WO2022168570A1 - Dispositif d'échange d'ions et appareil de production d'eau ultrapure - Google Patents

Dispositif d'échange d'ions et appareil de production d'eau ultrapure Download PDF

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Publication number
WO2022168570A1
WO2022168570A1 PCT/JP2022/001262 JP2022001262W WO2022168570A1 WO 2022168570 A1 WO2022168570 A1 WO 2022168570A1 JP 2022001262 W JP2022001262 W JP 2022001262W WO 2022168570 A1 WO2022168570 A1 WO 2022168570A1
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WIPO (PCT)
Prior art keywords
ion exchange
container
exchange device
exchange resin
metallic material
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Ceased
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PCT/JP2022/001262
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English (en)
Japanese (ja)
Inventor
晃彦 津田
恭平 蔦野
俊裕 中村
広 菅原
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Organo Corp
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Organo Corp
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Publication date
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Publication of WO2022168570A1 publication Critical patent/WO2022168570A1/fr
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    • 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

Definitions

  • the present invention relates to an ion exchange device and an ultrapure water production device.
  • ultrapure water In the manufacturing process of semiconductor devices and liquid crystal devices, ultrapure water from which impurities have been highly removed is used for various purposes such as cleaning processes. Even a very small amount of metal components contained in ultrapure water has a great effect on the characteristics of the device, so strict control of the concentration is required. In recent years, with the rapid increase in integration and miniaturization of semiconductor devices, the requirements for metal concentration in ultrapure water have become more and more stringent, and ultrapure water with a metal concentration of pg/L level is required. . Ultrapure water is generally produced by sequentially treating raw water (river water, groundwater, industrial water, etc.) with a pretreatment system, a primary pure water system, and a secondary pure water system (subsystem).
  • Patent Documents 1 and 2 It is known that metal components are eluted from pipes and pumps used during the manufacturing process. Therefore, in the ultrapure water production apparatus having the system described above, several proposals have been made to minimize the influence of elution of metal components (see, for example, Patent Documents 1 and 2).
  • Some of the subsystems described above are equipped with an ion exchange resin tower (ion exchange device) filled with ion exchange resin.
  • an ion-exchange resin tower for example, is installed at the most downstream side of the subsystem, so that even if metal components are eluted upstream, the effect of the ion-exchange resin tower on the ultrapure water quality can be suppressed. can do.
  • the ion-exchange resin column itself also causes the elution of metal components. Therefore, in order to meet recent strict requirements for metal concentration in ultrapure water, it is required to minimize the elution of metal components from the ion-exchange resin tower.
  • an object of the present invention is to provide an ion exchange device and an ultrapure water production device that minimize the elution of metal components.
  • the ion exchange apparatus of the present invention communicates with a container filled with an ion exchange resin and an opening formed in the bottom surface of the container, and treats water treated with the ion exchange resin. and a screen provided at the opening to prevent the ion-exchange resin from flowing out of the container to the outlet channel, and the portion in contact with the treated water of the outlet channel and
  • Each wetted portion of the screen with treated water is made of a non-metallic material or a metallic material substantially free of iron, nickel, chromium, manganese, aluminum, lead, or copper.
  • the ultrapure water production apparatus of the present invention has the ion exchange device described above.
  • FIG. 1 is a schematic diagram showing the configuration of an ultrapure water production apparatus according to an embodiment of the present invention
  • FIG. 1 is a schematic cross-sectional view of an ion exchange device according to one embodiment of the present invention
  • FIG. 1 is a schematic diagram showing the configuration of an ultrapure water production apparatus according to one embodiment of the present invention
  • FIG. 2 is a schematic cross-sectional view of an ion exchange apparatus that constitutes the ultrapure water production apparatus.
  • the illustrated configuration of the ultrapure water production apparatus is merely an example, and does not limit the present invention.
  • the ultrapure water production apparatus 20 includes a primary pure water tank 21, a pump 22, a heat exchanger 23, an ultraviolet oxidation device 24, an ion exchange device 1, a membrane degassing device 25, and an ultrafiltration (UF). and a membrane device 26 . These constitute a secondary pure water system (subsystem), which sequentially processes the primary pure water produced in the primary pure water system (not shown) to produce ultrapure water, which is then used. It feeds point 27.
  • a secondary pure water system subsystem
  • the water to be treated (primary pure water) stored in the primary pure water tank 21 is pumped out by the pump 22 and supplied to the heat exchanger 23 .
  • the water to be treated is supplied to the ultraviolet oxidation device 24 and irradiated with ultraviolet rays. In this way, all organic carbon (TOC) in the water to be treated is decomposed.
  • ion components such as metal ions are removed from the water to be treated by ion exchange treatment in the ion exchange device 1 .
  • fine particles are removed in the UF membrane device 26 .
  • Part of the ultrapure water thus obtained is supplied to the point of use 27 and the rest is returned to the primary pure water tank 21 .
  • Primary pure water is supplied to the primary pure water tank 21 from a primary pure water system (not shown) as needed.
  • the primary pure water tank 21, the pump 22, the heat exchanger 23, the ultraviolet oxidation device 24, the membrane degassing device 25, and the UF membrane device 26 are generally used in the subsystem of the ultrapure water production system. can be used.
  • the ion exchange device 1 a non-regenerative mixed bed type ion exchange device (cartridge polisher) in which a cation exchange resin and an anion exchange resin are packed in a mixed bed, which is common in a subsystem of an ultrapure water production device. can be used, but its configuration has the following features.
  • the ion exchange device 1 has a resin tower 10 which is a cylindrical container filled with a mixed-bed ion exchange resin (a mixture of a cation exchange resin and an anion exchange resin) 2 .
  • the resin tower 10 has a tower body 11 , an upper socket 12 attached to the upper part of the tower body 11 , and a lower socket 13 attached to the lower part of the tower body 11 .
  • the upper socket 12 defines an inlet channel 12a for circulating the water to be treated from the ultraviolet oxidation device 24, and the lower socket 13 defines an outlet channel for circulating the treated water treated with the ion exchange resin 2. 13a.
  • the flat and horizontal upper surface 3 in the resin tower 10 is formed with an inlet (opening) 12b communicating with the inlet channel 12a, and the flat and horizontal bottom 4 in the resin tower 10 is formed with an outlet channel 13a.
  • An outflow port (opening) 13b communicating with is formed.
  • the ion exchange device 1 includes an upper collector screen 5 (covered over the inlet 12b) provided to cover the inlet 12b in the resin tower 10, and an outlet 13b in the resin tower 10. and a lower collector screen 6 provided (covering the outlet 13b).
  • Each of the collector screens 5 and 6 is composed of a cylindrical wedge wire screen with one end open.
  • the upper collector screen 5 is attached at its open top end to the inlet 12b and the lower collector screen 6 is attached at its open lower end to the outlet 13b.
  • the collector screens 5 and 6 have the function of allowing the water to be treated to flow into the resin tower 10 from the inlet channel 12a and the treated water to flow out from the resin tower 10 into the outlet channel 13a. ing.
  • the lower collector screen 6 has the function of preventing the ion exchange resin 2 from flowing out from the inside of the resin tower 10 to the outlet channel 13a.
  • the slit width of the wedge wire screen is set according to the particle size of the ion-exchange resin used, but is not particularly limited as long as it does not generate a differential pressure when water is passed.
  • the material of the resin tower 10 is not particularly limited as long as it has strength suitable for the filling amount of the ion exchange resin 2 .
  • the tower body 11 can be made of composite material such as fiber reinforced plastic (FRP), and the sockets 12 and 13 can be made of synthetic resin such as polyvinyl chloride (PVC).
  • FRP fiber reinforced plastic
  • PVC polyvinyl chloride
  • the tower body 11, the upper socket 12 and the lower socket 13 are integrally formed in consideration of the initial cost and maintainability.
  • a higher-strength metal material such as stainless steel (SUS) can be used.
  • metal components such as calcium and cobalt elute from FRP, and metal components such as calcium and zinc elute from PVC.
  • metal components such as iron and nickel are more eluted from SUS than from fluororesins such as perfluoroalkoxy fluororesin (PFA). Therefore, in this embodiment, in order to suppress such elution of metal components, the inner surface of the resin tower 10, which is the liquid-contacting portion, is lined with a non-metallic material.
  • nonmetallic material examples include synthetic resins, and specific examples include fluororesins such as polytetrafluoroethylene (PTFE) and polyvinylidene fluoride (PVDF), and polypropylene (PP).
  • PTFE polytetrafluoroethylene
  • PVDF polyvinylidene fluoride
  • PP polypropylene
  • the sockets 12 and 13 that define the inlet channel 12a and the outlet channel 13a may themselves be made of fluororesin such as PTFE or PP.
  • the cost will be very high.
  • the cost will be 5 million yen or more.
  • the cost will be 5 million yen or more.
  • the ion-exchange resin 2 is filled in the lower part, the eluted metal components can be removed by the ion-exchange resin 2. .
  • the part is a part where even if the metal component is eluted therefrom, the metal component may be treated with the ion exchange resin 2 in a later stage. Conversely, it is preferable that at least a portion of the liquid-contacting portion of the resin tower 10 is lined.
  • the part is a part where even if the metal component is eluted from there, there is no possibility that the metal component will be treated with the ion exchange resin 2 in a later stage. This is the inner surface of the passage 13b which is the wetted portion.
  • the curved surface 8 that connects the bottom surface 4 and the side surface 7 in the resin tower 10 does not necessarily need to be lined, but the elution of the metal component can be more reliably performed. In order to suppress it, it is preferable that such a curved surface 8 is also lined.
  • the bottom surface 4 is not a flat horizontal surface but is a curved surface such as a conical surface or a hemispherical surface, and the outflow port 13a is formed at the bottommost portion of the curved surface, the bottom surface 4 is not lined. good too.
  • the material of the collector screens 5 and 6 it is preferable to use a non-metallic material such as a synthetic resin from the viewpoint of suppressing the elution of metal components. It is preferable to use a metal material with as little elution as possible. Specifically, it is preferable to use a metal material substantially free of iron, nickel, chromium, manganese, aluminum, lead, or copper. Such metal materials include, for example, titanium. According to the concept described above, for the upper collector screen 5 of the two collector screens 5 and 6, the material may be selected in consideration of only strength, and may be made of SUS, for example. The term "substantially free” as used herein means that they may be contained as impurities as long as they do not affect the quality of the treated water even if they are eluted.
  • the test results verified by the present inventors regarding the elution of metal components from the resin tower 10 and the collector screens 5 and 6 will be described below.
  • the inventors of the present invention have found the following. That is, when ultrapure water with a metal concentration of ng/L level is required, it may have been sufficient to consider only the elution of metal components from the resin tower 10, but the recent stringent requirement level (i.e. pg/L level), it is important to consider elution not only from the resin tower 10, but also from other components, especially the collector screens 5,6.
  • Test 1 First, in order to confirm the elution of the metal components from the metal container, the inventors measured the concentration of the metal components in the sample water at the outlet of the container when the sample water was passed through the container. Specifically, the sample water is passed through a SUS (SUS316) container filled with a non-regenerative ion exchange resin, and then passed through a monolithic ion exchanger installed at the outlet of the container. did. After the metal components in the sample water flowing out of the container were captured by the ion exchanger, the captured metal components were eluted with the eluent, and the amounts of various metals in the eluent were measured.
  • SUS SUS316
  • a container having an inner diameter of 1200 mm and a height of 1000 mm was used, and as sample water, ultrapure water was passed through the container at a flow rate of 50 L/(L-resin ⁇ h).
  • As an eluent 100 mL of nitric acid obtained by diluting high-concentration nitric acid (trade name: TAMAPURE AA-100) manufactured by Tama Chemical Industry Co., Ltd. to 1N or higher was used.
  • the metal content was measured using an inductively coupled plasma mass spectrometer (ICP-MS), and the metal concentration in the sample water flowing out of the container was calculated by dividing the measured metal content by the concentration ratio of the eluent.
  • ICP-MS inductively coupled plasma mass spectrometer
  • PFA non-metallic
  • Table 1 shows the measurement results for metallic and non-metallic containers.
  • Test 2 Next, in order to confirm the elution of metal components from the metal collector screen, the present inventors compared the amount of metal components eluted with and without a metal collector screen installed in the resin tower. did. Specifically, a resin tower similar to the resin tower shown in FIG. 1 was prepared except that it was not filled with ion exchange resin and that the wetted part was not lined. Then, a test was conducted in the same procedure as in Test 1 above, in the case where SUS (SUS304) collector screens were installed at the inlet and outlet of the resin tower, and in the case where they were not installed. Various metal concentrations were calculated. As the resin tower, an FRP tower body with an inner diameter of 400 mm and a height of 1000 mm and a PVC socket were used. watered. Other conditions are the same as in Test 1 described above.
  • Table 2 shows the measurement results with and without the collector screen installed.
  • the installation of a metal (SUS304) collector screen significantly increased the amount of eluted iron.
  • the collector screen is a wedge wire screen formed into a cylindrical shape, and due to its structure, it is difficult to apply a lining made of a non-metallic material.
  • the measurement results shown in Table 2 indicate that the material of the collector screen should be a non-metallic material, or from the viewpoint of strength, the metallic elements contained in SUS (specifically, iron, nickel, chromium, Manganese, aluminum, lead, or copper) are shown to be preferred.
  • Table 3 shows the measurement results when a SUS collector screen and a titanium collector screen are installed.
  • At least the bottom surface 4 and the inner surface of the outlet channel 13b of the liquid-contacting portion of the resin tower 10 are lined with a non-metallic material.
  • at least the material of the lower collector screen 6 is a non-metallic material or a metallic material substantially free of iron, nickel, chromium, manganese, aluminum, lead or copper, preferably titanium. .
  • the lining material for the resin tower 10 is preferably a non-metallic material such as a synthetic resin as described above, but a metallic material may be used as long as the elution amount of the metallic component is as small as possible. , iron, nickel, chromium, manganese, aluminum, lead, or copper.
  • the lower collector screen 6 itself does not necessarily have to be made of the above-mentioned material, and only the surface (liquid contact part) in contact with the treated water may be made of the above-mentioned material.
  • it may consist of a metallic material substantially free of iron, nickel, chromium, manganese, aluminum, lead, or copper.
  • a pipe connected to the outlet flow path 13a is attached to the lower part of the resin tower 10.
  • the pipe is made of metal such as SUS, it is preferable that the inner surface of the pipe is also lined.
  • the material is preferably a nonmetallic material, specifically a synthetic resin such as fluororesin, or iron, nickel, chromium, manganese, aluminum, lead, or copper. It may be a metal material that does not substantially contain it.
  • the configuration of the ultrapure water production device 1 is not limited to the illustrated configuration, and therefore the installation position of the ion exchange device 1 is also not limited to the illustrated position.
  • the membrane degasser 25 may be omitted, thereby placing the ion exchange device 1 immediately upstream of the most downstream UF membrane device 26 in the subsystem.
  • the membrane degassing device 25 and the UF membrane device 26 may be omitted, thereby placing the ion exchange device 1 at the most downstream side of the subsystem.
  • the above-described configuration of the ion exchange device 1 is not limited to the ion exchange device installed in the subsystem as in the present embodiment, and may be applied to the ion exchange device that constitutes the primary pure water system. .
  • the packing form of the ion exchange resin to be packed in the ion exchange device 1 is not limited to the above-described mixed bed form of the cation exchange resin and the anion exchange resin, but a double bed form of the cation exchange resin and the anion exchange resin.
  • the cation exchange resin or anion exchange resin may be in single bed form.
  • a chelate resin may be filled. Therefore, for example, the ion exchange device 1 may be packed with a single bed of chelate resin, or packed with multiple beds or mixed beds of at least one of the cation exchange resin and the anion exchange resin and the chelate resin. can be anything.
  • REFERENCE SIGNS LIST 1 ion exchange device 2 ion exchange resin 3 top surface 4 bottom surface 5 upper collector screen 6 lower collector screen 7 side surface 8 curved surface 10 resin tower (container)
  • REFERENCE SIGNS LIST 11 container body 12 upper socket 12a inlet channel 12b inlet 13 lower socket 13a outlet channel 13b outlet (opening) 20 ultrapure water production device 21 primary pure water tank 22 pump 23 heat exchanger 24 ultraviolet oxidizer 25 membrane degassing device 26 ultrafiltration membrane device 27 point of use

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Water By Ion Exchange (AREA)

Abstract

L'invention concerne un dispositif d'échange d'ions 1 qui comprend : un récipient 10 rempli d'une résine échangeuse d'ions 2 ; un canal d'écoulement de sortie 13a qui est en communication avec une ouverture 13b formée dans une surface de fond 4 du récipient 10 et qui est destiné à permettre à l'eau traitée avec la résine échangeuse d'ions 2 de s'écouler à travers celle-ci ; et un tamis 6 qui est disposé dans l'ouverture 13b et qui empêche la résine échangeuse d'ions 2 de s'écouler du récipient 10 vers le canal d'écoulement de sortie 13a, chacune des parties en contact avec le liquide du canal d'écoulement de sortie 13a en contact avec l'eau traitée et une partie en contact avec le liquide du tamis 6 en contact avec l'eau traitée est formée d'un matériau non métallique, ou d'un matériau métallique qui ne contient sensiblement pas de fer, nickel, chrome, manganèse, aluminium, plomb ou cuivre.
PCT/JP2022/001262 2021-02-05 2022-01-17 Dispositif d'échange d'ions et appareil de production d'eau ultrapure Ceased WO2022168570A1 (fr)

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JP2021-017487 2021-02-05
JP2021017487A JP7759728B2 (ja) 2021-02-05 2021-02-05 イオン交換装置および超純水製造装置

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4028251A (en) * 1975-10-14 1977-06-07 William Deneen Agitator for solids-containing vessels
JPH05103999A (ja) * 1991-10-18 1993-04-27 Tosoh Corp イオン交換樹脂塔
JPH11105847A (ja) * 1997-09-30 1999-04-20 Toho Titanium Co Ltd チタン製飲料容器並びにその製造方法
JP2007117781A (ja) * 2005-10-24 2007-05-17 Japan Organo Co Ltd イオン交換樹脂、イオン交換樹脂カラム、イオン交換樹脂の含有金属不純物量低減方法、精製装置、及び精製方法
JP2008256364A (ja) * 2007-03-30 2008-10-23 Kurita Water Ind Ltd 液体クロマトグラフィ用のフィルタ、その製造方法および液体クロマトグラフィ装置
JP2011067793A (ja) * 2009-09-28 2011-04-07 Kurita Water Ind Ltd イオン交換装置
JP2011206722A (ja) * 2010-03-30 2011-10-20 Kurita Water Ind Ltd イオン交換装置及び超純水製造装置用サブシステム

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4028251A (en) * 1975-10-14 1977-06-07 William Deneen Agitator for solids-containing vessels
JPH05103999A (ja) * 1991-10-18 1993-04-27 Tosoh Corp イオン交換樹脂塔
JPH11105847A (ja) * 1997-09-30 1999-04-20 Toho Titanium Co Ltd チタン製飲料容器並びにその製造方法
JP2007117781A (ja) * 2005-10-24 2007-05-17 Japan Organo Co Ltd イオン交換樹脂、イオン交換樹脂カラム、イオン交換樹脂の含有金属不純物量低減方法、精製装置、及び精製方法
JP2008256364A (ja) * 2007-03-30 2008-10-23 Kurita Water Ind Ltd 液体クロマトグラフィ用のフィルタ、その製造方法および液体クロマトグラフィ装置
JP2011067793A (ja) * 2009-09-28 2011-04-07 Kurita Water Ind Ltd イオン交換装置
JP2011206722A (ja) * 2010-03-30 2011-10-20 Kurita Water Ind Ltd イオン交換装置及び超純水製造装置用サブシステム

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TW202239715A (zh) 2022-10-16
JP7759728B2 (ja) 2025-10-24
JP2022120535A (ja) 2022-08-18
JP2025126310A (ja) 2025-08-28

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