態による超純水製造システムの微粒子管理方法について図１を参照にして詳細に説明する。
Hereinafter, the fine particle management method of the ultrapure water production system according to the first embodiment of the present invention will be described in detail with reference to FIG.
本実施形態の超純水製造システムの微粒子管理方法を適用可能なサブシステムは、前述した図５に示すものと基本的には同じ構成を有する。すなわち、図１において、サブシテム１は、一次純水Ｗを貯留するためのサブタンク２と、このサブタンク２に貯留した一次純水Ｗの供給ライン３の基端部に設けられたポンプ４と、このポンプ４の後段に設けられた熱交換器５、低圧ＵＶ照射酸化装置６、非再生型混床式イオン交換装置７及び微粒子除去膜装置としての限外濾過膜（ＵＦ膜）分離装置８とを有する。そして、ＵＦ膜分離装置８の出口側と非再生型混床式イオン交換装置７の出口側にそれぞれ切替可能に微粒子数を計測する手段である微粒子計（ＰＣ）９が接続されている。この微粒子計９としては、栗田工業社製「Ｋ－ＬＡＭＩＣ」（商品名）、ＰＭＳ社製「ＵＤＩ－５０」（商品名）などを用いることができる。
The subsystem to which the particulate management method of the ultrapure water production system of the present embodiment can be applied has basically the same configuration as that shown in FIG. That is, in FIG. 1, the sub-system 1 includes a sub-tank 2 for storing the primary pure water W, a pump 4 provided at the base end portion of the supply line 3 of the primary pure water W stored in the sub-tank 2, A heat exchanger 5, a low-pressure UV irradiation oxidizer 6, a non-regenerative mixed bed ion exchanger 7, and an ultrafiltration membrane (UF membrane) separator 8 as a fine particle removal membrane device provided at the subsequent stage of the pump 4. Have. A fine particle meter (PC) 9 is connected 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 to measure the number of fine particles in a switchable manner. As the fine particle counter 9, “K-LAMIC” (trade name) manufactured by Kurita Kogyo Co., Ltd., “UDI-50” (trade name) manufactured by PMS, etc. can be used.
上述したようなサブシステム１の運転時には、ポンプ４を稼動してサブタンク２内の一次純水Ｗを熱交換器５、低圧ＵＶ照射酸化装置６、非再生型混床式イオン交換装置７に順次通水し、非再生型混床式イオン交換装置７の処理水Ｗ２をＵＦ膜分離装置８に通水して超純水Ｗ１を得る。そして、得られた超純水Ｗ１をユースポイントＰＯＵに供給する。一方、ユースポイントＰＯＵで使用されなかった超純水Ｗ１は循環ライン３Ａを経てサブタンク２に返送され、再度処理される。
During the operation of the sub-system 1 as described above, the pump 4 is operated and the primary pure water W in the sub-tank 2 is sequentially transferred to the heat exchanger 5, the low-pressure UV irradiation oxidizer 6, and the non-regenerative mixed bed ion exchanger 7. Water is passed through and the treated water W2 of the non-regenerative mixed bed ion exchange device 7 is passed through the UF membrane separation device 8 to obtain ultrapure water W1. Then, the obtained ultrapure water W1 is supplied to the use point POU. On the other hand, the ultrapure water W1 that has not been used at the use point POU is returned to the sub tank 2 via the circulation line 3A and is processed again.
なお、本実施形態における超純水Ｗ１としては、抵抗率：１８．１ＭΩ・ｃｍ以上、微粒子：粒径５０ｎｍ以上で１０００個／Ｌ以下、生菌：１個／Ｌ以下、ＴＯＣ（Ｔｏｔａｌ Ｏｒｇａｎｉｃ Ｃａｒｂｏｎ）：１μｇ／Ｌ以下、全シリコン：０．１μｇ／Ｌ以下、金属類：１ｎｇ／Ｌ以下、イオン類：１０ｎｇ／Ｌ以下、過酸化水素；３０μｇ／Ｌ以下、水温：２５±２℃のものが好適である。
In addition, as the ultrapure water W1 in the present embodiment, resistivity: 18.1 MΩ · cm or more, fine particles: particle size of 50 nm or more and 1000 / L or less, viable bacteria: 1 / L or less, TOC (Total Organic Carbon ): 1 μg / L or less, Total silicon: 0.1 μg / L or less, Metals: 1 ng / L or less, Ions: 10 ng / L or less, Hydrogen peroxide: 30 μg / L or less, Water temperature: 25 ± 2 ° C. Is preferred.
次にこのような超純水製造システムの微粒子管理方法について説明する。
［通常時運転］
上述したような超純水の製造工程において、微粒子計９をＵＦ膜分離装置８の出口側と非再生型混床式イオン交換装置７の出口側とにそれぞれ所定のタイミングで適宜切り替えることで、ＵＦ膜分離装置８の出口側の超純水Ｗ１の微粒子数と、非再生型混床式イオン交換装置７の処理水Ｗ２の微粒子数を測定する。そして、超純水Ｗ１の微粒子数が１個／ｍＬ以下であり、非再生型混床式イオン交換装置７の処理水Ｗ２の微粒子数が１０個／ｍＬ以下であれば、サブシテム１の運転を継続して、超純水Ｗ１をユースポイントＰＯＵへ供給する。 Next, a particle management method for such an ultrapure water production system will be described.
[Normal operation]
In the manufacturing process of ultrapure water as described above, thefine particle counter 9 is appropriately switched 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 at predetermined timings, The number of fine particles of the ultrapure water W1 on the outlet side of the UF membrane separation device 8 and the number of fine particles of the treated water W2 of the non-regenerative mixed bed ion exchange device 7 are measured. If the number of fine particles in the ultrapure water W1 is 1 / mL or less and the number of particles in the treated water W2 of the non-regenerative mixed bed ion exchange apparatus 7 is 10 / mL or less, the operation of the sub-system 1 is performed. Continue to supply ultrapure water W1 to the use point POU.
［通常時運転］
上述したような超純水の製造工程において、微粒子計９をＵＦ膜分離装置８の出口側と非再生型混床式イオン交換装置７の出口側とにそれぞれ所定のタイミングで適宜切り替えることで、ＵＦ膜分離装置８の出口側の超純水Ｗ１の微粒子数と、非再生型混床式イオン交換装置７の処理水Ｗ２の微粒子数を測定する。そして、超純水Ｗ１の微粒子数が１個／ｍＬ以下であり、非再生型混床式イオン交換装置７の処理水Ｗ２の微粒子数が１０個／ｍＬ以下であれば、サブシテム１の運転を継続して、超純水Ｗ１をユースポイントＰＯＵへ供給する。 Next, a particle management method for such an ultrapure water production system will be described.
[Normal operation]
In the manufacturing process of ultrapure water as described above, the
［微粒子数管理運転］
一方、オフラインモニターである微粒子計９で計測されたＵＦ膜分離装置８の出口側の超純水Ｗ１の微粒子数が１個／ｍＬ以下であっても、非再生型混床式イオン交換装置７の処理水Ｗ２の微粒子数が１０個／ｍＬを超えたら、サブシテム１の運転を一旦停止し、非再生型混床式イオン交換装置７を交換する。これによりＵＦ膜分離装置８の出口側の超純水Ｗ１の微粒子数を１個／ｍＬ以下に保持することができ、微粒子数が基準値を超えた超純水Ｗ１がユースポイントＰＯＵへ供給されるのを未然に防止することができる。なお、このような管理を行ってもＵＦ膜分離装置８の出口側の超純水Ｗ１の微粒子数が１個／ｍＬを超える場合には、ＵＦ膜分離装置８に破断が生じたと判断して、ＵＦ膜分離装置８を交換するなどすればよい。 [Particle count control]
On the other hand, even if the number of fine particles in the ultrapure water W1 on the outlet side of the UFmembrane separation device 8 measured by the fine particle meter 9 which is an offline monitor is 1 / mL or less, the non-regenerative mixed bed ion exchange device 7 is used. When the number of fine particles in the treated water W2 exceeds 10 / mL, the operation of the sub-system 1 is temporarily stopped, and the non-regenerative mixed bed ion exchanger 7 is replaced. As a result, the number of fine particles of the ultrapure water W1 on the outlet side of the UF membrane separation device 8 can be maintained at 1 / mL or less, and the ultrapure water W1 with the number of fine particles exceeding the reference value is supplied to the use point POU. Can be prevented in advance. Even if such management is performed, if the number of fine particles of the ultrapure water W1 on the outlet side of the UF membrane separator 8 exceeds 1 / mL, it is determined that the UF membrane separator 8 has been broken. The UF membrane separation device 8 may be replaced.
一方、オフラインモニターである微粒子計９で計測されたＵＦ膜分離装置８の出口側の超純水Ｗ１の微粒子数が１個／ｍＬ以下であっても、非再生型混床式イオン交換装置７の処理水Ｗ２の微粒子数が１０個／ｍＬを超えたら、サブシテム１の運転を一旦停止し、非再生型混床式イオン交換装置７を交換する。これによりＵＦ膜分離装置８の出口側の超純水Ｗ１の微粒子数を１個／ｍＬ以下に保持することができ、微粒子数が基準値を超えた超純水Ｗ１がユースポイントＰＯＵへ供給されるのを未然に防止することができる。なお、このような管理を行ってもＵＦ膜分離装置８の出口側の超純水Ｗ１の微粒子数が１個／ｍＬを超える場合には、ＵＦ膜分離装置８に破断が生じたと判断して、ＵＦ膜分離装置８を交換するなどすればよい。 [Particle count control]
On the other hand, even if the number of fine particles in the ultrapure water W1 on the outlet side of the UF
＜作用機構＞
このような効果が得られるのは以下のような作用機構による。すなわち、一般にイオン交換装置では、溶解性シリカは非常に除去しやすいのに対し、コロイダルシリカはホウ素よりも非常に除去しにくい（破過しやすい）ことが報告されている（「ＵＰＷ Ｍｉｃｒｏ ２０１７，ＵＰＷ ＩＲＤＳ ａｎｄ ＳＥＭＩ ｕｐｄａｔｅ」Ｓｌａｖａ Ｌｉｂｍａnら）。そして、このホウ素は、一次純水Ｗ中に含まれているナトリウムイオン（Ｎａ＋）、塩素イオン（Ｃｌ－）あるいは炭酸イオン（ＨＣＯ３ －）よりも非常に除去しにくい（破過しやすい）。すなわち、コロイダルシリカは、ナトリウムイオン（Ｎａ＋）、塩素イオン（Ｃｌ－）、炭酸イオン（ＨＣＯ３ －）よりもはるかに破過しやすいことになる。 <Action mechanism>
Such an effect is obtained by the following mechanism. That is, it is generally reported that in an ion exchange apparatus, soluble silica is very easy to remove, whereas colloidal silica is much more difficult to remove (easy to break through) than boron ("UPW Micro 2017, UPW IRDS and SEMI update "Slava Libman et al.). This boron is much more difficult to remove (easy to break through) than sodium ions (Na + ), chlorine ions (Cl − ) or carbonate ions (HCO 3 − ) contained in the primary pure water W. . That is, colloidal silica is much easier to break through than sodium ions (Na + ), chlorine ions (Cl − ), and carbonate ions (HCO 3 − ).
このような効果が得られるのは以下のような作用機構による。すなわち、一般にイオン交換装置では、溶解性シリカは非常に除去しやすいのに対し、コロイダルシリカはホウ素よりも非常に除去しにくい（破過しやすい）ことが報告されている（「ＵＰＷ Ｍｉｃｒｏ ２０１７，ＵＰＷ ＩＲＤＳ ａｎｄ ＳＥＭＩ ｕｐｄａｔｅ」Ｓｌａｖａ Ｌｉｂｍａnら）。そして、このホウ素は、一次純水Ｗ中に含まれているナトリウムイオン（Ｎａ＋）、塩素イオン（Ｃｌ－）あるいは炭酸イオン（ＨＣＯ３ －）よりも非常に除去しにくい（破過しやすい）。すなわち、コロイダルシリカは、ナトリウムイオン（Ｎａ＋）、塩素イオン（Ｃｌ－）、炭酸イオン（ＨＣＯ３ －）よりもはるかに破過しやすいことになる。 <Action mechanism>
Such an effect is obtained by the following mechanism. That is, it is generally reported that in an ion exchange apparatus, soluble silica is very easy to remove, whereas colloidal silica is much more difficult to remove (easy to break through) than boron ("UPW Micro 2017, UPW IRDS and SEMI update "Slava Libman et al.). This boron is much more difficult to remove (easy to break through) than sodium ions (Na + ), chlorine ions (Cl − ) or carbonate ions (HCO 3 − ) contained in the primary pure water W. . That is, colloidal silica is much easier to break through than sodium ions (Na + ), chlorine ions (Cl − ), and carbonate ions (HCO 3 − ).
そこで、本発明者らが検討した結果、非再生型混床式イオン交換装置７の出口側、すなわちＵＦ膜分離装置８の入口側における微粒子数の増加は、主にコロイダルシリカ粒子に起因することがわかった。従来、非再生型混床式イオン交換装置７は、その出口側に導電率計や比抵抗計などのイオン負荷を計測する手段を設けてイオン負荷を計測し、これが所定の値よりも大きくなったら定期的に交換していたが、これではコロイダルシリカの微粒子はＵＦ膜分離装置８に流入してしまう。これに対し本実施形態のように非再生型混床式イオン交換装置７の処理水の微粒子数に視点をおいて管理することで、微粒子がＵＦ膜分離装置８の出口に到達する前に非再生型混床式イオン交換装置７を交換することができるので、ＵＦ膜分離装置８の出口における超純水Ｗ１の微粒子数の安定化を図ることができる。そして、超純水Ｗ１の微粒子数が増加しないことを微粒子計９により計測して確認すればよい。
Therefore, as a result of the study by the present inventors, the increase in the number of fine particles on the outlet side of the non-regenerative mixed bed ion exchange device 7, that is, the inlet side of the UF membrane separation device 8 is mainly caused by colloidal silica particles. I understood. Conventionally, the non-regenerative mixed bed ion exchange apparatus 7 is provided with means for measuring an ion load such as a conductivity meter and a specific resistance meter on the outlet side thereof to measure the ion load, which becomes larger than a predetermined value. However, the colloidal silica particles flow into the UF membrane separation device 8. On the other hand, by controlling the number of treated water fine particles in the non-regenerative mixed bed ion exchange device 7 as in the present embodiment, it is possible to control the fine particles before they reach the outlet of the UF membrane separation device 8. Since the regenerative mixed bed type ion exchange device 7 can be exchanged, the number of fine particles of the ultrapure water W1 at the outlet of the UF membrane separation device 8 can be stabilized. Then, it may be confirmed by measuring with the fine particle meter 9 that the number of fine particles of the ultrapure water W1 does not increase.
以上、本発明の第一の実施形態について添付図面を参照して説明してきたが、本発明は前記実施形態に限らず種々の変更実施が可能である。例えば、図２に示すようにＵＦ膜分離装置８の出口側に第一の微粒子計９Ａを設けるとともに非再生型混床式イオン交換装置７の出口側に第二の微粒子計９Ｂを設けて、非再生型混床式イオン交換装置７の処理水Ｗ２の微粒子数と、ＵＦ膜分離装置８の出口の超純水Ｗ１の微粒子数とをそれぞれ独立して計測する構成としても良い。また、微粒子数計測手段は、微粒子計９などはオフラインモニターでなく、遠心ろ過法を利用したオンラインモニターとしても良い。
As mentioned above, although 1st embodiment of this invention has been described with reference to an accompanying drawing, this invention is not restricted to the said embodiment, A various change implementation is possible. For example, as shown in FIG. 2, the first particle counter 9A is provided on the outlet side of the UF membrane separation device 8 and the second particle counter 9B is provided on the outlet side of the non-regenerative mixed bed ion exchanger 7. A configuration may be employed in which the number of fine particles in the treated water W2 of the non-regenerative mixed bed ion exchange device 7 and the number of fine particles in the ultrapure water W1 at the outlet of the UF membrane separation device 8 are independently measured. In addition, as for the fine particle count measuring means, the fine particle counter 9 and the like may be an online monitor using a centrifugal filtration method instead of an offline monitor.
また、サブシステム１としては、前述した第一及び第二の実施形態のものに限らず種々のサブシステムに適用可能である。例えば、図３に示すように低圧紫外線（ＵＶ）照射酸化装置６の後段に白金族金属などを担持したイオン交換樹脂を充填した触媒樹脂（過酸化水素除去）装置１０、膜式脱気装置１１を設け、その後段に非再生型混床式イオン交換装置７及び限外濾過膜（ＵＦ膜）分離装置８をこの順に備えるものにも好適に適用可能である。さらに、サブシステム１として、例えば、図４に示すように非再生型混床式イオン交換装置７と限外濾過膜（ＵＦ膜）分離装置８の間に膜式脱気装置１２を設けたものにも好適に適用可能である。この場合、微粒子計９などの微粒子数計測手段は、非再生型混床式イオン交換装置７の出口側でＵＦ膜分離装置８より前であれば、膜式脱気装置１２などの他のエレメントが介在していてもよく、その場合、他のエレメントの出口側で微粒子数を計測してもよいし、非再生型混床式イオン交換装置７の直後で計測してもよい。
Further, the subsystem 1 is not limited to those of the first and second embodiments described above, and can be applied to various subsystems. For example, as shown in FIG. 3, a catalyst resin (hydrogen peroxide removal) device 10 and a membrane type deaeration device 11 in which an ion exchange resin carrying a platinum group metal or the like is placed downstream of the low pressure ultraviolet (UV) irradiation oxidizer 6. And a non-regenerative mixed bed ion exchange device 7 and an ultrafiltration membrane (UF membrane) separation device 8 in this order can be suitably applied. Further, as the subsystem 1, for example, as shown in FIG. 4, a membrane deaerator 12 is provided between a non-regenerative mixed bed ion exchanger 7 and an ultrafiltration membrane (UF membrane) separator 8 It can be suitably applied to. In this case, if the particle number measuring means such as the particle counter 9 is in front of the UF membrane separation device 8 on the outlet side of the non-regenerative mixed bed ion exchange device 7, other elements such as the membrane deaeration device 12 are used. In such a case, the number of fine particles may be measured at the outlet side of another element, or may be measured immediately after the non-regenerative mixed bed ion exchange device 7.
以下の具体的実施例により本発明をさらに詳細に説明する。
The present invention will be described in more detail by the following specific examples.
［実験例１］
図１に示す超純水製造システムにより、市水を原水として超純水の製造を行った。なお、サブシステム１を構成する低圧ＵＶ照射酸化装置６としては日本フォトサイエンス社製品を、非再生型混床式イオン交換装置７としては栗田工業社製「ＫＲ－ＦＭ」を、ＵＦ膜分離装置８としては栗田工業社製「ＫＵ－１５１０－ＨＰ－Ｈ」を、微粒子計９としては栗田工業社製「Ｋ－ＬＡＭＩＣ」をそれぞれ使用した。 [Experimental Example 1]
The ultrapure water production system shown in FIG. 1 was used to produce ultrapure water using city water as raw water. The low pressureUV irradiation oxidizer 6 constituting the subsystem 1 is a product of Japan Photoscience, the non-regenerative mixed bed ion exchanger 7 is “KR-FM” manufactured by Kurita Kogyo Co., Ltd., and a UF membrane separator. “KU-1510-HP-H” manufactured by Kurita Kogyo Co., Ltd. was used as 8, and “K-LAMIC” manufactured by Kurita Kogyo Co., Ltd. was used as the fine particle counter 9.
図１に示す超純水製造システムにより、市水を原水として超純水の製造を行った。なお、サブシステム１を構成する低圧ＵＶ照射酸化装置６としては日本フォトサイエンス社製品を、非再生型混床式イオン交換装置７としては栗田工業社製「ＫＲ－ＦＭ」を、ＵＦ膜分離装置８としては栗田工業社製「ＫＵ－１５１０－ＨＰ－Ｈ」を、微粒子計９としては栗田工業社製「Ｋ－ＬＡＭＩＣ」をそれぞれ使用した。 [Experimental Example 1]
The ultrapure water production system shown in FIG. 1 was used to produce ultrapure water using city water as raw water. The low pressure
上記超純水の製造システムでの超純水の製造工程において、非再生型混床式イオン交換装置７の処理水Ｗ２及びＵＦ膜分離装置８の出口の超純水Ｗ１の微粒子数を監視し、非再生型混床式イオン交換装置７の処理水Ｗ２の微粒子数が１０個／ｍＬを超えたら、非再生型混床式イオン交換装置７を交換する作業を繰り返した結果、ＵＦ膜分離装置８の出口の超純水Ｗ１の微粒子数が１個／ｍＬを超えることはなかった。これはＵＦ膜分離装置８への流入する処理水Ｗ２中のコロイダルシリカなどに起因する微粒子数を抑制することができるためであると考えられる。
In the ultrapure water production process in the ultrapure water production system, the number of fine particles in the treated water W2 of the non-regenerative mixed bed ion exchange device 7 and the ultrapure water W1 at the outlet of the UF membrane separation device 8 is monitored. When the number of fine particles of the treated water W2 of the non-regenerative type mixed bed ion exchanger 7 exceeds 10 / mL, the result of repeating the operation of replacing the non-regenerative type mixed bed ion exchanger 7 is a result of the UF membrane separation device. The number of fine particles of the ultrapure water W1 at the outlet of 8 did not exceed 1 / mL. This is considered to be because the number of fine particles caused by colloidal silica or the like in the treated water W2 flowing into the UF membrane separation device 8 can be suppressed.
［比較例１］
実施例１において、非再生型混床式イオン交換装置７の処理水Ｗ２の微粒子数を計測することなく、比抵抗計により比抵抗値を測定し、この比抵抗値からイオン負荷を判断し、イオン負荷が所定の値を超えたら非再生型混床式イオン交換装置７を交換する作業を繰り返した結果、ＵＦ膜分離装置８の出口の超純水Ｗ１の微粒子数が時間の経過とともに１個／ｍＬを超える傾向を示した。これはＵＦ膜分離装置８の経時劣化により部分的に破断が生じ、コロイダルシリカがリークしたためであると考えられる。 [Comparative Example 1]
In Example 1, without measuring the number of fine particles of the treated water W2 of the non-regenerative mixed-bed ion exchanger 7, the specific resistance value is measured by a specific resistance meter, and the ion load is determined from the specific resistance value. As a result of repeating the operation of replacing the non-regenerative mixed bed ion exchanger 7 when the ion load exceeds a predetermined value, the number of fine particles in the ultrapure water W1 at the outlet of the UF membrane separator 8 is one over time. The tendency which exceeded / mL was shown. This is presumably because the UF membrane separation device 8 was partially broken due to deterioration with time and colloidal silica leaked.
実施例１において、非再生型混床式イオン交換装置７の処理水Ｗ２の微粒子数を計測することなく、比抵抗計により比抵抗値を測定し、この比抵抗値からイオン負荷を判断し、イオン負荷が所定の値を超えたら非再生型混床式イオン交換装置７を交換する作業を繰り返した結果、ＵＦ膜分離装置８の出口の超純水Ｗ１の微粒子数が時間の経過とともに１個／ｍＬを超える傾向を示した。これはＵＦ膜分離装置８の経時劣化により部分的に破断が生じ、コロイダルシリカがリークしたためであると考えられる。 [Comparative Example 1]
In Example 1, without measuring the number of fine particles of the treated water W2 of the non-regenerative mixed-
１ サブシテム
２ サブタンク
３ 供給ライン
３Ａ 循環ライン
４ ポンプ
５ 熱交換器
６ 低圧紫外線（ＵＶ）照射酸化装置
７ 非再生型混床式イオン交換装置
８ 限外濾過膜（ＵＦ膜）分離装置（微粒子除去膜装置）
９，９Ａ，９Ｂ 微粒子計（微粒子数計測手段）
ＰＯＵ ユースポイント
Ｗ 一次純水
Ｗ１ 超純水
Ｗ２ 非再生型混床式イオン交換装置の処理水 DESCRIPTION OFSYMBOLS 1 Subsystem 2 Subtank 3 Supply line 3A Circulation line 4 Pump 5 Heat exchanger 6 Low pressure ultraviolet (UV) irradiation oxidation apparatus 7 Non-regenerative mixed bed type ion exchange apparatus 8 Ultrafiltration membrane (UF membrane) separation device (fine particle removal membrane) apparatus)
9, 9A, 9B Fine particle meter (particle number measuring means)
POU use point W Primary pure water W1 Ultra pure water W2 Non-regenerative mixed-bed ion exchanger treated water
２ サブタンク
３ 供給ライン
３Ａ 循環ライン
４ ポンプ
５ 熱交換器
６ 低圧紫外線（ＵＶ）照射酸化装置
７ 非再生型混床式イオン交換装置
８ 限外濾過膜（ＵＦ膜）分離装置（微粒子除去膜装置）
９，９Ａ，９Ｂ 微粒子計（微粒子数計測手段）
ＰＯＵ ユースポイント
Ｗ 一次純水
Ｗ１ 超純水
Ｗ２ 非再生型混床式イオン交換装置の処理水 DESCRIPTION OF
9, 9A, 9B Fine particle meter (particle number measuring means)
POU use point W Primary pure water W1 Ultra pure water W2 Non-regenerative mixed-bed ion exchanger treated water
Claims (6)
- 一次純水システムで製造した一次純水を非再生型混床式イオン交換装置及び微粒子除去膜装置をこの順に備えたサブシステムで処理する超純水製造システムの微粒子管理方法であって、
前記微粒子除去膜装置の出口の超純水中の微粒子数を微粒子数計測手段により計測することで監視する一方、
前記非再生型混床式イオン交換装置の処理水の微粒子数を微粒子数計測手段により計測して、前記非再生型混床式イオン交換装置の処理水の微粒子数が所定の値を超えたら前記非再生型混床式イオン交換装置を交換する、
超純水製造システムの微粒子管理方法。 A method for managing fine particles of an ultrapure water production system in which primary pure water produced by a primary pure water system is processed by a subsystem comprising a non-regenerative mixed bed ion exchange device and a fine particle removal membrane device in this order,
While monitoring the number of fine particles in ultrapure water at the outlet of the fine particle removal film device by measuring the number of fine particles,
When the number of fine particles of treated water of the non-regenerative type mixed bed ion exchange apparatus is measured by a fine particle number measuring means, and the number of fine particles of treated water of the non-regenerative type mixed bed ion exchange apparatus exceeds a predetermined value, Replacing the non-regenerative mixed bed ion exchanger
Particle management method for ultrapure water production system. - 前記サブシステムが低圧紫外線（ＵＶ）照射酸化装置、非再生型混床式イオン交換装置及び前記微粒子除去膜装置としての限外濾過膜（ＵＦ膜）分離装置をこの順に備える、請求項１に記載の超純水製造システムの微粒子管理方法。 The sub-system includes a low-pressure ultraviolet (UV) irradiation oxidizer, a non-regenerative mixed-bed ion exchanger, and an ultrafiltration membrane (UF membrane) separator as the particulate removal membrane device in this order. Particle management method for ultrapure water production system.
- 前記サブシステムが低圧紫外線（ＵＶ）照射酸化装置、触媒樹脂（過酸化水素除去）装置、膜式脱気装置、非再生型混床式イオン交換装置及び前記微粒子除去膜装置としての限外濾過膜（ＵＦ膜）分離装置をこの順に備える、請求項１に記載の超純水製造システムの微粒子管理方法。 The sub-system is a low-pressure ultraviolet (UV) irradiation oxidizer, a catalyst resin (hydrogen peroxide removal) device, a membrane deaeration device, a non-regenerative mixed bed ion exchange device, and an ultrafiltration membrane as the particulate removal membrane device The fine particle management method for an ultrapure water production system according to claim 1, comprising a (UF membrane) separation device in this order.
- 前記サブシステムが低圧紫外線（ＵＶ）照射酸化装置、非再生型混床式イオン交換装置、膜式脱気装置及び前記微粒子除去膜装置としての限外濾過膜（ＵＦ膜）分離装置をこの順に備える、請求項１に記載の超純水製造システムの微粒子管理方法。 The subsystem includes a low-pressure ultraviolet (UV) irradiation oxidizer, a non-regenerative mixed bed ion exchanger, a membrane deaerator, and an ultrafiltration membrane (UF membrane) separator as the particulate removal membrane device in this order. The fine particle management method of the ultrapure water production system according to claim 1.
- 前記微粒子数計測手段が微粒子計であり、前記非再生型混床式イオン交換装置の処理水の微粒子数と前記微粒子除去膜装置の出口の超純水中の微粒子数とを１台の微粒子計を切り替えることで計測する、請求項１～４のいずれか一項に記載の超純水製造システムの微粒子管理方法。 The fine particle number measuring means is a fine particle meter, and the number of fine particles in treated water of the non-regenerative mixed bed ion exchange device and the number of fine particles in ultrapure water at the outlet of the fine particle removal membrane device are set as one fine particle meter. The method for managing fine particles in an ultrapure water production system according to any one of claims 1 to 4, wherein the measurement is performed by switching between the two.
- 前記微粒子数計測手段が微粒子計であり、前記非再生型混床式イオン交換装置の出口側及び前記微粒子除去膜装置の出口側にそれぞれ微粒子計を設けて、前記非再生型混床式イオン交換装置の処理水の微粒子数及び前記微粒子除去膜装置の出口の超純水中の微粒子数をそれぞれ計測する、請求項１～４のいずれか一項に記載の超純水製造システムの微粒子管理方法。 The fine particle number measuring means is a fine particle meter, and a non-regenerative mixed bed ion exchange is provided by providing a fine particle meter on each of an outlet side of the non-regenerative type mixed bed ion exchange device and an outlet side of the fine particle removal membrane device. The method for managing fine particles in an ultrapure water production system according to any one of claims 1 to 4, wherein the number of fine particles of treated water in the apparatus and the number of fine particles in ultrapure water at the outlet of the fine particle removal membrane device are respectively measured. .
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| 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 |
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