TW201726557A - Ultrapure water production apparatus and method for operating thereof that can efficiently remove boron and rapidly prevent leakage thereof - Google Patents
Ultrapure water production apparatus and method for operating thereof that can efficiently remove boron and rapidly prevent leakage thereof Download PDFInfo
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- TW201726557A TW201726557A TW105129663A TW105129663A TW201726557A TW 201726557 A TW201726557 A TW 201726557A TW 105129663 A TW105129663 A TW 105129663A TW 105129663 A TW105129663 A TW 105129663A TW 201726557 A TW201726557 A TW 201726557A
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- 229910052796 boron Inorganic materials 0.000 title claims abstract description 140
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 239000012498 ultrapure water Substances 0.000 title claims abstract description 65
- 229910021642 ultra pure water Inorganic materials 0.000 title claims abstract description 64
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 201
- 238000005342 ion exchange Methods 0.000 claims abstract description 58
- 239000012528 membrane Substances 0.000 claims abstract description 46
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 22
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 21
- 238000009296 electrodeionization Methods 0.000 claims description 55
- 238000011033 desalting Methods 0.000 claims description 26
- 238000010612 desalination reaction Methods 0.000 claims description 22
- 150000002500 ions Chemical class 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 239000003011 anion exchange membrane Substances 0.000 claims description 10
- 238000005341 cation exchange Methods 0.000 claims description 8
- -1 boron ions Chemical class 0.000 claims description 7
- 230000001172 regenerating effect Effects 0.000 abstract description 17
- 230000003647 oxidation Effects 0.000 abstract description 10
- 238000007254 oxidation reaction Methods 0.000 abstract description 10
- 238000002242 deionisation method Methods 0.000 abstract description 6
- 238000000746 purification Methods 0.000 abstract 2
- 238000011069 regeneration method Methods 0.000 description 21
- 230000008929 regeneration Effects 0.000 description 19
- 239000003957 anion exchange resin Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 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 5
- 239000003456 ion exchange resin Substances 0.000 description 5
- 229920003303 ion-exchange polymer Polymers 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000007872 degassing Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 239000007800 oxidant agent Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000012625 in-situ measurement Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
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- 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
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
- B01D61/46—Apparatus therefor
- B01D61/48—Apparatus therefor having one or more compartments filled with ion-exchange material, e.g. electrodeionisation
-
- 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
-
- 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
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
- B01D61/52—Accessories; Auxiliary operation
-
- 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
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
- B01D61/54—Controlling or regulating
-
- 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
- B01D61/58—Multistep processes
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
- C02F1/4695—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis electrodeionisation
-
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
Abstract
Description
本發明是有關於一種製造半導體、液晶等電子產業領域中所利用的超純水的超純水製造裝置及該超純水製造裝置的運轉方法。特別是有關於一種可有效率地去除硼且預防其洩漏的超純水製造裝置及其運轉方法。The present invention relates to an ultrapure water production apparatus for producing ultrapure water used in the field of electronics industries such as semiconductors and liquid crystals, and an operation method of the ultrapure water production apparatus. In particular, there is an ultrapure water manufacturing apparatus and a method of operating the same that can efficiently remove boron and prevent leakage thereof.
先前，半導體等電子產業領域中使用的超純水是藉由利用包括預處理系統、一次純水系統以及對一次純水進行處理的子系統的超純水製造裝置，對原水進行處理來製造。Previously, ultrapure water used in the field of electronics such as semiconductors was manufactured by treating raw water by an ultrapure water manufacturing apparatus including a pretreatment system, a primary pure water system, and a subsystem for treating primary pure water.
該超純水製造裝置中，預處理系統包括凝聚、加壓浮起（沈澱）、過濾（膜濾）裝置等，以去除原水中的懸浮物質或膠體物質。該過程中亦可去除高分子系有機物、疏水性有機物等。另外，一次純水系統基本上具備逆滲透（Reverse Osmosis，RO）膜分離裝置以及再生型離子交換裝置（混合床（mixed bed）式或者四床五塔式等），RO膜分離裝置中，不僅去除鹽類，而且去除離子性、膠體性的總有機碳（Total Organic Carbon，TOC）。再生型離子交換裝置中，不僅去除鹽類，而且藉由利用離子交換樹脂進行吸附或者離子交換而去除TOC成分。In the ultrapure water manufacturing apparatus, the pretreatment system includes a coagulation, a pressurized floating (precipitation), a filtration (membrane filtration) device, and the like to remove suspended matter or colloidal substances in the raw water. In this process, polymer organic substances, hydrophobic organic substances, and the like can also be removed. In addition, the primary pure water system basically has a reverse osmosis (RO) membrane separation device and a regenerative ion exchange device (mixed bed type or four bed five-column type), and the RO membrane separation device not only Remove salts and remove ionic, colloidal total organic carbon (TOC). In the regenerative ion exchange apparatus, not only salts but also TOC components are removed by adsorption or ion exchange using an ion exchange resin.
進而，子系統基本上具備低壓紫外線（ultraviolet，UV）氧化裝置、以及非再生型混合床式離子交換裝置及超濾（ultrafiltration，UF）膜分離裝置，以進一步提高一次純水的純度而成為超純水。低壓UV氧化裝置中，藉由自低壓紫外線燈發出的185 nm的紫外線，將TOC分解為有機酸，進而分解至CO2 。而且，藉由分解而生成的有機物及CO2 於後段的非再生型混合床式離子交換裝置中被去除。UF膜分離裝置中，微粒子被去除，離子交換樹脂的流出粒子亦被去除。Further, the subsystem basically includes a low-pressure ultraviolet (UV) oxidation device, a non-regeneration type mixed bed type ion exchange device, and an ultrafiltration (UF) membrane separation device to further improve the purity of the primary pure water and become super Pure water. In a low-pressure UV oxidation device, TOC is decomposed into an organic acid by 185 nm ultraviolet light emitted from a low-pressure ultraviolet lamp, and further decomposed into CO 2 . Further, the organic matter and CO 2 produced by the decomposition are removed in the non-regeneration type mixed bed type ion exchange apparatus in the subsequent stage. In the UF membrane separation device, the fine particles are removed, and the effluent particles of the ion exchange resin are also removed.
如上所述的現有的超純水製造裝置的子系統中，若自一次純水系統中洩漏弱離子成分、特別是硼離子，則利用非再生型混合床式離子交換裝置加以去除，但非再生型混合床式離子交換裝置若某程度地吸附硼離子則必須進行更換。近年來，超純水所要求的硼濃度逐漸降低至0.1 ppt以下，非再生型混合床式離子交換裝置中，低濃度範圍下的硼的去除效率差，故而為了確實地維持硼的要求水質而必須提前更換非再生型混合床式離子交換裝置，存在其更換頻率變短的問題點。因此，如專利文獻1中所記載，考慮於子系統中設置電去離子裝置。 [現有技術文獻] [專利文獻]In the subsystem of the conventional ultrapure water production apparatus as described above, if a weak ion component, particularly boron ions, is leaked from the primary pure water system, it is removed by a non-regenerative mixed bed ion exchange device, but non-regenerated The mixed bed type ion exchange device must be replaced if it adsorbs boron ions to some extent. In recent years, the boron concentration required for ultrapure water has gradually decreased to less than 0.1 ppt. In the non-regenerative mixed bed type ion exchange apparatus, the removal efficiency of boron in a low concentration range is poor, so that in order to reliably maintain the required water quality of boron, The non-regenerative hybrid bed type ion exchange device must be replaced in advance, and there is a problem that the replacement frequency becomes short. Therefore, as described in Patent Document 1, it is considered to provide an electrodeionization device in the subsystem. [Prior Art Document] [Patent Literature]
[專利文獻1]日本專利特開平7-8948號公報[Patent Document 1] Japanese Patent Laid-Open No. 7-8948
[發明所欲解決的課題] 然而，於如專利文獻1中所記載般於子系統中設置電去離子裝置的情況下，由於在子系統中對與超純水接近的高純度的水進行處理，故而存在以下問題點：電難以流動，用以去離子的電阻變大，因此電流效率差，對電去離子裝置施加的負荷亦變大。另外，電去離子裝置由於考慮到其耐壓性而不太能夠增大被處理水的供給壓，而且處理水的吐出壓力較供給壓而言進一步變小，因此存在電去離子裝置的後段的處理變得不穩定故無法確保水質的穩定性、而且對於將超純水供給至使用點而言水壓不足的問題點。因此，於電去離子裝置的後段另行設置增壓泵等供給裝置，但必須考慮來自增壓泵的溶出物的處理，存在容易導致子系統的大型化的問題點。[Problems to be Solved by the Invention] However, in the case where the electrodeionization apparatus is provided in the subsystem as described in Patent Document 1, the high-purity water close to the ultrapure water is treated in the subsystem. Therefore, there is a problem that electricity is difficult to flow, and the resistance for deionization becomes large, so that the current efficiency is poor, and the load applied to the electrodeionization device also becomes large. Further, the electrodeionization apparatus is less likely to increase the supply pressure of the water to be treated in consideration of the pressure resistance thereof, and the discharge pressure of the treated water is further smaller than the supply pressure, so that there is a rear stage of the electrodeionization apparatus. The treatment becomes unstable, so that the stability of the water quality cannot be ensured, and the problem that the water pressure is insufficient for supplying the ultrapure water to the use point is insufficient. Therefore, a supply device such as a booster pump is separately provided in the subsequent stage of the electrodeionization apparatus. However, it is necessary to consider the treatment of the eluted material from the booster pump, and there is a problem that the size of the subsystem is likely to increase.
進而，無論是將超純水製造裝置設為哪一種構成的情況，均必須快速地偵檢出硼向由子系統所供給的超純水中的洩漏，但由於不存在原地測定0.1 ppt水準的硼濃度的機構，故而存在其偵檢困難的問題點。Further, in any case where the ultrapure water production apparatus is configured, it is necessary to quickly detect the leakage of boron into the ultrapure water supplied by the subsystem, but since there is no in situ measurement of 0.1 ppt level The mechanism of boron concentration has a problem in that it is difficult to detect.
本發明是鑒於所述課題而形成，目的在於提供一種可有效率地去除硼且迅速預防其洩漏的超純水製造裝置。另外，本發明的目的在於提供該超純水製造裝置的運轉方法。The present invention has been made in view of the above problems, and it is an object of the invention to provide an ultrapure water production apparatus which can efficiently remove boron and quickly prevent leakage thereof. Further, it is an object of the invention to provide a method of operating the ultrapure water production apparatus.
[解決課題的手段] 鑒於所述目的，第一，本發明提供一種超純水製造裝置，其具有一次純水系統以及子系統，所述子系統具備對由該一次純水系統所獲得的一次純水進行處理的離子交換裝置及UF膜裝置，並且所述超純水製造裝置於所述一次純水系統的後段且所述子系統的前段具備硼濃度測定機構及電去離子裝置（發明1）。[Means for Solving the Problem] In view of the object, first, the present invention provides an ultrapure water manufacturing apparatus having a primary pure water system and a subsystem having the same time obtained by the primary pure water system An ion exchange device and a UF membrane device which are treated with pure water, and the ultrapure water production device is provided with a boron concentration measuring mechanism and an electrodeionization device in the latter stage of the primary pure water system and in the front stage of the subsystem (Invention 1 ).
依據所述發明（發明1），預先測量電去離子裝置對於一次純水的硼去除率，利用硼濃度測定機構來連續監視一次純水的硼濃度。通用的硼監測器等硼偵檢機構的硼的偵檢水準為10 ppb，讀值為1 ppb水準，將由硼濃度測定機構所偵檢的硼濃度乘以電去離子裝置的硼去除率而得者假設為電去離子裝置的處理水的硼濃度。而且，經子系統處理的超純水的硼濃度至少變得小於該電去離子裝置的處理水，因此以電去離子裝置處理水的硼濃度為基準，來判斷經子系統處理的超純水的硼濃度，若一次純水的硼濃度穩定，則繼續連續運轉，適當地對子系統的處理水（超純水）的硼濃度進行精密分析，若其上升率變大，則判斷為子系統的離子交換裝置接近穿透而將其更換，藉此可有效率地去除硼，而且可迅速地預防硼的洩漏。According to the invention (Invention 1), the boron removal rate of the primary pure water is measured in advance by the electrodeionization apparatus, and the boron concentration of the pure water is continuously monitored by the boron concentration measuring means. The boron detection level of a boron detector such as a general-purpose boron monitor is 10 ppb, and the reading value is 1 ppb. The boron concentration detected by the boron concentration measuring mechanism is multiplied by the boron removal rate of the electrodeionization device. It is assumed that the boron concentration of the treated water is the electrodeionization device. Moreover, the boron concentration of the ultrapure water treated by the subsystem becomes at least smaller than the treated water of the electrodeionization device, and therefore the ultrapure water treated by the subsystem is determined based on the boron concentration of the treated water of the electrodeionization device. If the boron concentration of the primary pure water is stable, the continuous operation is continued, and the boron concentration of the treated water (ultra-pure water) of the subsystem is appropriately analyzed. If the rising rate is increased, the subsystem is judged to be a subsystem. The ion exchange device is replaced by penetration and is replaced, whereby boron can be efficiently removed, and leakage of boron can be quickly prevented.
所述發明（發明1）中，較佳為所述一次純水系統具有逆滲透膜裝置及離子交換裝置（發明2）。In the invention (Invention 1), it is preferable that the primary pure water system has a reverse osmosis membrane device and an ion exchange device (Invention 2).
依據所述發明（發明2），可於一次純水系統中效率良好地去除硼。According to the invention (Invention 2), boron can be efficiently removed in a primary pure water system.
所述發明（發明1、發明2）中，較佳為所述電去離子裝置具備：陰極及陽極、配置於該陰極及陽極之間的陽離子交換膜及陰離子交換膜、以及由該些陽離子交換膜及陰離子交換膜所劃分形成的除鹽室及濃縮室，且於所述除鹽室及所述濃縮室中填充有離子交換體，並且具有向所述濃縮室中通入濃縮水的濃縮水通水機構以及向所述除鹽室中通入原水而取出去離子水的機構（發明3）。In the invention (Invention 1 and Invention 2), it is preferable that the electrodeionization device includes a cathode and an anode, a cation exchange membrane and an anion exchange membrane disposed between the cathode and the anode, and exchange of the cations a desalting compartment and a concentrating compartment formed by dividing the membrane and the anion exchange membrane, and the ion stripping body is filled in the desalting compartment and the concentrating compartment, and the concentrated water having a concentrated water is introduced into the concentrating compartment A water passing means and a mechanism for taking out deionized water by introducing raw water into the desalting chamber (Invention 3).
依據所述發明（發明3），具有此種構成的電去離子裝置由於硼的去除率高且可維持大致一定的去除率，故而可將由硼濃度測定機構所偵檢的硼的濃度乘以電去離子裝置的硼去除率而得者，精度良好地假設為電去離子裝置的處理水的硼濃度。According to the invention (Invention 3), since the electrodeionization apparatus having such a configuration has a high removal rate of boron and can maintain a substantially constant removal rate, the concentration of boron detected by the boron concentration measuring means can be multiplied by electricity. The boron removal rate of the deionization apparatus is accurately determined to be the boron concentration of the treated water of the electrodeionization apparatus.
所述發明（發明3）中，較佳為所述濃縮水通水機構將已通入所述除鹽室中的去離子水作為濃縮水而通水（發明4）。In the invention (Invention 3), it is preferable that the concentrated water-passing means passes the deionized water that has passed through the desalination chamber as concentrated water to pass water (Invention 4).
依據所述發明（發明4），由於藉由將已通入除鹽室中的去離子水通入至濃縮室中，除鹽水自身離子成分為微量，故而可減少濃縮室與除鹽室的離子濃度的差距，可提高硼的去除率，因此不需要長期更換子系統的離子交換裝置。According to the invention (Invention 4), since the deionized water which has passed through the desalting compartment is introduced into the concentrating compartment, the ionic component of the demineralized water is a trace amount, so that the ions of the concentrating compartment and the desalting compartment can be reduced. The difference in concentration can increase the removal rate of boron, so there is no need to replace the subsystem's ion exchange device for a long time.
所述發明（發明4）中，較佳為所述濃縮水通水機構將所述濃縮水自與所述除鹽室的去離子水取出口接近的一側導入至該濃縮室內，並且自與除鹽室的原水入口接近的一側流出（發明5）。In the invention (Invention 4), preferably, the concentrated water passage means introduces the concentrated water into the concentration chamber from a side close to the deionized water outlet of the desalination chamber, and is self-contained The raw water inlet of the desalination chamber flows out on the side close to it (Invention 5).
依據所述發明（發明5），電去離子裝置由於在除鹽室中越朝向與去離子水取出口接近的一側，離子濃度越降低，故而藉由與此反向地自與去離子水取出口接近的一側將去離子水供給至濃縮室中，可於除鹽室與濃縮室的全域中縮小除鹽室與濃縮室的離子濃度的差距，硼離子的去除率的提高效果大，因此可進一步提高硼的去除率，故而不需要長期更換子系統的離子交換裝置。According to the invention (Invention 5), since the electrodeion concentration device is lowered toward the side close to the deionized water take-out port in the desalination chamber, the ion concentration is lowered, and thus, the deionized water is taken in reverse. The side close to the outlet supplies deionized water to the concentrating chamber, and the difference in ion concentration between the desalting chamber and the concentrating chamber can be reduced in the entire range of the desalting chamber and the concentrating chamber, and the removal rate of boron ions is greatly enhanced. The boron removal rate can be further increased, so that the ion exchange device of the subsystem is not required to be replaced for a long period of time.
另外，第二，本發明提供一種超純水製造裝置的運轉方法，所述超純水製造裝置具有一次純水系統、以及具備對由該一次純水系統所獲得的一次純水進行處理的離子交換裝置及UF膜裝置的子系統，且於所述一次純水系統的後段且所述子系統的前段具備硼濃度測定機構及電去離子裝置；所述超純水製造裝置的運轉方法的特徵在於：當將被處理水連續地通入一次純水系統及子系統中來製造超純水時，根據所述電去離子裝置的硼離子的去除率以及由所述硼濃度測定機構測定的硼濃度，來判斷是否需要更換所述子系統的離子交換裝置（發明6）。Further, the second aspect of the present invention provides an operation method of an ultrapure water production apparatus having a primary pure water system and an ion having a primary pure water obtained by the primary pure water system a subsystem of the exchange device and the UF membrane device, and a boron concentration measuring mechanism and an electrodeionization device in a rear stage of the primary pure water system and in a front stage of the subsystem; characteristics of an operation method of the ultrapure water manufacturing device When the treated water is continuously introduced into the pure water system and the subsystem to produce ultrapure water, the boron ion removal rate according to the electrodeionization device and the boron determined by the boron concentration measuring mechanism The concentration is used to determine whether it is necessary to replace the ion exchange device of the subsystem (Invention 6).
依據所述發明（發明6），預先測量電去離子裝置對於一次純水的硼去除率，以硼濃度測定機構來連續監視一次純水的硼濃度。通用的硼監測器等硼偵檢機構的硼的偵檢水準為10 ppb，讀值為1 ppb水準，將由硼濃度測定機構所偵檢的硼濃度乘以電去離子裝置的硼去除率而得者，假設為電去離子裝置的處理水的硼濃度，可根據該硼濃度、以及所述子系統的超純水的硼濃度來判斷是否需要更換離子交換裝置。According to the invention (Invention 6), the boron removal rate of the primary pure water is measured in advance, and the boron concentration of the pure water is continuously monitored by the boron concentration measuring means. The boron detection level of a boron detector such as a general-purpose boron monitor is 10 ppb, and the reading value is 1 ppb. The boron concentration detected by the boron concentration measuring mechanism is multiplied by the boron removal rate of the electrodeionization device. It is assumed that the boron concentration of the treated water in the electrodeionization apparatus can be determined based on the boron concentration and the boron concentration of the ultrapure water of the subsystem to determine whether or not the ion exchange device needs to be replaced.
所述發明（發明6）中，較佳為所述一次純水系統具有逆滲透膜裝置及離子交換裝置（發明7）。In the invention (Invention 6), it is preferable that the primary pure water system has a reverse osmosis membrane device and an ion exchange device (Invention 7).
依據所述發明（發明7），可於一次純水系統中效率良好地去除硼。According to the invention (Invention 7), boron can be efficiently removed in a primary pure water system.
所述發明（發明6、發明7）中，較佳為所述電去離子裝置具備：陰極及陽極、配置於該陰極及陽極之間的陽離子交換膜及陰離子交換膜、以及由該些陽離子交換膜及陰離子交換膜所劃分形成的除鹽室及濃縮室，且於所述除鹽室及所述濃縮室中填充有離子交換體，並且具有向所述濃縮室中通入濃縮水的濃縮水通水機構以及向所述除鹽室中通入原水而取出去離子水的機構（發明8）。In the invention (Invention 6 and Invention 7), it is preferable that the electrodeionization device includes a cathode and an anode, a cation exchange membrane and an anion exchange membrane disposed between the cathode and the anode, and exchange of the cations a desalting compartment and a concentrating compartment formed by dividing the membrane and the anion exchange membrane, and the ion stripping body is filled in the desalting compartment and the concentrating compartment, and the concentrated water having a concentrated water is introduced into the concentrating compartment A water passing means and a mechanism for taking out deionized water by introducing raw water into the desalting chamber (Invention 8).
依據所述發明（發明8），由於藉由將已通入除鹽室中的去離子水通入至濃縮室中，除鹽水自身離子成分為微量，故而可減少濃縮室與除鹽室的離子濃度的差距，可提高硼的去除率，因此不需要長期更換子系統的離子交換裝置。According to the invention (Invention 8), since the deionized water which has passed through the desalting compartment is introduced into the concentrating compartment, the ionic component of the demineralized water is a trace amount, so that the ions of the concentrating compartment and the desalting compartment can be reduced. The difference in concentration can increase the removal rate of boron, so there is no need to replace the subsystem's ion exchange device for a long time.
所述發明（發明8）中，較佳為所述濃縮水通水機構將已通入所述除鹽室中的處理水的一部分作為所述濃縮水而導入（發明9）。In the invention (Invention 8), it is preferable that the concentrated water passage means introduces a part of the treated water that has passed through the desalination chamber as the concentrated water (Invention 9).
依據所述發明（發明9），由於藉由將已通入除鹽室中的去離子水通入至濃縮室中，除鹽水自身離子成分為微量，故而可減少濃縮室與除鹽室的離子濃度的差距，可提高硼的去除率，因此不需要長期更換子系統的離子交換裝置。According to the invention (Invention 9), since the deionized water which has passed through the desalting compartment is introduced into the concentrating compartment, the ionic component of the demineralized water is a trace amount, so that the ions of the concentrating compartment and the desalting compartment can be reduced. The difference in concentration can increase the removal rate of boron, so there is no need to replace the subsystem's ion exchange device for a long time.
所述發明（發明9）中，較佳為將所述濃縮水自所述濃縮室的與所述除鹽室的去離子水取出口接近的一側導入，並且自所述濃縮室的與所述除鹽室的原水入口接近的一側流出（發明10）。In the invention (Invention 9), it is preferable that the concentrated water is introduced from a side of the concentrating chamber close to a deionized water take-out port of the desalination chamber, and from the concentrating chamber The side of the raw water inlet of the salt removal chamber flows out (Invention 10).
依據所述發明（發明10），電去離子裝置由於在除鹽室中，越朝向與去離子水取出口接近的一側，離子濃度越降低，故而藉由與此反向地將去離子水自與去離子水取出口接近的一側供給至濃縮室中，可於除鹽室與濃縮室的全域中縮小除鹽室與濃縮室的離子濃度的差距，硼離子的去除率的提高效果大，故而可進一步提高硼的去除率，因此不需要長期更換子系統的離子交換裝置。According to the invention (Invention 10), since the electrodeionization device is directed toward the side close to the deionized water extraction port in the desalination chamber, the ion concentration is lowered, so that deionized water is reversed by this. It is supplied to the concentrating chamber from the side close to the deionized water take-out port, and the difference in ion concentration between the desalting chamber and the concentrating chamber can be reduced in the entire range of the desalting chamber and the concentrating chamber, and the removal rate of boron ions is greatly enhanced. Therefore, the removal rate of boron can be further increased, so that it is not necessary to replace the ion exchange device of the subsystem for a long period of time.
[發明的效果] 依據本發明，於一次純水系統的後段設置硼濃度測定機構及電去離子裝置，以硼濃度測定機構來連續監視一次純水的硼濃度，將由該硼濃度測定機構所測定的硼濃度乘以電去離子裝置的硼去除率而得者假設為電去離子裝置的處理水的硼濃度，以該電去離子裝置處理水的硼濃度為基準，與經子系統處理的二次純水（超純水）的硼濃度的實測值進行比較，若實測值大於既定的值，則更換子系統的離子交換裝置，藉此可不導致硼的洩漏且效率良好地更換子系統的離子交換裝置。[Effect of the Invention] According to the present invention, a boron concentration measuring means and an electrodeionization apparatus are provided in the latter stage of the primary pure water system, and the boron concentration of the pure water is continuously monitored by the boron concentration measuring means, and is determined by the boron concentration measuring means. The boron concentration is multiplied by the boron removal rate of the electrodeionization device, which is assumed to be the boron concentration of the treated water of the electrodeionization device, based on the boron concentration of the treated water of the electrodeionization device, and the second processed by the subsystem. The measured value of the boron concentration of the sub-pure water (ultra-pure water) is compared. If the measured value is greater than the predetermined value, the ion exchange device of the subsystem is replaced, thereby preventing the boron from leaking and replacing the ion of the subsystem efficiently. Exchange device.
以下，參照隨附圖式，對本發明的第一實施形態的超純水製造裝置進行說明。Hereinafter, an ultrapure water production apparatus according to a first embodiment of the present invention will be described with reference to the accompanying drawings.
圖1是表示本發明的第一實施形態的超純水製造裝置的流程圖，圖1中，超純水製造裝置1具備一次純水系統2以及子系統3，一次純水系統2具有逆滲透膜（RO）裝置4以及再生型混合床式離子交換裝置5，且於該再生型混合床式離子交換裝置5的後段具有作為硼濃度測定機構的硼監測器6及電去離子裝置7，該電去離子裝置7經由經氮封的子儲槽8而與子系統3連接。而且，子系統3包括：子儲槽8、供給泵P、UV氧化裝置9、非再生型混合床式離子交換裝置10及超濾膜（UF膜）11，並成為自超濾膜（UF膜）11經由使用點UP而回流至子儲槽8的構成。1 is a flow chart showing an ultrapure water production apparatus according to a first embodiment of the present invention. In FIG. 1, an ultrapure water production apparatus 1 is provided with a primary pure water system 2 and a subsystem 3, and the primary pure water system 2 has reverse osmosis. a membrane (RO) device 4 and a regenerative mixed bed ion exchange device 5, and a boron monitor 6 and an electrodeionization device 7 as a boron concentration measuring mechanism in the subsequent stage of the regenerative mixed bed ion exchange device 5, The electrodeionization device 7 is connected to the subsystem 3 via a nitrogen-sealed sub-storage tank 8. Further, the subsystem 3 includes a sub-tank 8, a supply pump P, a UV oxidation device 9, a non-regeneration type mixed bed type ion exchange device 10, and an ultrafiltration membrane (UF membrane) 11, and is a self-ultrafiltration membrane (UF membrane). The configuration of 11 is returned to the sub tank 8 via the use point UP.
該超純水製造裝置1中，硼監測器6可使用能夠進行硼濃度為10 ppb水準、讀值為1 ppb水準的測定的通用的硼監測器，例如可使用中央科學（Central Kagaku）（股）銷售的西福斯（SIEVERS）超純水測定線上硼分析計。In the ultrapure water manufacturing apparatus 1, the boron monitor 6 can use a general-purpose boron monitor capable of performing a measurement having a boron concentration of 10 ppb and a reading value of 1 ppb, for example, Central Kagaku ( ) The sale of the SIEVERS ultrapure water determination line boron analyzer.
另外，電去離子裝置7可適當使用具有如圖2及圖3所示的構成者。Further, the electrodeionization apparatus 7 can be suitably used as shown in FIGS. 2 and 3.
圖2中，電去離子裝置7是於電極（陽極21、陰極22）之間交替排列多個陰離子交換膜23及陽離子交換膜24而交替形成有濃縮室25及除鹽室26者，於除鹽室26中混合或多層狀地填充有離子交換樹脂、離子交換纖維或包含接枝交換體等的離子交換體（陰離子交換體及陽離子交換體）。另外，於濃縮室25與陽極室27及陰極室28中亦填充有離子交換體。In Fig. 2, the electrodeionization device 7 is a plurality of anion exchange membranes 23 and cation exchange membranes 24 alternately arranged between electrodes (anode 21 and cathode 22) to alternately form a concentration chamber 25 and a desalination chamber 26. The salt chamber 26 is filled or multi-layered with an ion exchange resin, an ion exchange fiber, or an ion exchanger (an anion exchanger and a cation exchanger) including a graft exchanger. Further, an ion exchanger is also filled in the concentrating chamber 25, the anode chamber 27, and the cathode chamber 28.
於該電去離子裝置7中設置有：向除鹽室26中通入再生型混合床式離子交換裝置5的一次純水W1而取出處理水W2的通水機構（未圖示）、以及向濃縮室25中通入濃縮水W3的濃縮水通水機構（未圖示），本實施形態中成為如下構成：將濃縮水W3自與除鹽室26的處理水W2的取出口接近的一側導入至濃縮室25內，並且自與除鹽室26的原水入口接近的一側流出，即，自與除鹽室26中的一次純水W1的流通方向相反的方向，將濃縮水W3導入至濃縮室25中而將濃縮排水W4吐出。The electro-deionization apparatus 7 is provided with a water-passing mechanism (not shown) for taking out the treated water W2 into the single-purity W1 of the regenerative mixed bed type ion exchange device 5 into the desalination chamber 26, and In the concentrating chamber 25, a concentrated water-passing mechanism (not shown) through which the concentrated water W3 is supplied is used. In the present embodiment, the concentrated water W3 is disposed from the outlet of the treated water W2 of the desalination chamber 26. It is introduced into the concentrating chamber 25 and flows out from the side close to the raw water inlet of the desalination chamber 26, that is, the concentrated water W3 is introduced from the direction opposite to the flow direction of the primary pure water W1 in the desalination chamber 26. The concentrated drain W4 is discharged from the concentrating chamber 25.
具體而言，較佳為如圖3所示，將由除鹽室26所獲得的處理水W2的一部分導入至濃縮室25中而使用處理水W2作為濃縮水W3，藉此成為離子濃度降低的濃縮水W3。Specifically, as shown in FIG. 3, a part of the treated water W2 obtained by the desalination chamber 26 is introduced into the concentrating chamber 25, and the treated water W2 is used as the concentrated water W3, whereby the concentration of the ion concentration is lowered. Water W3.
進而，作為子系統3的UV氧化裝置9，可使用通常於超純水製造裝置中使用的照射具有185 nm附近的波長的UV的UV氧化裝置，例如使用低壓水銀燈的UV氧化裝置。Further, as the UV oxidizing device 9 of the subsystem 3, a UV oxidizing device for irradiating UV having a wavelength of around 185 nm, which is usually used in an ultrapure water producing apparatus, for example, a UV oxidizing device using a low pressure mercury lamp can be used.
對具有如上所述的構成的超純水製造裝置的運轉方法進行說明。首先，將視需要利用未圖示的預處理機構實施了預處理的被處理水W供給至一次純水系統2中，利用逆滲透膜（RO）裝置4以及再生型混合床式離子交換裝置5進行處理。逆滲透膜（RO）裝置4中，除了去除鹽類以外，還去除離子性、膠體性的TOC。再生型混合床式離子交換裝置5中，除了去除鹽類以外，還去除由離子交換樹脂所吸附或者經離子交換的TOC成分，從而製造一次純水W1。An operation method of the ultrapure water production apparatus having the above configuration will be described. First, the treated water W subjected to pretreatment by a pretreatment mechanism (not shown) is supplied to the primary pure water system 2 as needed, and the reverse osmosis membrane (RO) unit 4 and the regenerative mixed bed type ion exchange unit 5 are used. Process it. In the reverse osmosis membrane (RO) apparatus 4, in addition to salt removal, ionic and colloidal TOC are removed. In the regenerative mixed bed type ion exchange apparatus 5, in addition to the removal of salts, the TOC component adsorbed or ion-exchanged by the ion exchange resin is removed, and the primary pure water W1 is produced.
而且，於本實施形態中，對於該再生型混合床式離子交換裝置5的一次純水W1，利用硼的偵檢水準為10 ppb、讀值為1 ppb水準的硼監測器6來連續監視硼濃度[B]。而且，將該一次純水W1以電去離子裝置7進行處理後，將所獲得的處理水W2供給至子儲槽8中。Further, in the present embodiment, boron is continuously monitored for the primary pure water W1 of the regenerative mixed bed type ion exchange apparatus 5 using a boron monitor 6 having a detection level of boron of 10 ppb and a reading value of 1 ppb. Concentration [B]. Then, the primary pure water W1 is treated by the electrodeionization device 7, and the obtained treated water W2 is supplied to the sub-tank 8.
此時，藉由測定對硼濃度已知的既定的一次純水W1進行處理時的電去離子裝置7的處理水W2中的硼濃度，來預先計算硼去除率。電去離子裝置7的硼去除率較佳為99%以上，特佳為99.99%以上。特別是如所述的圖2及圖3所示的電去離子裝置較佳為將硼去除率設為99.99%以上。而且，可將一次純水W1的硼濃度、與電去離子裝置7的硼去除率的積假設為處理水W2的硼濃度[B1]（例如，若一次純水W1的硼濃度[B]為1 ppb以下且電去離子裝置7的硼去除率為99.99%，則作為處理水W2的硼濃度[B1]的硼濃度可假設為0.1 ppt以下）。如此，即便對子系統3供給的處理水W2的硼濃度為1 ppb以下，亦可連續地監視。At this time, the boron removal rate is calculated in advance by measuring the boron concentration in the treated water W2 of the electrodeionization apparatus 7 when the predetermined primary pure water W1 having a known boron concentration is treated. The boron removal rate of the electrodeionization device 7 is preferably 99% or more, and particularly preferably 99.99% or more. In particular, the electrodeionization apparatus shown in Figs. 2 and 3 as described above preferably has a boron removal rate of 99.99% or more. Further, the product of the boron concentration of the primary pure water W1 and the boron removal rate of the electrodeionization device 7 can be assumed to be the boron concentration [B1] of the treated water W2 (for example, if the boron concentration [B] of the primary pure water W1 is When the boron removal rate of the electrodeionization device 7 is 1 ppb or less and the boron removal rate is 99.99%, the boron concentration of the boron concentration [B1] as the treatment water W2 can be assumed to be 0.1 ppt or less. In this manner, even if the boron concentration of the treated water W2 supplied to the subsystem 3 is 1 ppb or less, continuous monitoring can be performed.
繼而，將供給至子儲槽8中的處理水W2利用泵P來供給並加以處理。子系統3中，進行利用UV氧化裝置9、非再生型混合床式離子交換裝置10及超濾膜11的處理。UV氧化裝置9中，利用由UV燈發出的波長為185 nm的紫外線，將TOC分解為有機酸，進而分解至CO2 水準。所分解的有機酸及CO2 於後段的非再生型混合床式離子交換裝置10中被去除。超濾膜11中，微小粒子被去除，非再生型混合床式離子交換裝置10的流出粒子亦被去除，從而獲得二次純水（超純水）W5。將該二次純水W5供給至使用點UP後，未使用部分被返送至子儲槽8中。Then, the treated water W2 supplied to the sub tank 8 is supplied and processed by the pump P. In the subsystem 3, processing by the UV oxidation device 9, the non-regeneration type mixed bed type ion exchange device 10, and the ultrafiltration membrane 11 is performed. In the UV oxidation device 9, the TOC is decomposed into an organic acid by ultraviolet rays having a wavelength of 185 nm emitted from a UV lamp, and further decomposed to a CO 2 level. The decomposed organic acid and CO 2 are removed in the subsequent non-regeneration type mixed bed ion exchange apparatus 10. In the ultrafiltration membrane 11, the fine particles are removed, and the effluent particles of the non-regeneration type mixed bed type ion exchange device 10 are also removed, thereby obtaining secondary pure water (ultra-pure water) W5. After the secondary pure water W5 is supplied to the use point UP, the unused portion is returned to the sub tank 8.
於如上所述的超純水製造裝置1的運轉中，子系統3的處理水即二次純水（超純水）W5的硼濃度由於通常大幅度低於處理水W2的硼濃度[B1]，故而電去離子裝置7的處理水W2的硼濃度[B1]若考慮到子系統3中的減少部分而為要求水質以下的水準，則視為在水質上「無問題」而連續運轉即可。例如，若二次純水W5的硼的要求水質為0.1 ppt、電去離子裝置7的硼去除率為99.99%且可利用子系統3來降低至1/10以下，則若一次純水W1的硼濃度為10 ppb以下便可連續運轉。In the operation of the ultrapure water production apparatus 1 as described above, the boron concentration of the secondary pure water (ultra-pure water) W5 of the treated water of the subsystem 3 is usually significantly lower than the boron concentration of the treated water W2 [B1]. Therefore, if the boron concentration [B1] of the treated water W2 of the electrodeionization apparatus 7 is a level below the required water quality in consideration of the reduced portion in the subsystem 3, it is considered that the water quality is "no problem" and can be continuously operated. . For example, if the required water quality of boron of the secondary pure water W5 is 0.1 ppt, the boron removal rate of the electrodeionization apparatus 7 is 99.99%, and the subsystem 3 can be used to reduce it to 1/10 or less, if the pure water W1 is once Continuous operation is possible with a boron concentration of 10 ppb or less.
而且，由於長期的使用，非再生型混合床式離子交換裝置10的硼去除能力下降，硼容易洩露至二次純水W5中，因此較佳為定期地進行二次純水W5的精密分析，實際測量二次純水W5的實際的硼濃度。並且，若將該硼濃度的實測值[B2]與處理水W2的硼濃度[B1]進行對比，而存在硼濃度的實測值[B2]的值相對於處理水W2的硼濃度[B1]的減少率下降的傾向，則即便於硼濃度[B2]超過0.1 ppt之前亦較佳為更換非再生型混合床式離子交換裝置10。如上所述，能夠防止硼向二次純水W5中的洩漏於未然。而且，因是在實際上顯示出非再生型混合床式離子交換裝置10的性能下降的傾向之後再更換非再生型混合床式離子交換裝置10，因此其更換頻率亦少，故而經濟性亦優異。Further, since the boron removal ability of the non-regeneration type mixed bed type ion exchange apparatus 10 is lowered and the boron is easily leaked into the secondary pure water W5 due to long-term use, it is preferable to perform the precise analysis of the secondary pure water W5 periodically. The actual boron concentration of the secondary pure water W5 was actually measured. Further, when the measured value [B2] of the boron concentration is compared with the boron concentration [B1] of the treated water W2, the value of the measured value [B2] of the boron concentration is relative to the boron concentration [B1] of the treated water W2. The tendency of the decrease rate to decrease is preferably to replace the non-regeneration type mixed bed type ion exchange apparatus 10 even before the boron concentration [B2] exceeds 0.1 ppt. As described above, it is possible to prevent leakage of boron into the secondary pure water W5. In addition, since the non-regeneration type mixed bed type ion exchange apparatus 10 is replaced after the performance of the non-regeneration type mixed bed type ion exchange apparatus 10 is actually lowered, the frequency of replacement is small, and the economy is excellent. .
特別是於本實施形態中，作為電去離子裝置7，將該處理水W2的一部分作為濃縮水W3，在與除鹽室26的通水方向相反的方向上以對流一次流過方式通入濃縮室25中，並自濃縮室25中將濃縮排水W4排出至系統外，因此越靠近除鹽室26的取出側，濃縮室25的濃縮水W3中的離子濃度越低，由濃度擴散所引起的對除鹽室26的影響變小，因此硼的去除率提高。另外，電去離子裝置7的供水由於是一次純水W1，故而離子少（例如電阻较大而为18 MΩ・cm左右），因此需要大量的電流，但藉由在除鹽室26及濃縮室25的兩者中填充離子交換體，可使除鹽室26及濃縮室25中的電阻下降，從而能夠減少運轉費用。In the present embodiment, in particular, a part of the treated water W2 is used as the concentrated water W3 as the electro-deionization device 7, and is condensed in a direction opposite to the water-passing direction of the desalination chamber 26 by convection. In the chamber 25, the concentrated drain W4 is discharged from the concentrating chamber 25 to the outside of the system. Therefore, the closer to the take-out side of the desalination chamber 26, the lower the ion concentration in the concentrated water W3 of the concentrating chamber 25 is caused by the concentration diffusion. The influence on the desalination chamber 26 becomes small, so the removal rate of boron is increased. Further, since the water supply to the electrodeionization apparatus 7 is the primary pure water W1, the amount of ions is small (for example, the resistance is large and is about 18 MΩ·cm), so a large amount of current is required, but by the desalination chamber 26 and the concentrating chamber. When the ion exchanger is filled in both of 25, the electric resistance in the desalting compartment 26 and the concentrating compartment 25 can be lowered, and the running cost can be reduced.
進而，於本實施形態中，由於使用經氮封者作為子儲槽8，故而可抑制空氣中的二氧化碳或氧的溶解，從而抑制二次純水W5的比電阻的下降。Further, in the present embodiment, since the nitrogen sealer is used as the sub-tank 8, the dissolution of carbon dioxide or oxygen in the air can be suppressed, and the decrease in the specific resistance of the secondary pure water W5 can be suppressed.
繼而，基於圖4，對本發明的第二實施形態的超純水製造裝置進行說明。Next, an ultrapure water production apparatus according to a second embodiment of the present invention will be described based on Fig. 4 .
第二實施形態的超純水製造裝置設為如下構成：於所述的第一實施形態中，具備一次純水系統2及子系統3，且子系統3具有：UV氧化裝置9、陰離子交換樹脂裝置12、除氣膜13、非再生型混合床式離子交換裝置10及超濾膜（UF膜）11。The ultrapure water production apparatus according to the second embodiment is configured as follows: in the first embodiment, the primary pure water system 2 and the subsystem 3 are provided, and the subsystem 3 has a UV oxidation device 9, an anion exchange resin. The apparatus 12, the degassing membrane 13, the non-regeneration type mixed bed type ion exchange apparatus 10, and the ultrafiltration membrane (UF membrane) 11.
藉由如上所述般於子系統中設置陰離子交換樹脂裝置12及除氣膜13，則雖電去離子裝置7其自身不具有氣密性故而存在微量的二氧化碳或氧混入至一次純水W1中的風險，但由於能夠利用陰離子交換樹脂裝置12來去除CO2 ，並且利用除氣膜13來去除溶存氧等殘存的氣體成分，故而能夠減少溶存氣體成分。By providing the anion exchange resin device 12 and the degassing film 13 in the subsystem as described above, although the electrodeionization device 7 does not have airtightness itself, a small amount of carbon dioxide or oxygen is mixed into the primary pure water W1. However, since the anion exchange resin device 12 can be used to remove CO 2 and the degassing film 13 can be used to remove residual gas components such as dissolved oxygen, the dissolved gas component can be reduced.
以上，已基於所述實施形態對本發明進行了說明，但本發明並不限定於所述實施形態，可進行多種的變形實施，一次純水系統2與子系統3並不限定於本實施例的構成，可設為多種構成。例如，一次純水系統2中亦可將逆滲透膜（RO）裝置4串聯為2段。另外，第一實施形態中，雖於子系統3中設置有UV氧化裝置9，但視情況亦可不設置UV氧化裝置9。進而，子儲槽8雖使用經氮封者，但亦可為通常的子儲槽，視情況亦可不使用子儲槽8。進而，亦可為了二次純水W5的水質測定用途而設置比電阻計等其他的水質分析機構，原地測量二次純水W5的水質，若比電阻較既定的設定值而言下降，則更換非再生型混合床式離子交換裝置10。 [實施例]Although the present invention has been described above based on the above embodiments, the present invention is not limited to the above-described embodiments, and various modifications can be made. The primary pure water system 2 and the subsystem 3 are not limited to the embodiment. The configuration can be various configurations. For example, the reverse osmosis membrane (RO) unit 4 may be connected in series to two stages in the primary pure water system 2. Further, in the first embodiment, the UV oxidizer 9 is provided in the subsystem 3, but the UV oxidizer 9 may not be provided as the case may be. Further, although the sub-tank 8 is made of a nitrogen sealer, it may be a normal sub-tank, and the sub-tank 8 may not be used as the case may be. Furthermore, other water quality analysis means such as a resistance meter may be provided for the water quality measurement use of the secondary pure water W5, and the water quality of the secondary pure water W5 may be measured in situ, and if the specific resistance is lower than a predetermined set value, The non-regenerative mixed bed type ion exchange device 10 is replaced. [Examples]
以下，列舉實施例及比較例，對本發明進行更具體的說明，但本發明並不限定於下述實施例。Hereinafter, the present invention will be more specifically described by way of examples and comparative examples, but the present invention is not limited to the following examples.
[實施例1] 利用包括逆滲透膜（RO）裝置4及再生型混合床式離子交換裝置5的一次純水系統2，對靜岡縣榛原郡吉田鎮的自來水（被處理水）W進行處理。利用硼監測器6來測定該一次純水W1的硼濃度，另一方面，以電去離子裝置7進行處理，將處理水W2儲留於子儲槽8中。利用依序具備UV氧化裝置9、陰離子交換樹脂裝置12、除氣膜13、非再生型混合床式離子交換裝置10及超濾膜（UF膜）11的子系統3，對該子儲槽8內的處理水W2進行通水處理，從而製造二次純水W5。[Example 1] The tap water (treated water) W of Yoshida Town, Sugawara-gun, Shizuoka Prefecture was treated with a primary pure water system 2 including a reverse osmosis membrane (RO) apparatus 4 and a regenerative mixed bed type ion exchange apparatus 5. . The boron monitor 6 is used to measure the boron concentration of the primary pure water W1. On the other hand, the treatment is performed by the electrodeionization device 7, and the treated water W2 is stored in the sub-tank 8. The sub-reservoir 8 is provided by a subsystem 3 including a UV oxidizing device 9, an anion exchange resin device 12, a degassing film 13, a non-regeneration type mixed bed type ion exchange device 10, and an ultrafiltration membrane (UF membrane) 11 in this order. The treated water W2 in the inside is subjected to water treatment to produce secondary pure water W5.
此外，電去離子裝置7是使用以下裝置。 電去離子裝置：栗田工業（股）製造的KCDI-UPz，於除鹽室26、濃縮室25及電極室27、電極室28中填充離子交換樹脂，將處理水W2的一部分以對流方式通入至濃縮室25中，硼去除率為99.99%以上。Further, the electrodeionization device 7 uses the following devices. Electrodeionization apparatus: KCDI-UPz manufactured by Kurita Industrial Co., Ltd., is filled with ion exchange resin in the desalting compartment 26, the concentrating compartment 25, the electrode compartment 27, and the electrode compartment 28, and a part of the treated water W2 is convectively introduced. In the concentration chamber 25, the boron removal rate is 99.99% or more.
於該超純水製造裝置的運轉中，硼監測器6的值穩定為1 ppb～5 ppb，從而推測處理水W2的硼濃度為0.1 ppt以下，故而連續運轉。對該處理水W2的硼濃度進行每月1次的精密分析，硼濃度穩定為0.1 ppt以下，二次純水W5的硼濃度亦為0.1 ppt以下。而且，二次純水W5的比電阻值大致為18.2 MΩ・cm，為超純水水準，即便經過3年亦穩定，從而於3年間不需要更換子系統3的非再生型混合床式離子交換裝置10。In the operation of the ultrapure water production apparatus, the value of the boron monitor 6 is stabilized at 1 ppb to 5 ppb, and the boron concentration of the treated water W2 is estimated to be 0.1 ppt or less, so that the operation is continuously performed. The boron concentration of the treated water W2 is precisely analyzed once a month, the boron concentration is stabilized at 0.1 ppt or less, and the boron concentration of the secondary pure water W5 is also 0.1 ppt or less. Further, the specific resistance of the secondary pure water W5 is approximately 18.2 MΩ·cm, which is an ultrapure water level, and is stable even after three years, so that the non-regeneration type mixed bed ion exchange of the subsystem 3 does not need to be replaced for three years. Device 10.
[比較例1] 於實施例1中，不使用電去離子裝置7，於非再生型混合床式離子交換裝置10的後段設置硼監測器6來進行監視。[Comparative Example 1] In the first embodiment, the boron ion monitor 6 was provided in the subsequent stage of the non-regeneration type mixed bed type ion exchange apparatus 10 without using the electrodeionization apparatus 7, and monitoring was performed.
於該超純水製造裝置的運轉中，由於在3週內硼監測器6的值超過1 ppb，故而必須更換非再生型混合床式離子交換裝置10。In the operation of the ultrapure water production apparatus, since the value of the boron monitor 6 exceeds 1 ppb within 3 weeks, the non-regeneration type mixed bed type ion exchange apparatus 10 must be replaced.
[比較例2] 實施例1中，雖於子系統3的非再生型混合床式離子交換裝置10的後段設置硼監測器6來進行監視，但無法偵檢硼濃度，難以根據非再生型混合床式離子交換裝置10的穿透來判斷更換時期。[Comparative Example 2] In the first embodiment, the boron monitor 6 is provided in the subsequent stage of the non-regeneration type mixed bed type ion exchange apparatus 10 of the subsystem 3 for monitoring, but the boron concentration cannot be detected, and it is difficult to mix according to the non-regeneration type. The penetration of the bed type ion exchange device 10 determines the replacement period.
[比較例3] 於實施例1中，除了在一次純水裝置2中不使用電去離子裝置7，且於子系統3的UV氧化裝置9的後段配置電去離子裝置以外，以相同的方式利用硼監測器6進行監視。[Comparative Example 3] In Example 1, except that the electrodeionization device 7 was not used in the primary pure water device 2, and the electrodeionization device was disposed in the latter stage of the UV oxidation device 9 of the subsystem 3, in the same manner. Monitoring is performed using the boron monitor 6.
於如上所述的超純水製造裝置的運轉中，硼監測器6的值穩定為1 ppb～5 ppb，但流入子系統3的水的硼濃度大，而且設置於子系統3中的電去離子裝置的處理水的水壓低且不穩定，因此設置於該後段的陰離子交換樹脂裝置12等中的處理亦不穩定，因此二次純水W5的每月1次的精密分析中硼濃度的變動大，難以根據非再生型混合床式離子交換裝置10的穿透來判斷更換時期。另外，亦確認到電去離子裝置的性能的下降，其被視為受UV氧化裝置9中所產生的氧化性物質的影響。In the operation of the ultrapure water manufacturing apparatus as described above, the value of the boron monitor 6 is stabilized at 1 ppb to 5 ppb, but the concentration of boron flowing into the subsystem 3 is large, and the electricity set in the subsystem 3 is set. Since the water pressure of the treated water in the ion device is low and unstable, the treatment in the anion exchange resin device 12 or the like provided in the subsequent stage is also unstable. Therefore, the variation of the boron concentration in the precision analysis of the secondary pure water W5 once a month is performed. Large, it is difficult to judge the replacement period based on the penetration of the non-regenerative mixed bed type ion exchange device 10. In addition, a decrease in the performance of the electrodeionization device was also confirmed, which was considered to be affected by the oxidizing substance generated in the UV oxidizing device 9.
1‧‧‧超純水製造裝置
2‧‧‧一次純水系統
3‧‧‧子系統
4‧‧‧逆滲透膜（RO）裝置
5‧‧‧再生型混合床式離子交換裝置
6‧‧‧硼監測器（硼濃度測定機構）
7‧‧‧電去離子裝置
8‧‧‧子儲槽
9‧‧‧UV氧化裝置
10‧‧‧非再生型混合床式離子交換裝置
11‧‧‧超濾膜（UF膜）
12‧‧‧陰離子交換樹脂裝置
13‧‧‧除氣膜
21‧‧‧陽極
22‧‧‧陰極
23‧‧‧陰離子交換膜
24‧‧‧陽離子交換膜
25‧‧‧濃縮室
26‧‧‧除鹽室
27‧‧‧電極室（陽極室）
28‧‧‧電極室（陰極室）
W‧‧‧被處理水
W1‧‧‧一次純水
W2‧‧‧處理水
W3‧‧‧濃縮水
W4‧‧‧濃縮排水
W5‧‧‧二次純水（超純水）
P‧‧‧泵（供給泵）
UP‧‧‧使用點1‧‧‧Ultra pure water manufacturing equipment
2‧‧‧A pure water system
3‧‧‧ subsystem
4‧‧‧ Reverse osmosis membrane (RO) device
5‧‧‧Regeneration type mixed bed ion exchange unit
6‧‧ ‧ boron monitor (boron concentration measuring mechanism)
7‧‧‧Electrical deionization device
8‧‧‧ sub-storage tank
9‧‧‧UV oxidation unit
10‧‧‧Non-regeneration type mixed bed ion exchange unit
11‧‧‧Ultrafiltration membrane (UF membrane)
12‧‧‧ Anion exchange resin device
13‧‧‧Degas film
21‧‧‧Anode
22‧‧‧ cathode
23‧‧‧ Anion exchange membrane
24‧‧‧Cation exchange membrane
25‧‧‧Concentration room
26‧‧‧Desalting room
27‧‧‧Electrode chamber (anode chamber)
28‧‧‧electrode chamber (cathode chamber)
W‧‧‧ treated water
W1‧‧‧A pure water
W2‧‧‧ treated water
W3‧‧‧ Concentrated water
W4‧‧‧Concentrated drainage
W5‧‧‧Second pure water (ultra pure water)
P‧‧‧ pump (supply pump)
UP‧‧‧ use point
圖1是表示本發明的第一實施形態的超純水製造裝置的流程圖。 圖2是表示所述第一實施形態的超純水製造裝置中使用的電去離子裝置的構成的示意性剖面圖。 圖3是表示圖2的電去離子裝置的系統圖。 圖4是表示本發明的第二實施形態的超純水製造裝置的流程圖。Fig. 1 is a flowchart showing an ultrapure water producing apparatus according to a first embodiment of the present invention. FIG. 2 is a schematic cross-sectional view showing a configuration of an electrodeionization apparatus used in the ultrapure water production apparatus according to the first embodiment. Fig. 3 is a system diagram showing the electrodeionization apparatus of Fig. 2; Fig. 4 is a flow chart showing an apparatus for producing an ultrapure water according to a second embodiment of the present invention.
1‧‧‧超純水製造裝置 1‧‧‧Ultra pure water manufacturing equipment
2‧‧‧一次純水系統 2‧‧‧A pure water system
3‧‧‧子系統 3‧‧‧ subsystem
4‧‧‧逆滲透膜(RO)裝置 4‧‧‧ Reverse osmosis membrane (RO) device
5‧‧‧再生型混合床式離子交換裝置 5‧‧‧Regeneration type mixed bed ion exchange unit
6‧‧‧硼監測器(硼濃度測定機構) 6‧‧ ‧ boron monitor (boron concentration measuring mechanism)
7‧‧‧電去離子裝置 7‧‧‧Electrical deionization device
8‧‧‧子儲槽 8‧‧‧ sub-storage tank
9‧‧‧UV氧化裝置 9‧‧‧UV oxidation unit
10‧‧‧非再生型混合床式離子交換裝置 10‧‧‧Non-regeneration type mixed bed ion exchange unit
11‧‧‧超濾膜(UF膜) 11‧‧‧Ultrafiltration membrane (UF membrane)
W‧‧‧被處理水 W‧‧‧ treated water
W1‧‧‧一次純水 W1‧‧‧A pure water
W2‧‧‧處理水 W2‧‧‧ treated water
W5‧‧‧二次純水(超純水) W5‧‧‧Second pure water (ultra pure water)
P‧‧‧泵(供給泵) P‧‧‧ pump (supply pump)
UP‧‧‧使用點 UP‧‧‧ use point
Claims (10)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2016014922A JP6119886B1 (en) | 2016-01-28 | 2016-01-28 | Ultrapure water production apparatus and operation method of ultrapure water production apparatus |
| JP2016-014922 | 2016-01-28 |
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| Publication Number | Publication Date |
|---|---|
| TW201726557A true TW201726557A (en) | 2017-08-01 |
| TWI710529B TWI710529B (en) | 2020-11-21 |
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| TW105129663A TWI710529B (en) | 2016-01-28 | 2016-09-13 | Ultrapure water production device and operation method of ultrapure water production device |
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| JP (1) | JP6119886B1 (en) |
| KR (1) | KR102602540B1 (en) |
| CN (1) | CN108602705A (en) |
| SG (1) | SG11201806360WA (en) |
| TW (1) | TWI710529B (en) |
| WO (1) | WO2017130454A1 (en) |
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| JP2019089018A (en) * | 2017-11-14 | 2019-06-13 | オルガノ株式会社 | Method of operating pure production apparatus and pure water production apparatus |
| JP7454330B2 (en) | 2018-06-20 | 2024-03-22 | オルガノ株式会社 | Boron removal method in treated water, boron removal system, ultrapure water production system, and boron concentration measurement method |
| KR102637681B1 (en) * | 2018-06-27 | 2024-02-15 | 노무라마이크로사이엔스가부시키가이샤 | Electric deionization device, ultrapure water production system, and ultrapure water production method |
| JP7192519B2 (en) * | 2019-01-22 | 2022-12-20 | 栗田工業株式会社 | Ultra-pure boron-removed ultra-pure water production apparatus and ultra-pure boron-removed ultra-pure water production method |
| JP2020142178A (en) * | 2019-03-05 | 2020-09-10 | 栗田工業株式会社 | Ultrapure water production apparatus and method for operating the ultrapure water production apparatus |
| JP7289206B2 (en) * | 2019-03-13 | 2023-06-09 | オルガノ株式会社 | Boron removal device, boron removal method, pure water production device, and pure water production method |
| CN110185676A (en) * | 2019-06-05 | 2019-08-30 | 深圳市粤永能源环保科技有限公司 | A kind of pure water hydraulics system |
| CN110217924A (en) * | 2019-06-21 | 2019-09-10 | 长沙如洋环保科技有限公司 | A kind of use for laboratory water purification machine |
| JP7129965B2 (en) * | 2019-12-25 | 2022-09-02 | 野村マイクロ・サイエンス株式会社 | Pure water production method, pure water production system, ultrapure water production method, and ultrapure water production system |
| JP6863510B1 (en) * | 2019-12-25 | 2021-04-21 | 栗田工業株式会社 | Control method of ultrapure water production equipment |
| JP7368310B2 (en) * | 2020-05-20 | 2023-10-24 | オルガノ株式会社 | Boron removal equipment and boron removal method, and pure water production equipment and pure water production method |
| CN112337323B (en) * | 2020-09-28 | 2021-06-15 | 南京工业大学 | PVDF (polyvinylidene fluoride) polymer separation membrane and preparation method thereof |
| JP2022060806A (en) * | 2020-10-05 | 2022-04-15 | オルガノ株式会社 | Pure water production system and pure water production method |
| JP7205576B1 (en) | 2021-07-19 | 2023-01-17 | 栗田工業株式会社 | Operation method of pure water production system |
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| JPH08117744A (en) * | 1994-10-21 | 1996-05-14 | Nomura Micro Sci Co Ltd | Method for detecting break of ion exchange apparatus |
| JP3426072B2 (en) * | 1996-01-17 | 2003-07-14 | オルガノ株式会社 | Ultrapure water production equipment |
| JP3794268B2 (en) * | 2001-01-05 | 2006-07-05 | 栗田工業株式会社 | Electrodeionization apparatus and operation method thereof |
| JP2003266097A (en) * | 2002-03-13 | 2003-09-24 | Kurita Water Ind Ltd | Ultrapure water making apparatus |
| JP3794354B2 (en) * | 2002-07-08 | 2006-07-05 | 栗田工業株式会社 | Electrodeionization equipment |
| JP2004261643A (en) * | 2003-02-14 | 2004-09-24 | Kurita Water Ind Ltd | Electrodeionization apparatus, and operating method therefor |
| JP2009028695A (en) * | 2007-07-30 | 2009-02-12 | Kurita Water Ind Ltd | Apparatus and method for manufacturing pure water |
| JP4993136B2 (en) * | 2008-08-08 | 2012-08-08 | 栗田工業株式会社 | Pure water production apparatus and pure water production method |
| JP5617231B2 (en) * | 2009-11-27 | 2014-11-05 | 栗田工業株式会社 | Method and apparatus for purifying ion exchange resin |
| EP2735546B1 (en) * | 2012-11-21 | 2018-02-07 | Ovivo Inc. | Treatment of water, particularly for obtaining ultrapure water |
| JP6362299B2 (en) * | 2013-03-27 | 2018-07-25 | 栗田工業株式会社 | Operation method of ion exchange resin apparatus and ion exchange resin apparatus |
| JP6205865B2 (en) * | 2013-06-04 | 2017-10-04 | 栗田工業株式会社 | Operation management method for pure water production equipment |
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| JP6119886B1 (en) | 2017-04-26 |
| KR102602540B1 (en) | 2023-11-15 |
| WO2017130454A1 (en) | 2017-08-03 |
| KR20180103964A (en) | 2018-09-19 |
| TWI710529B (en) | 2020-11-21 |
| CN108602705A (en) | 2018-09-28 |
| JP2017131846A (en) | 2017-08-03 |
| SG11201806360WA (en) | 2018-08-30 |
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