TW201127491A - Ion-exchange device, process and equipment for producing same, and method and device for forming ion-exchange resin layer - Google Patents

Ion-exchange device, process and equipment for producing same, and method and device for forming ion-exchange resin layer Download PDF

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TW201127491A
TW201127491A TW99121231A TW99121231A TW201127491A TW 201127491 A TW201127491 A TW 201127491A TW 99121231 A TW99121231 A TW 99121231A TW 99121231 A TW99121231 A TW 99121231A TW 201127491 A TW201127491 A TW 201127491A
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Taiwan
Prior art keywords
ion exchange
exchange resin
pump
container
water
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TW99121231A
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Chinese (zh)
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TWI494166B (en
Inventor
Shin Sato
Masamitsu Ikeda
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Kurita Water Ind Ltd
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Priority claimed from JP2009155660A external-priority patent/JP5391874B2/en
Priority claimed from JP2009266401A external-priority patent/JP5407801B2/en
Application filed by Kurita Water Ind Ltd filed Critical Kurita Water Ind Ltd
Publication of TW201127491A publication Critical patent/TW201127491A/en
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Publication of TWI494166B publication Critical patent/TWI494166B/en

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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/42Treatment of water, waste water, or sewage by ion-exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J47/00Ion-exchange processes in general; Apparatus therefor
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/02Non-contaminated water, e.g. for industrial water supply
    • C02F2103/04Non-contaminated water, e.g. for industrial water supply for obtaining ultra-pure water

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

Abstract

A process for producing an ion-exchange device is provided in which ion-exchange resins are prevented from being fouled by airborne dust. An anion-exchange resin and a cation-exchange resin are purified and metered respectively through receiving tanks (11, 21), purification columns (14, 24), storage tanks (16, 26), and metering tanks (19, 29), mixed together in a mixing tank (30), and then filled into a vessel (33). The metering tanks (19, 29), the mixing tank (30), and the vessel to be filled (33) are disposed in a clean room (41) having a degree of cleanliness of 10,000 or higher. The produced ion-exchange device is subjected to a water-passing test, and the effluent water is analyzed in a high-cleanliness clean room (42) having a degree of cleanliness of 1,000 or higher.

Description

201127491 六、發明說明: 【發明所屬之技術領域】 本:發明係關於在容器充塡離子交換樹脂而製作離子交 換裝置之方法及設備,特別是關於適用於超純水製造過程 等所使用之離子交換裝置的製作之離子交換裝置製作方法 及設備。本發明是關於藉由該方法及設備所製作之離子交 換裝置。此外’本發明係關於在容器內充塡離子交換樹脂 而形成離子交換樹脂層之方法及裝置。本發明係關於具有 藉由該方法及裝置所形成之離子交換樹脂層的離子交換裝 置。 【先前技術】 以往’作爲離子交換裝置大多是採用以下的構造(特 別是固定式離子交換裝置)。這種離子交換裝置的構造, 是將陽離子交換樹脂、陰離子交換樹脂、其等的混合樹脂 或其等與其他樹脂的混合樹脂充塡於容器內而形成離子交 換樹脂層’讓被處理液通過而進行離子交換處理。而且, 離子交換樹脂層飽和之後,停止讓被處理液通過,讓再生 液通過而將離子交換樹脂層予以再生,接著讓洗淨液通過 而進行洗淨後’再度開始讓被處理液通過而再度開始進行 離子交換處理。 然而’像追樣父互且反覆進行離子交換處理和再生之 離子父換裝置’在進行離子交換樹脂層的再生時,有無法 進行離子交換處理的缺點。因此是取代這種離子交換裝置 -5- 201127491 而有一種單元交換式的離子交換裝置, 的主體容器內充塡離子交換樹脂之拆裝 充塡單元,將其搬運至現場後安裝於離 離子交換處理,當離子交換樹脂層飽和 置將離子交換樹脂充塡單元卸下,更換 行離子交換處理,另一方面卸下的離子 被回收,將使用過的離子交換樹脂按照 用。 逭種單元交換式的離子交換裝置是 換裝置卸下的離子交換樹脂充塡單元不 棄之非再生型離子交換裝置、將離子交 予以再使用之再生使用型離子交換裝置 包含:對每個回收的單元分別將離子交 :從單元收集離子交換樹脂而予以再生 交換樹脂充塡於單元而搬運至現場待機 換裝置而進行離子交換處理的方式等等 專利文獻1 (日本特開平9-70546號 子交換單元,是在主體容器充塡離子交 讓從容器突出的管連接於原水管、處理 2圖係該文獻所記載的離子交換單元u。 ’是在具有開口部la的容器1內充塡調〗 脂2。在開口部ia裝設蓋6。在蓋6上設: 導入口 3,並將原水導入路4和處理水取 狀。原水導入路4是插到容器I內的底部 其是採用在可搬式 式的離子交換樹脂 子交換裝置而進行 後,從離子交換裝 新的單元而繼續進 交換樹脂充塡單元 需要而進行再生使 包含:將從離子交 進行再生而直接廢 換樹脂進行再生而 。在後者的情況是 換樹脂再生的方式 ,將再生後的離子 後,安裝於離子交 〇 公報)所記載的離 換樹脂而構成,是 水管等來使用。第 該離子交換單元U 整後的離子交換樹 有離子交換樹脂的 出路5設置成貫穿 ,在其下端設置過 -6- 201127491 爐器4a。 安裝在處理水取出路5的下端之過濾器5 a是位於容器1 內的上部。 離子交換樹脂2是透過樹脂導入口 3充塡於容器1內。 導入口 3之後被密閉。樹脂導入口 3,是在連接時用來進行 排水、排出空氣等,而在離子交換處理時通常是密閉的。 該離子交換單元,是以在連結器4b、5b的位置被切離 的狀態施以密封並搬運至現場進行安裝。而且,利用連結 器4b、5b和伸縮接頭7、8連接,以進行原水的導入及處理 水(超純水)的取出(參照段落0 0 2 1〜0 0 2 2 )。 作爲離子交換樹脂,是包含:將陽離子交換樹脂或陰 離子交換樹脂單獨充塡的情況,將兩者以容量比1 : 3〜3 : 1的比例混合充塡的情況。(段落0 0 1 8 ) 安裝於離子交換系統之離子交換單元U,是將原水從 離子交換裝置的原水流路(未圖示)通過原水導入路4、 第1過濾器4a而導入容器1,藉由通過離子交換樹脂層2進 行離子交換;處理水則是在第2過濾器5 a收集後從處理水 取出路5通過離子交換裝置的處理水流路(未圖示)而被 取出。當離子交換樹脂2飽和之後,將離子交換單元U利用 連結器4b、5b卸下而更換成新的單元,以繼續進行離子交 換處理。 使用過的離子交換單元U,是以卸下的狀態搬運而回 收’按照需要將離子交換樹脂取出而予以再生,再生後的 離子交換樹脂再度充塡於容器1而構成離子交換裝置,以 -7- 201127491 再度供離子交換處理。 爲了在上述離子交換單元U的主體容器1充塡離子交換 樹脂’是讓離子交換樹脂分散於水中而以漿體狀導入,挾 帶的水藉由過濾器4a、5 a分離而排出。依據此方法,要在 主體容器1充塡一定量的離子交換樹脂會有困難。 在專利文獻4 (日本特開2002-28501號)揭示的例子 ’是在離子交換樹脂移動容器收容離子交換樹脂後搬運至 現場,在現場充塡於離子交換裝置而供進行離子交換,當 飽和後則從'離子交換裝置將離子交換樹脂取出而收容於離 子交換樹脂移動容器之後,搬運至再生裝置之設置場所, 將再生後的離子交換樹脂再度收容於離子交換樹脂移動容 器而搬運至現場。作爲這種離子交換樹脂移動容器,是具 備與容器內的過濾構件(相當於過濾器)連接的配管,離 子交換樹脂是分散於水中而以漿體狀導入,挾帶水則藉由 過濾構件分離而排出,藉此來充塡離子交換樹脂,但並未 揭示使離子交換樹脂充塡量成爲一定量。 離子交換樹脂,在乾燥狀態下要量取一定的樹脂量是 容易的。但在離子交換時,由於離子交換樹脂是充塡於液 相來使用,又是以離子交換樹脂層的容積爲基準來表示特 性並進行處理’因此充塡於容器之樹脂量’是要求以存在 於液相的狀態成爲一定容量。在此情況’離子交換樹脂是 以分散於水中之漿體狀來導入充塡於容器’但由於無法使 漿體中的離子交換樹脂濃度成爲一定’即使量取漿體仍無 法充塡一定量的樹脂。 -8 - 201127491 就充塡一定量樹脂的方法而言,事先量取要充塡的樹 脂再進行充塡的方法,必須事先量取一定量之再生後的樹 脂’再讓其於水中分散成漿體狀而導入,因此須採用複雜 步驟的組合而變得麻煩,實際上會有困難。又對每個容器 測定樹脂重量的方法,由於所存在的水量會影響重量的計 測’實際上難以進行正確的計量。再者,利用目視來計測 樹脂充塡量的方法,必須反覆進行停止通液和目視計測, 又若容器大型化而使樹脂充塡量變多,則難以進行正確的 5十測,而有問題點存在著。 一般而言,若在一定容積的容器內將內容物充塡至裝 滿爲止’其充塡量的容量會成爲一定。在專利文獻1、4, 充塡於容器內之離子交換樹脂層並未裝滿,在容器的上部 殘留有未形成離子交換樹脂層的空間。在如此般具有餘裕 的容器中,雖難以充塡一定量的離子交換樹脂,但藉由將 容器及配置於其中之過濾器和配管等的構造、配置等予以 定型化’其容量成爲一定容積,若在這種一定容積的容器 內將離子交換樹脂充塡至裝滿爲止,離子交換樹脂層的容 量應會成爲一定。 若在一般容器以漿體狀導入離子交換樹脂,無用的水 也會被導入。由於難以使漿體中的離子交換樹脂濃度成爲 一定’要使所充塡的離子交換樹脂容量成爲一定是困難的 。相對於此’如專利文獻1、2所示,具備與容器內的過濾 器連接之配管,使離子交換樹脂以分散於水中之浆體狀導 入,將挾帶水藉由過爐器分離排出,藉此來充塡離子交換 -9 - 201127491 樹脂的方法,若裝滿時,所充塡之離子交換樹脂的容量應 會成爲一定。 然而,將離子交換樹脂漿體藉由泵輸送的情況,若裝 滿後仍藉由泵進行輸送,樹脂的充塡密度變得過高而變得 無法進行通水,或發生樹脂破碎,或過濾器和配管容易堵 塞,而存在諸多問題點。在此情況,雖可考慮根據供應漿 體的壓力上昇來檢測出容器內之離子交換樹脂已裝滿以停 止供應漿體,但爲了正確地檢測出壓力上昇以停止供應漿 體’必須採用複雜的裝置和控制機構等,而且很難將漿體 中的離子交換樹脂從挾帶水分離而形成充塡密度均一的充 塡層,因此存在著諸多的問題。 在專利文獻5 (日本特開2002-22 1 1 60號)記載著,作 爲流體壓驅動式泵是使用空氣壓驅動式隔膜泵。該空氣壓 驅動式隔膜泵是屬於雙隔膜式的泵,在兩個泵室分別設有 隔膜’接合於主軸(貫穿中間壁且可滑動)的前端而形成 一體化’藉此可進行往復移動。然而未並揭示出使離子交 換樹脂充塡量成爲一定量。 在專利文獻6 (日本特開2007-305019號)揭示一種控 制機構’在空氣壓驅動式泵等,當泵驅動用的空氣壓到達 既定壓力的時點,解除作用於泵之空氣壓而停止驅動泵。 然而該控制機構’是在起因於隔膜等的損傷而發生空轉, 造成驅動用空氣壓上昇的情況,用來檢測出該空氣壓的上 昇而停止驅動泵,其並未揭示出使離子交換樹脂充塡量成 爲一定量。 -10- 201127491 在下述專利文獻2、3記載著用來精製處理離子交換樹 脂之方法及精製用的藥劑。 〔專利文獻〕 專利文獻1:日本特開平9-70546號公報 專利文獻2:日本特開平5_15789號公報 專利文獻3:日本特開平9_2〇ι539號公報 專利文獻4:日本特開2〇〇2_285〇1號 專利文獻5:日本特開2〇〇2_22116〇號 專利文獻6:日本特開2〇〇7_3〇5〇19號 在半導體產業’在半導體製品的洗淨及其他用途會用 到超純水,對該超純水的水質要求是越來越嚴格,例如, 金屬濃度爲lppt以下,視情況也會有要求O.lppt以下的超 高水質的情況。 在這種情況’爲了防止來自離子交換裝置之金屬等的 滲漏’必須在離子交換裝置充塡高度精製的離子交換樹脂 〇 然而,以往是在大氣中將高度精製的離子交換樹脂充 塡於容器,因此空氣中的塵埃會混入,而可能使離子交換 樹脂發生微量的污染。 【發明內容】 本發明的第1目的在於,提供一種可防止空氣中的塵 埃污染離子交換樹脂之離子交換裝置的製作方法及設備, -11 - 201127491 以及使用該方法及設備所製作出之離子交換裝置。 本發明的第2目的在於提供:藉由簡單的機構和操作 能在短時間正確地將一定量的離子交換樹脂充塡於容器而 形成離子交換樹脂層,且能防止離子交換樹脂之高密度充 塡和破碎或配管的堵塞之離子交換層的形成方法及裝置, 以及具有使用該方法及裝置所形成之離子交換樹脂層的離 子交換裝置。 第1態樣之離子交換裝置的製作方法及設備,是將精 製處理後的離子交換樹脂充塡於容器來製作離子交換裝置 之方法,其特徵在於:將離子交換樹脂充塡於該容器之充 塡步驟是在無塵室內進行。 第2態樣之離子交換裝置的製作方法及設備,是在第1 態樣中,將離子交換樹脂以不接觸大氣的狀態進行精製處 理後,經由配管而以不接觸大氣的狀態朝前述充塡步驟移 送。 第3態樣之離子交換裝置的製作方法及設備,是在第1 或第2態樣中,將進行精製處理之精製設備複數個並列設 置,在一個精製設備僅處理同一種類的離子交換樹脂,關 於不同種類之離子交換樹脂’是在不同的精製設備進行處 理。 第4態樣之離子交換裝置的製作方法及設備,是在第3 態樣中’將複數種類的離子交換樹脂分別在不同的精製設 備進行精製後,藉由不同的計量槽進行計量之後,在混合 槽混合而充塡於前述容器。 -12- 201127491 第5態樣之離子交換裝置的製作方法及設備,是在第1 至4之任一態樣中,前述無塵室之潔淨度爲等級1 0000以下 〇 第6態樣之離子交換裝置的製作方法及設備,是在第1 至5之任一態樣中,對於充塡離子交換樹脂後之離子交換 裝置,在前述無塵室內進行超純水之通水,分析來自離子 交換裝置之流出水以檢查離子交換裝置。 第7態樣之離子交換裝置的製作方法及設備,是在第6 態樣中,前述流出水之分析是在潔淨度等級1 000以下之高 潔淨度無塵室內進行。又本發明之無塵室的潔淨度,是表 示1立方呎(1 ft3 )的容積空間中0.3 a m以上的浮游微粒子 的數目,等級1 〇〇〇〇表示1立方呎中有1 0000個微粒子,等 級1 000表示1立方呎中有1 000個微粒子。 在第1〜7態樣之離子交換裝置的製作方法及設備,由 於將離子交換樹脂充塡於容器之充塡步驟是在無塵室內進 行’可防止在該充塡步驟讓空氣中的塵埃混入離子交換裝 置內。因此’藉由使用該方法及設備所製作出的離子交換 裝置,可製造出水質良好的超純水。本發明是在超純水製 造裝置中’特別適用於作爲子系統(二次純水系統)的離 子父換精製處理裝置(Ion Exchange Polisher,非再生型 離子交換裝置)的製作方法及設備。本發明特別適用於作 爲製造局純度的超純水之超純水製造裝置,例如作爲製造 晶圓、製造半導體等所使用之超純水製造裝置的離子交換 裝置之製作方法及設備。依據具有本發明的方法及設備所 -13- 201127491 製作之離子交換裝置之超純水製造裝置,容易 濃度ippt以下(進一步爲o.ippt以下)之超純水 依據第2態樣的方法及設備,由於在精製 的移送步驟中離子交換樹脂不接觸大氣,因此 些步驟中空氣中的塵埃混入離子交換樹脂。 依據第3態樣的方法及設備,由於不同種 換樹脂是由互相不同的精製設備進行精製處理 止不同種類的離子交換樹脂混入離子交換樹脂c 依據第4態樣的方法及設備,由於計量槽 子交換樹脂的種類而分別設置,即使是混床型 置,仍可混合充塡符合規定之離子交換樹脂。 像第5態樣那樣,無塵室的潔淨度宜爲等 〇 依據第6態樣的方法及設備,是對充塡離 後的離子交換裝置進行通水,檢查流出水的水 出貨,因此可確保離子交換裝置的品質。在澤 於該水質檢查是在潔淨度等級1 000以下之高潔 室內進行,因此檢査精度高。 第8態樣之離子交換樹脂層的形成方法及 離子交換樹脂和水的混合漿體導入容器,將水 分離後從容器排出,藉此在容器內充塡離子交 成離子交換樹脂層的方法及裝置,其特徵在於 離子交換樹脂和水的混合漿體是藉由流體 供應至容器, 製造出金屬 〇 步驟及其後 可防止在這 類的離子交 ,因此可防 和。 也是按照離 離子交換裝 i 1 0000以下 子交換樹脂 質後再進行 ;7態樣,由 淨度的無塵 裝置,是將 藉由過濾器 換樹脂而形 壓驅動式泵 -14- 201127491 當前述栗驅動用的流體壓到達既定壓力的時點’解除 作用於泵之流體壓而停止驅動泵。 第9態樣之離子交換樹脂層的形成方法及裝置’是在 第8態樣中,當泵驅動用的流體壓到達既定壓力的時點解 除作用於泵之流體壓而停止驅動栗後’再度開始驅動泵, 當泵驅動用的流體壓再度到達既定壓力的時點,解除作用 於泵之流體壓而停止驅動泵。 第1 〇態樣之離子交換樹脂層的形成方法及裝置,是在 第8或9態樣中,容器係具備:連接於第1過濾器之原水導 入路、連接於第2過濾器之處理水取出路、以及樹脂導入 路;通過樹脂導入路將離子交換樹脂和水的混合漿體導入 容器,藉由第1及/或第2過濾器將水分離後從原水導入路 及/或處理水取出路排出,藉此在容器內形成離子交換樹 脂層。 第1 1態樣之離子交換樹脂層的形成方法及裝置,是在 第8〜1 〇態樣中,流體壓驅動式泵是空氣壓驅動式泵,且具 備:當泵驅動用的空氣壓到達既定壓力的時點,解除作用 於泵之空氣壓而停止驅動泵之控制機構。 在第8 ~ 1 1態樣’作爲流體壓驅動式泵較佳爲空氣壓驅 動式隔膜泵。 在第8〜1 1態樣,離子交換樹脂較佳爲陽離子交換樹脂 和陰離子交換樹脂的混合樹脂。 【實施方式】 -15- 201127491 以下,參照第1圖來說明第1〜7態樣的實施形態。在本 實施形態,是將陰離子交換樹脂和陽離子交換樹脂分別精 製及計量後,混合充塡於容器。 陰離子交換樹脂,是從撓性容器袋等送到專用的收容 槽111進行貯留。該收容槽1 Π內的陰離子交換樹脂’是透 過泵1 1 2及配管1 1 3送到精製塔(調整塔)1 1 4。在該精製 塔,藉由超純水和調整用藥品來進行離子交換樹脂的精製 。作爲調整用藥品’可使用前述專利文獻1〜3等所記載之 各種藥品。精製處理排水被送往回收系統(圖示省略), 處理後以超純水的形式回收再利用。又後述之陽離子交換 樹脂的精製塔也進行同樣的處理,處理排水也進行同樣的 回收。 精製處理後的陰離子交換樹脂,透過配管115、貯槽 116、泵117、配管118而送往計量槽119。 陽離子交換樹脂,被貯留於專用的收容槽121,經由 泵122、配管123送往精製塔124,經精製處理後,透過配 管125、貯槽126、泵127、配管128送往計量槽129。 該等的計量槽1 19、129和其後方之混合槽130等是設 置於潔淨度10000以下的無塵室141內。在計量槽119、129 內以既定量計量後之陰離子交換樹脂和陽離子交換樹脂, 分別透過專用的配管1 19a、129a而導入混合槽130進行混 合。混合後的離子交換樹脂,透過泵1 3 1、配管1 3 2送往容 器進行充塡。作爲容器133,是使用構造與前述第2圖 相同者’離子交換樹脂是從容器1 3 3的樹脂導入口充塡於 -16- 201127491 容器133內而構成離子交換裝置。 充塡完成後,將樹脂導入口密閉。然後,離子交換裝 置被送往無塵室141內的檢查步驟。在該檢查步驟’是從 設置於容器1 3 3之原水導入口透過配管1 3 5導入超純水’從 處理水取出口取出的處理水,則是透過配管1 3 6送往分析 室1 42內的分析機器1 3 7進行水質分析。檢查排水是透過配 管1 3 8朝向回收系統排出。如果檢查結果合格的話,將容 器133之原水導入口及處理水取出口密閉,透過無塵室出 入口 143朝向無塵室141外送出。不合格的離子交換裝置也 從出入口 143朝向無塵室141外取出。上述分析室142,是 潔淨度1000以下之高潔淨度無塵室。 該第1圖的離子交換裝置之製作方法,由於將離子交 換樹脂充塡於容器133之充塡步驟是在潔淨度1 0000以下的 無麈室141內進行,可防止在該充塡步驟讓空氣中的塵埃 混入離子交換裝置內。因此,藉由使用如此般製作出的離 子交換裝置,可製造水質良好的超純水。 在本實施形態,在精製塔114、124內以不接觸大氣的 狀態將陰離子交換樹脂、陽離子交換樹脂施以精製處理之 後,將離子交換樹脂以不接觸大氣的狀態藉由配管1 1 5、 118、125、128進行移送,在計量槽119、129及混合槽130 以不接觸大氣的狀態進行計量和混合,因此可防止在該等 的移送、計量及混合步驟空氣中的塵埃混入離子交換樹脂 〇 此外’在本實施形態’陰離子交換樹脂及陽離子交換 -17- 201127491 樹脂分別使用專用的收容槽111、121、精製塔114、124、 貯槽1 16、126、計量槽1 19、129及各配管以及泵進行移送 、精製及計量,因此可防止在該等步驟讓不同種的離子交 換樹脂混入離子交換樹脂。此外,由於是將未混入不同種 離子交換樹脂之純粹僅由單一種類構成的陰離子交換樹脂 及陽離子交換樹脂進行計量及混合而充塡於容器133,因 此可製作符合規定之混合充塡有陰離子交換樹脂及陽離子 交換樹脂之混床型離子交換裝置。 在本實施形態,是對充塡離子交換樹脂後的離子交換 裝置進行超純水之通水,檢查流出水的水質後再進行出貨 ,因此可確實地讓高品質的離子交換裝置出貨。由於該水 質檢查是在潔淨度等級1〇〇〇以下之高潔淨度的無塵室142 內進行,因此檢查精度高。 在上述實施形態,是將陰離子交換樹脂和陽離子交換 樹脂分別藉由專用的收容槽1 1 1 ~計量槽1 1 9以及收容槽 121〜計量槽129進行處理、移送,又在陰離子交換樹脂是 使用不同型號的樹脂時,是對各型號設置專用的收容槽〜 計量槽的管線,藉由各型號專用的管線來處理陰離子交換 樹脂。關於陽離子交換樹脂也是,在使用不同型號的樹脂 時,是對各型號設置專用的管線,對每個型號藉由專用的 管線進行處理。如此,可防止不同型號的陰離子交換樹脂 混入陰離子交換樹脂中,或不同型號的陽離子交換樹脂混 入陽離子交換樹脂中。 在上述實施形態,是將陰離子交換樹脂和陽離子交換 -18- 201127491 樹脂藉由計量槽1 1 9、1 2 9計量後,在混合槽1 3 0混合而充 塡於容器〗3 3 ’但僅將來自計量槽1 1 9之陰離子交換樹脂或 來自計量槽129之陽離子交換樹脂充塡於容器133而製作陰 離子交換裝置或陽離子交換裝置亦可。 在本發明較佳爲,在容器附設條碼以管理進展及來歷 〇 以下說明第1 ~ 7態樣的實施例及比較例。 〔實施例1〕 使用第1圖所示的離子交換裝置製作設備,在第2圖所 示的容器(72L )將陰離子交換樹脂和陽離子交換樹脂以1 :1混合而製作出離子交換裝置。對該離子交換裝置,將 表1所示金屬離子濃度的超純水以SV = 60/h的狀態進行24小 時的通水。第24小時所採取之離子交換裝置流出水的水質 顯示於表1。 〔比較例1〕 在第1圖,除了使用未設置無塵室141之離子交換裝置 製作設備以外,是與實施例1同樣地製作出離子交換裝置 ’進行通水試驗。第24小時所採取之離子交換裝置流出水 的水質顯示於表1。 -19- 201127491 〔表1〕 (單位ppt)201127491 VI. Description of the Invention: [Technical Field of the Invention] This invention relates to a method and apparatus for producing an ion exchange device by charging an ion exchange resin in a container, and more particularly to an ion suitable for use in an ultrapure water manufacturing process. Method and apparatus for manufacturing an ion exchange device for manufacturing a switching device. The present invention relates to an ion exchange device fabricated by the method and apparatus. Further, the present invention relates to a method and apparatus for forming an ion exchange resin layer by charging an ion exchange resin in a container. The present invention relates to an ion exchange apparatus having an ion exchange resin layer formed by the method and apparatus. [Prior Art] Conventionally, as the ion exchange device, the following structure (especially a fixed ion exchange device) has been adopted. In the structure of the ion exchange apparatus, a cation exchange resin, an anion exchange resin, a mixed resin thereof, or the like, or a mixed resin of the other resin and the like are filled in a container to form an ion exchange resin layer to allow the liquid to be treated to pass therethrough. Perform ion exchange treatment. After the ion exchange resin layer is saturated, the passage of the treatment liquid is stopped, the regeneration liquid is passed, and the ion exchange resin layer is regenerated. Then, the cleaning liquid is passed through and washed, and then the treatment liquid is again passed and the treatment liquid is again passed. The ion exchange treatment is started. However, when the ion exchange resin layer is regenerated by the ion exchange resin layer which is subjected to ion exchange treatment and regeneration, the latter is incapable of performing ion exchange treatment. Therefore, in place of the ion exchange device-5-201127491, there is a unit exchange type ion exchange device, in which the main container is filled with an ion exchange resin disassembly and charging unit, which is transported to the site and then installed in ion exchange. In the treatment, when the ion exchange resin layer is saturated, the ion exchange resin charging unit is removed, and the ion exchange treatment is replaced, and on the other hand, the removed ions are recovered, and the used ion exchange resin is used. The ion exchange device of the unit exchange type is a non-regeneration type ion exchange device which is not discarded by the ion exchange resin charging unit, and the regenerative ion exchange device for reusing the ion is included: for each recovery In the unit, the ion exchange is carried out: the ion exchange resin is collected from the unit, and the regeneration exchange resin is charged to the unit and transported to the on-site standby device for ion exchange treatment. Patent Document 1 (Japanese Patent Laid-Open No. 9-70546) The exchange unit is connected to the raw water pipe by a tube in which the ion exchange of the main body is filled with the ion, and the ion exchange unit u described in the document is processed. 'It is filled in the container 1 having the opening la The grease 2 is provided with a lid 6 in the opening portion ia. The lid 6 is provided with a guide inlet 3, and the raw water introduction path 4 and the treated water take shape. The raw water introduction path 4 is inserted into the bottom of the container I. After the ion exchange resin sub-exchange device of the portable type is carried out, it is necessary to continue the regeneration of the exchange resin charging unit from the new unit of ion exchange, and to include: In the latter case, the resin is regenerated and the resin is directly exchanged for regeneration. In the latter case, the resin is regenerated, and the regenerated resin is attached to the ion exchange product. To use. The ion exchange unit of the first ion exchange unit U has an outlet 5 for ion exchange resin disposed therethrough, and a furnace -6-201127491 is provided at the lower end thereof. The filter 5a installed at the lower end of the treated water take-out path 5 is located at the upper portion inside the container 1. The ion exchange resin 2 is filled in the container 1 through the resin introduction port 3. The inlet 3 is then sealed. The resin introduction port 3 is used for draining, discharging air, and the like at the time of connection, and is usually sealed during ion exchange treatment. The ion exchange unit is sealed by being cut away from the position of the connectors 4b and 5b and transported to the site for mounting. Further, the connectors 4b and 5b are connected to the expansion joints 7, 8 to carry out the introduction of the raw water and the removal of the treated water (ultra-pure water) (see paragraphs 0 0 2 1 to 0 0 2 2 ). The ion exchange resin may be a case where the cation exchange resin or the anion exchange resin is separately charged, and the two are mixed and charged at a ratio of a capacity ratio of 1:3 to 3:1. (Paragraph 0 0 1 8) The ion exchange unit U attached to the ion exchange system introduces raw water from the raw water flow path (not shown) of the ion exchange device into the container 1 through the raw water introduction path 4 and the first filter 4a. The ion exchange is performed by the ion exchange resin layer 2, and the treated water is taken out from the treated water take-out path 5 through the treated water flow path (not shown) of the ion exchange apparatus after the second filter 5a is collected. After the ion exchange resin 2 is saturated, the ion exchange unit U is detached by the connectors 4b, 5b and replaced with a new unit to continue the ion exchange treatment. The used ion exchange unit U is transported in a state of being removed and recovered. The ion exchange resin is taken out and regenerated as necessary, and the regenerated ion exchange resin is refilled in the container 1 to form an ion exchange device. - 201127491 Re-exchanged for ion exchange. In order to charge the ion exchange resin in the main body container 1 of the ion exchange unit U, the ion exchange resin is dispersed in water and introduced as a slurry, and the water of the crucible is separated by the filters 4a and 5a and discharged. According to this method, it is difficult to charge a certain amount of ion exchange resin in the main body container 1. In the example disclosed in Patent Document 4 (JP-A-2002-28501), the ion exchange resin is transported to the ion exchange resin, and then transported to the site, and is filled in the ion exchange device for ion exchange at the site. Then, the ion exchange resin is taken out from the ion exchange device and stored in the ion exchange resin moving container, and then transported to the installation place of the regeneration device, and the regenerated ion exchange resin is again stored in the ion exchange resin moving container and transported to the site. The ion exchange resin moving container is provided with a pipe connected to a filter member (corresponding to a filter) in the container. The ion exchange resin is dispersed in water and introduced in a slurry form, and the water is separated by a filter member. While discharging, thereby charging the ion exchange resin, it was not revealed that the ion exchange resin was charged in a certain amount. The ion exchange resin is easy to measure a certain amount of resin in a dry state. However, in the case of ion exchange, since the ion exchange resin is used in the liquid phase, and the characteristics are expressed on the basis of the volume of the ion exchange resin layer, the amount of the resin which is filled in the container is required to exist. The state in the liquid phase becomes a certain capacity. In this case, the ion exchange resin is introduced into the container in the form of a slurry dispersed in water. However, since the concentration of the ion exchange resin in the slurry cannot be made constant, even if the slurry is measured, the amount cannot be filled. Resin. -8 - 201127491 For the method of filling a certain amount of resin, the method of pre-measuring the resin to be filled and then filling it must measure a certain amount of the regenerated resin beforehand and then disperse it into water. It is introduced in a body shape, so it is necessary to use a combination of complicated steps to become troublesome, and actually it is difficult. Further, the method of measuring the weight of the resin for each container is difficult to perform accurate measurement because the amount of water present affects the measurement of the weight. In addition, the method of measuring the amount of resin charge by visual inspection must be repeated to stop the liquid passing and the visual measurement, and if the container is enlarged to increase the amount of resin charge, it is difficult to perform accurate measurement, and there is a problem. keeping it. In general, if the contents are filled in a container of a certain volume until they are full, the capacity of the charge will be constant. In Patent Documents 1 and 4, the ion exchange resin layer filled in the container is not filled, and a space in which the ion exchange resin layer is not formed remains in the upper portion of the container. In such a container having a margin, it is difficult to charge a certain amount of the ion exchange resin, but the capacity and the volume of the container and the filter, the piping, and the like disposed therein are fixed. If the ion exchange resin is filled to a full volume in such a container of a certain volume, the capacity of the ion exchange resin layer should be constant. If the ion exchange resin is introduced into the slurry in a general container, useless water is also introduced. Since it is difficult to make the concentration of the ion exchange resin in the slurry constant, it is difficult to make the capacity of the ion exchange resin charged. In contrast, as shown in Patent Documents 1 and 2, a pipe connected to a filter in a container is provided, and an ion exchange resin is introduced into a slurry dispersed in water, and the water is separated and discharged by a furnace. The method of charging the ion exchange-9 - 201127491 resin, if filled, the capacity of the ion exchange resin to be charged should be constant. However, when the ion exchange resin slurry is transported by a pump, if it is still transported by a pump after being filled, the density of the resin becomes too high, and it becomes impossible to pass water, or the resin is broken, or filtered. The tubes and piping are easily blocked, and there are many problems. In this case, although it is considered that the ion exchange resin in the container is filled to stop the supply of the slurry according to the pressure rise of the supply slurry, in order to correctly detect the pressure rise to stop the supply of the slurry, it is necessary to employ complicated It is difficult to separate the ion exchange resin in the slurry from the entrained water to form a filling layer having a uniform density, and thus there are many problems. It is described in Patent Document 5 (JP-A-2002-22 1 1 60) that an air pressure-driven diaphragm pump is used as the fluid pressure-driven pump. The air pressure driven diaphragm pump is a double diaphragm type pump in which two diaphragm chambers are respectively provided with a front end of a diaphragm which is engaged with a main shaft (which is slidable through the intermediate wall) so as to be reciprocally movable. However, it has not been revealed that the ion exchange resin is charged in a certain amount. Patent Document 6 (JP-A-2007-305019) discloses a control mechanism 'in an air pressure-driven pump or the like, when the air pressure for driving the pump reaches a predetermined pressure, the air pressure acting on the pump is released to stop driving the pump. . However, the control mechanism ' idling due to damage of the diaphragm or the like causes the driving air pressure to rise, and detects the rise of the air pressure to stop driving the pump, which does not reveal that the ion exchange resin is charged. The amount of sputum becomes a certain amount. -10-201127491 Patent Documents 2 and 3 below describe a method for purifying an ion exchange resin and a reagent for purification. [Patent Document 1] Japanese Patent Laid-Open No. Hei 9-70546 Patent Document 2: Japanese Laid-Open Patent Publication No. Hei No. Hei No. Hei. Patent Document No. 1: Japanese Patent Laid-Open No. 2-221-2116 Patent Document 6: Japanese Patent Publication No. 2〇〇7_3〇5〇19 In the semiconductor industry, ultra-pure water is used for cleaning and other uses of semiconductor products. The water quality requirements for the ultrapure water are becoming more and more strict. For example, the metal concentration is below lppt, and depending on the situation, there is a case where ultra-high water quality below O.lppt is required. In this case, in order to prevent leakage of metal or the like from the ion exchange device, it is necessary to charge the ion exchange resin highly purified in the ion exchange device. However, in the past, highly purified ion exchange resin is filled in the atmosphere in the container. Therefore, dust in the air may be mixed in, which may cause a slight contamination of the ion exchange resin. SUMMARY OF THE INVENTION A first object of the present invention is to provide a method and a device for manufacturing an ion exchange device capable of preventing dust from contaminating an ion exchange resin in air, -11 - 201127491, and ion exchange using the method and the device Device. A second object of the present invention is to provide an ion exchange resin layer which can accurately fill a certain amount of ion exchange resin in a container in a short time by a simple mechanism and operation, and can prevent high density charging of the ion exchange resin. A method and apparatus for forming an ion exchange layer which is chopped and clogged or packed, and an ion exchange apparatus having an ion exchange resin layer formed using the method and apparatus. The method and apparatus for producing an ion exchange device according to a first aspect are a method for producing an ion exchange device by charging a purified ion exchange resin in a container, wherein the ion exchange resin is charged to the container. The 塡 step is carried out in a clean room. In the first aspect, the ion exchange resin is purified by a state in which the ion exchange resin is not exposed to the atmosphere, and is then charged to the atmosphere without being in contact with the atmosphere via a pipe. Step transfer. In the first or second aspect, in the first or second aspect, the purification apparatus for performing the purification treatment is provided in parallel, and only one ion exchange resin of the same type is processed in one purification apparatus. About different types of ion exchange resins' are processed in different refining equipment. The method and apparatus for producing the ion exchange apparatus according to the fourth aspect are described in the third aspect, in which a plurality of kinds of ion exchange resins are separately purified by different refining apparatuses, and then measured by different metering tanks. The mixing tank is mixed and filled in the aforementioned container. -12- 201127491 The method and apparatus for producing the ion exchange device according to the fifth aspect, in any one of the first to fourth aspects, the cleanliness of the clean room is a level of 1 0000 or less, and the sixth aspect of the ion In any one of the first to fifth aspects, in the method of manufacturing the exchange device, the ion exchange device after the ion exchange resin is charged, and the ultrapure water is passed through the clean room to analyze the ion exchange. The device drains water to inspect the ion exchange device. In the sixth aspect of the invention, in the sixth aspect, the analysis of the effluent water is performed in a clean room having a cleanliness level of 1 000 or less. Further, the cleanliness of the clean room of the present invention is the number of floating fine particles of 0.3 am or more in a volume of 1 cubic inch (1 ft3), and the level 1 〇〇〇〇 indicates that there are 1 000 fine particles in 1 cubic inch. A rating of 1 000 means that there are 1 000 particles in 1 cubic inch. In the method and apparatus for producing an ion exchange device according to the first to seventh aspects, the step of charging the ion exchange resin in the container is performed in the clean room to prevent dust from entering the air in the charging step. Inside the ion exchange unit. Therefore, ultra-pure water with good water quality can be produced by using the ion exchange device produced by the method and equipment. The present invention is a method and apparatus for producing an ion exchange polishing apparatus (Ion Exchange Polisher) which is particularly useful as a subsystem (secondary pure water system) in an ultrapure water production apparatus. The present invention is particularly suitable for use as an ultrapure water producing apparatus for producing ultrapure water of a purity of a standpoint, for example, as a method and apparatus for producing an ion exchange apparatus for manufacturing an ultrapure water manufacturing apparatus for use in manufacturing a wafer or the like. Method and apparatus for ultrapure water having an easy concentration of ippt or less (further below o.ippt) according to the second aspect, according to the ultrapure water manufacturing apparatus of the ion exchange apparatus manufactured by the method and apparatus of the present invention-13-201127491 Since the ion exchange resin does not come into contact with the atmosphere in the refining transfer step, dust in the air is mixed into the ion exchange resin in some steps. According to the method and apparatus of the third aspect, the different types of resin are refined by mutually different refining equipment, and the different types of ion exchange resins are mixed into the ion exchange resin. According to the fourth aspect, the method and equipment are used. The type of the exchange resin is separately provided, and even if it is a mixed bed type, it is possible to mix and fill the ion exchange resin which meets the requirements. As in the fifth aspect, the cleanliness of the clean room should be equal to that of the sixth aspect of the method and equipment, and the water is discharged from the ion exchange device after the charge and the water flowing out is checked. The quality of the ion exchange unit can be ensured. The water quality inspection is carried out in a clean room with a cleanliness level of 1 000 or less, so the inspection accuracy is high. a method for forming an ion exchange resin layer of the eighth aspect and a method for introducing a mixed slurry of an ion exchange resin and water into a container, separating the water and discharging the container from the container, thereby filling the container with ion exchanged ion exchange resin layer A device characterized in that a mixed slurry of an ion exchange resin and water is supplied to a container by a fluid to produce a metal ruthenium step and thereafter to prevent ion exchange in such a manner, thereby preventing it. It is also carried out according to the ion exchange device i 1 0000 or less sub-exchange resin; 7 state, the cleanness device by clarity, is a pressure-driven pump that will be replaced by a filter for the resin-14-201127491 When the fluid pressure for pumping reaches a predetermined pressure, the hydraulic pressure applied to the pump is released to stop driving the pump. In the eighth aspect, in the eighth aspect, when the fluid pressure for driving the pump reaches a predetermined pressure, the fluid pressure applied to the pump is released and the driving of the pump is stopped, and the process begins again. The pump is driven to stop the driving of the pump when the fluid pressure for driving the pump reaches the predetermined pressure again, releasing the fluid pressure acting on the pump. In a method and apparatus for forming an ion exchange resin layer according to a first aspect, in the eighth or ninth aspect, the container includes: a raw water introduction path connected to the first filter; and a treated water connected to the second filter. The path and the resin introduction path are taken out; the mixed slurry of the ion exchange resin and water is introduced into the container through the resin introduction path, and the water is separated by the first and/or second filter, and then taken out from the raw water introduction path and/or the treated water. The road is discharged, thereby forming an ion exchange resin layer in the container. The method and apparatus for forming an ion exchange resin layer according to the first aspect are the eighth to the first aspect, wherein the fluid pressure driven pump is an air pressure driven pump and has an air pressure for driving the pump to arrive. At the time of the predetermined pressure, the control mechanism that drives the pump is stopped by releasing the air pressure acting on the pump. In the eighth to eleventh aspect, the fluid pressure driven pump is preferably an air pressure driven diaphragm pump. In the eighth to eleventh aspect, the ion exchange resin is preferably a mixed resin of a cation exchange resin and an anion exchange resin. [Embodiment] -15 - 201127491 Hereinafter, embodiments of the first to seventh aspects will be described with reference to Fig. 1 . In the present embodiment, the anion exchange resin and the cation exchange resin are separately prepared and metered, and then mixed and filled in a container. The anion exchange resin is sent to a dedicated storage tank 111 from a flexible container bag or the like for storage. The anion exchange resin ' in the storage tank 1 is sent to the refining tower (adjusting tower) 1 1 4 through the pump 1 1 2 and the piping 1 1 3 . In the refining column, the ion exchange resin is purified by ultrapure water and an adjusting drug. As the medicine for adjustment, various medicines described in the above-mentioned Patent Documents 1 to 3 and the like can be used. The purified wastewater is sent to a recovery system (not shown), and is recycled as ultrapure water after treatment. Further, the same treatment was carried out in the purification column of the cation exchange resin to be described later, and the same treatment was carried out for the treatment of the drainage. The anion exchange resin after the purification treatment is sent to the metering tank 119 through the pipe 115, the storage tank 116, the pump 117, and the pipe 118. The cation exchange resin is stored in a dedicated storage tank 121, sent to the purification tower 124 via the pump 122 and the piping 123, and after being purified, is sent to the metering tank 129 through the piping 125, the storage tank 126, the pump 127, and the piping 128. The metering tanks 1 19 and 129 and the mixing tank 130 and the like behind the gauge tanks are disposed in the clean room 141 having a cleanliness of 10,000 or less. The anion exchange resin and the cation exchange resin which have been metered in the measurement tanks 119 and 129 are introduced into the mixing tank 130 through the dedicated pipes 1 19a and 129a, respectively, and mixed. The mixed ion exchange resin is sent to the container through the pump 133 and the pipe 1 3 2 for charging. The container 133 has the same structure as that of the second embodiment. The ion exchange resin is filled in the container 133 from the resin inlet of the container 133 to constitute an ion exchange device. After the filling is completed, the resin introduction port is sealed. Then, the ion exchange device is sent to the inspection step in the clean room 141. In the inspection step, the treated water taken out from the treated water take-out port is introduced from the raw water inlet of the container 133 through the pipe 135, and is sent to the analysis chamber 1 through the pipe 136. The internal analysis machine 1 3 7 performs water quality analysis. The drainage is checked through the piping 138 towards the recovery system. When the inspection result is acceptable, the raw water inlet port and the process water outlet port of the container 133 are sealed, and are sent out to the outside of the clean room 141 through the clean room inlet/outlet 143. The defective ion exchange device is also taken out from the inlet and outlet 143 toward the outside of the clean room 141. The analysis chamber 142 is a clean room having a cleanliness of 1000 or less. In the method for producing the ion exchange apparatus of Fig. 1, the charging step of charging the ion exchange resin to the container 133 is performed in the clean room 141 having a cleanliness of 1,000,000 or less, thereby preventing the air from being supplied in the charging step. The dust in the mixture is mixed into the ion exchange device. Therefore, by using the ion exchange device thus produced, ultrapure water having good water quality can be produced. In the present embodiment, after the anion exchange resin and the cation exchange resin are subjected to a purification treatment in a state where the atmosphere is not in contact with the atmosphere in the purification towers 114 and 124, the ion exchange resin is placed in the state of not contacting the atmosphere by the pipes 1 1 5 and 118. The 125 and 128 are transferred, and the metering tanks 119 and 129 and the mixing tank 130 are metered and mixed without being in contact with the atmosphere. Therefore, it is possible to prevent dust in the air in the transfer, metering, and mixing steps from being mixed into the ion exchange resin. Further, in the present embodiment, the anion exchange resin and the cation exchange-17-201127491 resin use dedicated storage tanks 111 and 121, refining towers 114 and 124, storage tanks 1 16 and 126, metering tanks 1 19 and 129, and pipes, respectively. The pump is transferred, refined, and metered, thereby preventing different types of ion exchange resins from being mixed into the ion exchange resin in these steps. In addition, since the anion exchange resin and the cation exchange resin which are purely composed of only a single type, which are not mixed with different kinds of ion exchange resins, are metered and mixed, and are filled in the container 133, it is possible to produce a mixed mixture having an anion exchange. Mixed bed type ion exchange device for resin and cation exchange resin. In the present embodiment, the ion exchange device after charging the ion exchange resin is passed through the ultrapure water, and the water quality of the effluent water is inspected and then shipped. Therefore, the high quality ion exchange device can be reliably shipped. Since the water quality inspection is performed in the clean room 142 having a high cleanliness level of 1 洁净 or less, the inspection accuracy is high. In the above embodiment, the anion exchange resin and the cation exchange resin are treated and transferred by the dedicated storage tank 1 1 1 to the metering tank 1 1 9 and the storage tank 121 to the metering tank 129, respectively, and are used in the anion exchange resin. For different types of resins, a dedicated storage tank to a metering tank is provided for each model, and the anion exchange resin is treated by a dedicated line for each model. Regarding the cation exchange resin, when different types of resins are used, dedicated lines are provided for each model, and each model is processed by a dedicated line. Thus, different types of anion exchange resins can be prevented from being mixed into the anion exchange resin, or different types of cation exchange resins can be mixed into the cation exchange resin. In the above embodiment, the anion exchange resin and the cation exchange -18-201127491 resin are metered by the metering tanks 1 1 9 and 1 29, and then mixed in the mixing tank 130 and filled in the container 〖3 3 ' but only An anion exchange device or a cation exchange device may be prepared by charging the anion exchange resin from the metering tank 111 or the cation exchange resin from the metering tank 129 to the vessel 133. In the present invention, it is preferable to attach a barcode to the container to manage the progress and the following. Examples and comparative examples of the first to seventh aspects will be described below. [Example 1] Using an ion exchange apparatus production apparatus shown in Fig. 1, an anion exchange resin and a cation exchange resin were mixed at a ratio of 1:1 in a vessel (72L) shown in Fig. 2 to prepare an ion exchange apparatus. In the ion exchange apparatus, ultrapure water having a metal ion concentration shown in Table 1 was passed through the water for 24 hours in a state of SV = 60 / h. The water quality of the effluent from the ion exchange unit taken at the 24th hour is shown in Table 1. [Comparative Example 1] In the first embodiment, an ion exchange device was produced in the same manner as in Example 1 except that an apparatus for producing an ion exchange device in which the clean room 141 was not provided was used. The water quality of the effluent from the ion exchange unit taken at the 24th hour is shown in Table 1. -19- 201127491 [Table 1] (unit ppt)

No. Cu Zn Fe Ca Na 原水(超純水) 0.01 0.01 0.01 0.02 0.01 實施例1 0.01 0.01 0.01 0.01 0.01 比較例1 0.45 0.3 0.01 0.2 0.01 從表1可知,藉由使用本發明方法及設備所製作之離 子交換裝置,可製造出高水質的超純水。 接著說明第8〜1 1態樣。 第8〜1 1態樣的離子交換樹脂層,是形成於純水製造裝 置、超純水製造裝置、廢水處理裝置、離子吸附裝置等的 離子交換裝置之離子交換樹脂層,是設置於固定式的離子 交換裝置、單元交換式的離子交換裝置、使用離子交換樹 脂移動容器之樹脂交換式的離子交換裝置等之離子交換樹 脂層。又其對象也包括:形成於上述單元交換式的離子交 換裝置所使用之離子交換樹脂充塡單元、樹脂交換式的離 子交換裝置所使用之離子交換樹脂移動容器、或是樹脂貯 槽等的容器之離子交換樹脂層。在其等當中,作爲其對象 較佳爲形成於單元交換式的離子交換裝置所使用之離子交 換樹脂充塡單元之離子交換樹脂層。 構成離子交換樹脂層之離子交換樹脂可列舉:陽離子 交換樹脂、陰離子交換樹脂、螫合樹脂、其他的選擇吸附 性樹脂、其等的混合樹脂,或是其等與非活性樹脂、其他 樹脂之混合樹脂等,都是呈粒狀的樹脂。該等樹脂不管是 全新樹脂或再使用樹脂皆可,但不論是哪個情況,較佳爲 -20- 201127491 將再生過的樹脂導入充塡於容器內而形成離子交換樹脂層 〇 充塡離子交換樹脂之容器並沒有特別的限定,可直接 充塡於要求形成離子交換樹脂層之容器。作爲這種容器可 列舉:固定式、樹脂交換式 '其他離子交換裝置的離子交 換塔、單元交換式的離子交換裝置所使用之離子交換樹脂 充塡單元'樹脂交換式的離子交換裝置所使用之離子交換 樹脂移動容器、樹脂貯槽、其他容器等。特別適用的是一 定容積的容器亦即能將一定容量的樹脂以一定的充塡密度 充塡’在裝滿時可形成一定容量的離子交換樹脂層。作爲 這種容器可列舉:單元交換式的離子交換裝置所使用之離 子交換樹脂充塡單元。 作爲充塡離子交換樹脂之容器較佳爲,具備樹脂導入 路(用來將離子交換樹脂和水的混合漿體導入容器)、過 濾器(在容器內將挾帶水予以分離)、以及分離水排出路 (將分離水從容器排出)等的充塡手段。較佳爲在具備該 等充塡手段的狀態下內容積爲一定的容器。此外,不具備 該等充塡手段之容器雖亦可,在此情況是藉由安裝該等的 充塡手段而使樹脂的充塡成爲可能。像離子交換塔、離子 交換樹脂充塡單元那樣,作爲離子交換處理用而在容器具 備:連接於第1過濾器之原水導入路、連接於第2過濾器之 處理水取出路、以及樹脂導入路的情況,其等之一方或兩 方可作爲前述充塡手段來使用。作爲過濾器較佳爲,爲了 避免粒徑〇.4~0· 5mm的離子交換樹脂流出而具有ο」〜〇 3 mm -21 - 201127491 的開口。 在第8〜1 1態樣,是將離子交換樹脂和水之混合漿體導 入容器以充塡離子交換樹脂,並將水藉由過濾器分離後從 容器排出,藉此在容器內形成離子交換樹脂層。在此情況 ,將離子交換樹脂和水的混合漿體藉由流體壓驅動式泵供 應至容器,並將分離水排出,若容器內裝滿離子交換樹脂 ’泵的吐出壓變高,伴隨著此使泵驅動用的流體壓也變高 。因此當泵驅動用的流體壓到達既定壓力的時點,將作用 於泵之流體壓解除,藉此停止驅動泵而能在容器內形成一 定容量的離子交換樹脂層。 在第8〜11態樣,離子交換樹脂的容量,是在純水(超 純水)中投入離子交換樹脂,直到樹脂層不產生變化爲止 ,一般而言是靜置10〜20分鐘而使其沉降的狀態下所測定 的容量。作爲離子交換樹脂是使用陽離子交換樹脂和陰離 子交換樹脂等的混合樹脂的情況,離子交換樹脂的容量是 在純水(超純水)中投入混合樹脂而使其靜置沉降的狀態 所測定的容量。離子交換樹脂,由於是將混合漿體以加壓 狀態進行充塡,形成於容器內之離子交換樹脂層的充塡密 度變高,因此構成離子交換樹脂層之樹脂容量,會有比相 當於容器容積之樹脂容量更多的情況。在本發明,是使加 壓狀態所充塡之離子交換樹脂的容量成爲一定。 離子交換樹脂和水的混合漿體,是上述離子交換樹脂 和水的混合漿體,若樹脂的混合比例變高,漿體的流動性 變低而樹脂變得容易堵塞,又若樹脂的混合比例變低則所 -22- 201127491 分離的水量變多而阻礙操作性。因此離子交換樹脂和水的 混合比例較佳爲,在周圍形成水相的狀態(尙未靜置沉降 而使水分離的狀態)下之離子交換樹脂和水的容量比爲( 70 : 30 )〜(90 : 10) 〇 在第8〜1 1態樣,離子交換樹脂和水的混合漿體是藉由 流體壓驅動式泵加壓後導入充塡於容器’這時混合漿體供 應至容器之供應壓(亦即泵的吐出壓)’較佳爲容易進行 樹脂的充塡操作且能避免樹脂破碎而均一充塡的壓力’一 般而言可設定成0.2 ~0.7 MPa範圍內的壓力。作爲這樣的充 塡壓力,若與離子交換裝置中施加於離子交換樹脂層之通 液壓的壓力相同,在單元交換式的離子交換裝置所使用之 離子交換樹脂充塡單元的情況,在離子交換裝置安裝單元 後,不須在通液之前實施離子交換樹脂層的調整就能開始 進行通液,因此較爲理想。 在上述泵吐出壓下將混合漿體供應至容器’當泵驅動 用的流體壓到達既定壓力的時點將作用於泵之流體壓解除 而停止驅動泵,藉此雖可在容器內形成一定容量的離子交 換樹脂層,但會有充塡密度不均一的情況’會有藉由最初 的充塡操作難以形成充塡密度完全均一的離子交換樹脂層 的情況。因此在一次的充塡操作而停止驅動泵之後’再度 開始驅動泵而供應漿體,當泵驅動用的流體壓再度到達既 定壓力的時點,解除作用於泵之流體壓而停止驅動泵,藉 此能夠形成均一充塡密度的離子交換樹脂層。在此情況較 佳爲,在最初的充塡操作而停止驅動泵之後’放置一定時 -23- 201127491 間,例如1〜2 0分鐘,更佳爲5〜10分鐘後再度開始驅動栗。 如此般反覆進行泵的停止和驅動只要一次即可,但越多次 其均一性越高,而能均一地充塡既定量的樹脂。 流體壓驅動式泵可具備:當泵驅動用的流體壓到達既 定壓力的時點,將作用於泵之流體壓予以解除之控制機構 。藉此當容器內充塡有既定量的離子交換樹脂而成爲裝滿 的時點,隨著漿體推入壓之上昇而使泵驅動用的流體壓上 昇,因此當泵驅動用的流體壓到達既定壓力的時點,會自 動解除作用於泵之流體壓。如此能在無過多或不足的離子 交換樹脂充塡量下讓泵的驅動停止。 檢測出泵之吐出壓並讓泵停止之控制機構、或是在泵 的吐出壓變高的時點自動停止栗之機構等,在樹脂和水的 混合系統是困難的而必須使用複雜的機構和操作,但在這 種系統,對應於裝滿樹脂所形成之泵吐出壓的上昇,泵驅 動用的流體壓會敏感地上昇,因此只要控制泵驅動用的流 體壓,就能對應於樹脂之裝滿而讓泵停止。在此情況,由 於泵驅動用的流體不含樹脂般的固態物質,其機器的構造 和操作運轉等可單純化。特別是若使用空氣作爲泵驅動用 的流體,機器的構造和運轉操作等會變得更單純化,相對 於系統進行之取入、排出等變容易,而能迅速地進行正確 的控制。 作爲流體壓驅動式泵,較佳爲空氣壓驅動式泵,藉由 採用空氣壓作爲流體壓所具備的優點包括:其產生、處理 及廢棄等容易,又在作用時被壓縮而能減少樹脂受衝擊所 -24- 201127491 發生的破損等。又較佳爲具備·•當泵驅動用的空氣 既定壓力的時點,可解除作用於栗之空氣壓而停止 之控制機構,藉此使控制變容易,不致損傷樹脂且 確的充塡密度充塡,而能形成一定容量的離子交換 。作爲空氣壓驅動式泵,雖亦可爲往復動活塞式泵 較佳爲空氣壓驅動式隔膜泵。藉由採用空氣壓驅動 泵’可減少對樹脂的衝擊,而能進一步減少樹脂的 且控制容易,能以正確的充塡密度進行充塡而形成 量的離子交換樹脂層。 作爲容器,當使用具備原水導入路(連接於参 器)、處理水取出路(連接於第2過濾器)及樹脂 的容器,例如是單元交換式的離子交換裝置所使用 交換樹脂充塡單元的情況,通過樹脂導入路將離子 脂和水的混合漿體導入容器,將水藉由第1及/或負 器予以分離,再從原水導入路及/或處理水取出路 藉此可在容器內形成離子交換樹脂層。如此般形成 換樹脂層的容器,可直接安裝於離子交換裝置,藉 處理液通液而進行離子交換處理,當飽和後將容器 讓樹脂再生後再度充塡,而能反覆地使用。 在第8〜1 1態樣作爲形成對象之離子交換樹脂層 純水製造裝置 '超純水製造裝置、廢水處理裝置、 附裝置等的不同目的之離子交換裝置,當所導入的 受限制的情況,作爲搬運所使用的水較佳爲,使用 要求純度之純水、超純水等來形成離子交換樹脂層 壓到達 驅動栗 能以正 樹脂層 等,但 式隔膜 損傷, 一定容 I 1過濾 導入路 之離子 交換樹 ;2過灑 排出, 離子交 此讓被 回收並 ,按照 離子吸 雜質量 對應於 ,又在 -25- 201127491 無塵室等的塵埃等較少的環境下進行充塡操作。 依據第8〜1 1態樣,將離子交換樹脂和水的混合漿體導 入容器,將水藉由過濾器分離而從容器排出,藉此在容器 內充塡離子交換樹脂而形成離子交換樹脂層的方法,是將 離子交換樹脂和水的混合漿體藉由流體壓驅動式泵供應至 容器,當前述泵驅動用的流體壓到達既定壓力的時點,解 除作用於栗之流體壓而停止驅動泵,藉此形成離子交換樹 脂層,因此利用簡單的機構和簡單的操作,在短時間內可 正確地將一定量的離子交換樹脂充塡於容器而形成離子交 換樹脂層及具有該離子交換樹脂層之離子交換裝置,而能 防止離子交換樹脂之高密度充塡和破碎、或是配管的堵塞 等。 以下,使用第3圖來說明第8〜1 1態樣之實施形態。在 第3圖’容器1是構成單元交換式的離子交換裝置所使用之 離子交換單元U,是與第2圖具有相同的構造。亦即離子交 換單元U,是在拆裝式的容器1的內部形成再生後的離子交 換樹脂層2。在容器1的上部形成開口部la,且安裝有蓋6 (將樹脂導入路3、原水導入路4及處理水取出路5予以一 體化)。在原水導入路4及處理水取出路5的下部,在延伸 至容器1內的前端部分別設有第1過濾器4a及第2過濾器5a 。此外,在原水導入路4及處理水取出路5的上部,分別安 裝著連結器4b、5b,而形成可連接於樹脂充塡裝置的伸縮 接頭7、8。伸縮接頭7、8,是藉由接頭9、10而連接於外 部流路1 1、1 2。 -26- 201127491 在第2圖,離子交換樹脂層2並未充塡於容器1的全體 ,而在容器1的上部形成有水層;在第3圖,離子交換樹脂 層2是以裝滿的狀態充塡於容器1的全體。此外,作爲離子 交換樹脂層2,是充塡陽離子交換樹脂和陰離子交換樹脂 的混合樹脂。其他之離子交換單元U的構造及對容器1充塡 樹脂之基本操作等,是和第2圖所說明的實質相同。 所製造之形成有離子交換樹脂層2之離子交換單元U, 與第2圖所說明的情況同樣的,是以在連結器4b、5b的位 置被切離的狀態施以密封並搬運至現場,安裝於離子交換 裝置後,將連結器4b、5b與相當於外部流路1 1、12之離子 交換裝置的原水流路及處理水流路(都省略圖示)連接而 供進行離子交換。這時的樹脂導入路3,是用來進行空氣 排出等。 在第3圖,爲了在容器1充塡混合樹脂,是設有陽離子 交換樹脂再生槽21、陰離子交換樹脂再生槽22、混合槽23 ,在其等進行離子交換樹脂之分離、再生、混合等之後, 將再生後的樹脂藉由泵30導入充塡於離子交換單元u之容 器1。 接著說明,從回收的離子交換單元U將使用過的離子 交換樹脂予以分離、再生後進行混合充塡的情況,從所回 收的離子交換單元u的容器1將構成離子交換樹脂層2之混 合樹脂從管線L 1導入陽離子交換樹脂再生槽2 1,從管線L2 輸送純水而將樹脂施以逆洗分離,將分離後的陰離子交換 樹脂從管線L 5導入陰離子交換樹脂再生槽2 2。接著從管線 -27- 201127491 L3對陽離子交換樹脂再生槽21進行再生劑(酸)之通液, 從管線L 4排出再生排液而將陽離子交換樹脂再生,將再生 後的陽離子交換樹脂從管線L6移送至混合槽23。又從管線 L7將純水送往陰離子交換樹脂槽22而將樹脂施以逆洗後, 從管線L8進行再生液(鹼)之通液,從管線L9將再生排液 排出而使陰離子交換樹脂再生,將再生後的陰離子交換樹 脂從管線LI 1移送至混合槽23。 在混合槽23,是從管線L1 2供應空氣及純水,並從管 線L 1 3供應純水而與樹脂混合,以形成樹脂與水的混合漿 體。該混合漿體,是從管線L1 4藉由泵30吸入、加壓而從 管線L1 5通過離子交換單元U之樹脂導入路3導入容器1 ,挾 帶水則藉由第1過濾器4a及第2過濾器5a分離後,通過伸縮 接頭7、8、接頭9、1 0而從外部流路1 1、1 2排出,藉此形 成離子交換樹脂層2。 栗30,是使用空氣壓驅動式隔膜泵。作爲該空氣壓驅 動式隔膜泵,例如採用專利文獻5 (日本特開2002-221 1 60 號)等所揭示之雙隔膜式栗。該泵30,是在鄰接於殼體31 而形成之兩個栗室32a、32b分別設置隔膜33a、33b,使其 等接合於主軸35 (貫穿中間壁34且可滑動)的前端而形成 一體化且能往復移動。 在泵室32a、32b之隔膜33a、33b的相反側形成驅動空 氣室363、3615(分別連通於驅動空氣路37&、3713)。在泵 室32a、32b的下部設置止回閥38a、3 8b,分別透過漿體吸 入路41而連通於管線L14。此外,在泵室32a、32b的上部 -28- 201127491 設置止回閥39a、39b,分別透過漿體供應路42而連通於管 線L15。驅動空氣路37a、37b是不與漿體供應路42交叉地 連結於切換閥43。切換閥43是連通於空氣供應路44和空氣 排出路45。 在泵30設置:當泵驅動用的空氣壓到達既定壓力的時 點會解除作用於泵之空氣壓而停止驅動泵之控制裝置5 0。 作爲該控制裝置5 0,例如採用專利文獻6 (日本特開2 0 0 7 -3 05 0 1 9號)所揭示的。該控制裝置50是由控制閥51、三向 閥52及調節閥53所構成。控制閥51,是被閥體54 (藉由調 節器5 5進行調節)區劃成第1流體室5 6和第2流體室5 7。在 第1流體室56設置驅動空氣入口 58及驅動空氣出口 59,來 自空氣壓縮機60而通過具有閥61的管線L16之壓縮空氣, 是從驅動空氣入口 58進入,從驅動空氣出口 59通過管線 L17而供應至切換閥43之空氣供應路44。 此外’在第1流體室56設有控制空氣出口 62,通過管 線L18連通於三向閥52,進一·步通過管線L19而連通於調節 閥53。在第2流體室57設置控制空氣入口 63,通過管線L21 連通於調節閥5 3。調節器5 5,藉由調整閥體5 4的位置,可 調節通過第1流體室5 6之驅動空氣的流量。在調節閥5 3設 置調節器6 4,可調節調節閥5 3之動作壓。在三向閥5 2設置 切換器6 5,可切換三向閥5 2的流路而排出控制空氣,而能 將控制閥51重置(reset)。 在上述構造’來自空氣壓縮機60之壓縮空氣,藉由閥 6 1進行流量調節,通過管線L 1 6而導入控制閥5 1之驅動空 -29- 201127491 氣入口 58,從驅動空氣出口 59通過管線L17供應給栗30的 切換閥43之空氣供應路44。在切換閥43,將驅動空氣路 37a、37b交互切換,以將驅動空氣交互導入驅動空氣室 36a、3 6b,這時從另一方的驅動空氣路37b、37a將驅動空 氣朝向空氣排出路45排出。藉此使隔膜33a、33b透過主軸 35朝同方向移動,從管線L1 4將混合漿體吸入加壓後,從 管線L1 5通過離子交換單元U的樹脂導入路3導入容器1。 第3圖顯示出,泵30將驅動空氣從切換閥43通過驅動 空氣路37b導入驅動空氣室36b,並將驅動空氣室36a的驅 動空氣從驅動空氣路37 a通過空氣排出路45往系統外排出 的狀態。這時驅動空氣室36a的驅動空氣被排出,而使隔 膜3 3a往中間壁34側移動,藉此使混合槽23的混合漿體從 管線L14進入泵30的漿體吸入路41,通過止回閥38 a而被吸 入泵室32a。在此同時隔膜33b會往泵室32b側移動,藉此 將泵室32b內的混合漿體加壓,而從止回閥39b進入漿體供 應路42,從管線L15通過離子交換單元U的樹脂導入路3而 導入容器1。這時由於將止回閥3 9a關閉,漿體供應路42的 混合漿體不致進入泵室32a。 接著切換閥43進行切換,而將驅動空氣從驅動空氣路 37a導入驅動空氣室36a,並將驅動空氣室36b的驅動空氣 通過驅動空氣路37b從切換閥43通過空氣排出路45往系統 外排出。藉此使隔膜33a、33b往第1圖的右方移動,從混 合槽23進入泵30的漿體吸入路41之混點漿體,通過止回閥 38b被吸入泵室32b。在此同時將泵室32a內的混合漿體加 -30- 201127491 壓,從止回閥3 9 a進入漿體供應路4 2,從管線L 1 5導入離子 交換單元U的容器1。如此般藉由切換閥43交互切換驅動空 氣及混合漿體的流路’可繼續進行混合漿體朝向容器1之 導入。 從管線L 1 5導入容器1之混合漿體,其中的離子交換樹 脂充塡於容器1內,挾帶水則藉由第1過濾器4a及第2過濾 器5 a分離,通過伸縮接頭7、8、接頭9、1〇而從外部流路 1 1、1 2排出,藉此形成離子交換樹脂層2。在離子交換樹 脂的充塡初期,容器1內之離子交換樹脂層2少’在水層多 量存在的狀態下’由於挾帶水會被分離排出’可將混合漿 體陸續導入,而藉由切換閥43之切換以反覆進行混合漿體 之供應。 隨著離子交換樹脂之充塡的進展,當在容器1內的全 體裝滿離子交換樹脂層2時,混合漿體變得無法進入容器1 內。如此泵3 0之吐出壓變高’伴隨此施加於隔膜3 3 a、3 3 b 之負荷變大,因此驅動空氣壓變高。在控制閥5 1 ’第1流 體室5 6內的驅動空氣的一部分是作爲控制空氣’從控制空 氣出口 6 2通過管線L 1 8供應給三向閥5 2 ’進一步通過管線 L 1 9供應給調節閥5 3,在驅動空氣壓到達既定壓力的時點 ,調節閥5 3會打開。 藉由打開調節閥5 3 ’控制空氣從調節閥5 3通過管線 L21、控制空氣入口 63進入第2流體室57 ’使閥體54往第1 圖的右方移動,將第〗流體室5 6封閉。藉此停止對泵3 0供 應驅動空氣,解除作用於泵30之驅動空氣壓而停止驅動栗 -31 - 201127491 3 〇。藉此,泵3 0停止對容器1供應混合漿體。在此階段, 由於容器1呈裝滿狀態,在容器1是形成一定容量之離子交 換樹脂層2。 如此般,在泵30的驅動空氣壓到達既定壓力的時點, 解除作用於泵3 0之驅動空氣壓而停止驅動泵3 0,藉此雖可 在容器1內形成一定容量的離子交換樹脂層2,但仍會有充 塡密度不均一的情況,因此在一次的充塡操作而停止驅動 泵30之後,放置一定時間(例如1〜10分鐘)後再度開始驅 動泵30而供應混合漿體,當驅動空氣壓再度到達既定壓力 的時點,解除作用於泵30之空氣壓而停止驅動泵30,藉此 能夠形成均一充塡密度的離子交換樹脂層2。 在再度開始驅動泵30時,藉由設置於三向閥52之切換 器65來切換三向閥52的流路,以將第2流體室57內的控制 空氣排出,藉此使控制閥5 1的閥體54復位而將控制閥5 1重 置。藉由讓泵30停止並放置,可解除容器1內之離子交換 樹脂層2的充塡應力,以形成均一的離子交換樹脂層2,且 將水層分離而在容器1內形成樹脂流入空間,這時將控制 閥5 1重置並再度開始驅動泵3 0,以再度開始對容器1內供 應混合漿體。在驅動空氣壓再度到達既定壓力的時點,將 調節閥5 3打開,解除作用於泵3 0之空氣壓而停止驅動栗3 0 。藉此可形成充塡密度更均一的離子交換樹脂層2。 如此般形成離子交換樹脂層2之後’或對於離子交換 樹脂層2的充塡量未嚴格要求的情況’可省略反覆的充塡 動作,而將容器1更換並對於下個容器1進行離子交換樹脂 -32- 201127491 層2的形成。容器1之更換’是在連結器4b、5b從伸縮接頭 7、8分離,更換成新的容器1。在更換成新的容器1後,藉 由切換器6 5切換三向閥5 2的流路而將控制閥5 1重置,藉此 對控制閥5 1的第1流體室56供應驅動空氣,再度開始藉由 栗3 0對谷器1供應混合獎體’與則述同樣地充塡離子交換 樹脂,而進行離子交換樹脂層2的形成。 調節閥5 3的動作壓,亦即讓調節閥5 3打開時的驅動空 氣壓是設定成〇·2〜〇.7MPa範圍內的壓力,藉由調節器64, 可將該壓力調節成容易進行樹脂的充塡操作且能避免樹脂 破碎而均一充塡的壓力。在此情況,不須測定或調整泵3 0 的吐出壓,只要調節調節閥5 3的動作壓,即可關閉控制閥 51而解除作用於泵30之空氣壓,以停止驅動泵30。 以下說明第8〜1 1態樣之實施例及比較例。 〔實施例2〜6〕 在第3圖所示的裝置,在容器1 (容積70L ),將陽離 子交換樹脂CRM (栗田工業株式會社製,商標)和陰離子 交換樹脂KR (栗田工業株式會社製,商標)以容量比i : 1 ·6混合成混合樹脂,將在周圍形成有水相的狀態(尙未 靜置沉降而讓水分離的狀態)之混合樹脂和水以容量比8 0 :20混合而成的混合漿體,在泵30設定壓爲0.294MPa下進 行充塡,以形成離子交換樹脂層2。當泵30到達0.29 4MP a 而停止後,放置10分鐘,再度在泵30設定壓爲〇.294MPa下 進行驅動,而進行充塡。將五個容器1依序更換而充塡的 -33- 201127491 結果顯示於表2。 [表2 ] ___層容量(L) 過多或不足量(L) 實施例2 70.5 0.5 實施例3 72.0 2.0 實施例4 71.5 1.5 實施例5 _ 71.0 1.0 實施例6 ---70.5 0.5 根據表2的結果’容器1內之離子交換樹脂層2的過多 或不足量的平均値爲+1.1L,相對於基準量(70L)之容量 比爲1 .5 7 % ’都是屬於過多的情況而沒有不足的例子’判 定爲合格。 〔比較例2 ~ 4〕 使用與實施例2〜6相同的容器及混合漿體,在第3圖所 示的容器1之樹脂導入路3設置漏斗,使用燒杯將混合漿體 倒入直到裝滿容器1爲止,在容器1形成離子交換樹脂層2 。將三個容器1依序更換的結果顯示於表3。 〔表3〕 層容量(L) 渦多或不足量(L) 比較例2 65 -5 比較例3 60 -10 比較例4 63 -7 根據表3的結果,在各例子中,容器1內的離子交換樹 -34- 201127491 脂層2的容量都呈現5〜10L範圍內的不足 第8〜1 1態樣可利用於:在純水製違 裝置、廢水處理裝置、離子吸附裝置等 使用之容器,將陽離子交換樹脂、陰離 的混合樹脂或其等與其他樹脂之混合棱 形成離子交換樹脂層之方法。 雖是使用特定的態樣來說明本發明 明之意圖及範圍下可進行各種的變更7! 具有通常知識者所能明白的。 又本申請案,是根據2009年6月3C 案(特願 2009-155660 號)及 2009 年 11 申請案(特願2009-266401號),將其 【圖式簡單說明】 第1圖係說明本發明的一態樣之離 方法及裝置之流程圖。 第2圖係離子交換裝置的截面圖。 第3圖係實施形態的離子交換樹脂 置之流程圖。 【主要元件符號說明】 1、133 :容器 1 a :開口部 ’且偏差很大。 裝置、超純水製造 的離子交換裝置所 子交換樹脂、其等 脂充塡於容器內以 ,但在不脫離本發 是所屬技術領域中 曰申請之日本申請 月24日申請之曰本 整體援用於本發明 子交換裝置的製作 層的形成方法及裝 -35- 201127491 2 :離子交換樹脂 3 :導入口 4 :原水導入路 4 a、5 a :過濾器 4b、5b :連結器 5 :處理水取出路 6 :蓋 7、8 :伸縮接頭 9、10 :接頭 1 1、1 2 :外部流路 2 1 :陽離子交換樹脂再生槽 22 :陰離子交換樹脂再生槽 2 3、1 3 0 :混合槽 30 、 112、 117、 122 、 127 、 131: ^ 31 :殻體 32a、32b :泵室 3 3 a、3 3 b :隔膜 3 4 :中間壁 35 :主軸 36a、36b:驅動空氣室 37a、37b:驅動空氣路 38a 、 38b 、 39a 、 39b :止回閥 41 :漿體吸入路 42 :漿體供應路 -36- 201127491 43 :切換閥 4 4 :空氣供應路 4 5 :空氣排出路 5 0 :控制裝置 5 1 :控制閥 5 2 :三向閥 5 3 :調節閥 5 4 :閥體 5 5、6 4 :調節器 5 6 :第1流體室 5 7 :第2流體室 5 8 :驅動空氣入口 5 9 :驅動空氣出口 6 0 :空氣壓縮機 61 ··閥 62 :控制空氣出口 6 3 :控制空氣入口 65 :切換器 1 1 1、1 2 1 :收容槽 129a、 132 113、 115、 118、 119a、 123、 125、 128、 、135、 136、 138:配管 1 1 4、1 2 4 :精製塔 1 1 6、1 2 6 :貯槽 1 1 9、1 2 9 :計量槽 -37- 201127491 1 3 7 :分析機 141 :無塵室 142 :分析室 143 :無塵室 Ll~9、LI 1〜1 U :離子交換 器 出入口 9、L21 :管線 單元 -38No. Cu Zn Fe Ca Na Raw water (ultra-pure water) 0.01 0.01 0.01 0.02 0.01 Example 1 0.01 0.01 0.01 0.01 0.01 Comparative Example 1 0.45 0.3 0.01 0.2 0.01 It can be seen from Table 1 that it is produced by using the method and apparatus of the present invention. The ion exchange device can produce ultra-pure water with high water quality. Next, the eighth to eleventh aspects will be described. The ion exchange resin layer of the eighth to the first aspect is an ion exchange resin layer formed in an ion exchange device such as a pure water production device, an ultrapure water production device, a wastewater treatment device, or an ion adsorption device, and is provided in a stationary type. An ion exchange resin layer such as an ion exchange device, a unit exchange type ion exchange device, or a resin exchange type ion exchange device using an ion exchange resin moving container. Further, the object includes: an ion exchange resin charging unit used in the unit exchange type ion exchange apparatus, an ion exchange resin moving container used in a resin exchange type ion exchange apparatus, or a container such as a resin storage tank. Ion exchange resin layer. Among them, the ion exchange resin layer of the ion exchange resin charging unit used in the unit exchange type ion exchange apparatus is preferably used as the object. Examples of the ion exchange resin constituting the ion exchange resin layer include a cation exchange resin, an anion exchange resin, a chelating resin, another selective adsorbent resin, a mixed resin thereof, or the like, or a mixture thereof with an inert resin or other resin. Resins and the like are all granular resins. These resins may be either a new resin or a resin, but in any case, it is preferably -20-201127491. The regenerated resin is introduced into a container to form an ion exchange resin layer and an ion exchange resin. The container is not particularly limited and may be directly filled in a container which is required to form an ion exchange resin layer. Examples of such a container include a fixed-type, resin-exchanged ion exchange column of another ion exchange device, and an ion exchange resin charging unit used in a unit exchange type ion exchange device, which is used in a resin exchange type ion exchange device. Ion exchange resin moving container, resin storage tank, other containers, and the like. It is particularly suitable for a container of a certain volume to be capable of charging a resin of a certain capacity at a certain filling density. When filled, a certain volume of ion exchange resin layer can be formed. As such a container, an ion exchange resin charging unit used in a unit exchange type ion exchange apparatus can be cited. The container filled with the ion exchange resin preferably includes a resin introduction path (for introducing a mixed slurry of ion exchange resin and water into the container), a filter (separating the water in the container), and separating the water. A charging means such as a discharge path (discharging the separated water from the container). It is preferable to have a container having a constant internal volume in a state in which such a charging means is provided. Further, a container which does not have such a charging means may be used, and in this case, charging of the resin is possible by attaching such a charging means. In the container, the raw water introduction path connected to the first filter, the treated water extraction path connected to the second filter, and the resin introduction path are provided in the container as the ion exchange treatment and the ion exchange resin charging unit. In the case of one or both of them, it can be used as the above-mentioned means of charging. Preferably, the filter has an opening of ο"~〇 3 mm -21 - 201127491 in order to prevent the ion exchange resin having a particle diameter of 44 to 0.5 mm from flowing out. In the eighth to eleventh aspect, a mixed slurry of an ion exchange resin and water is introduced into a container to fill the ion exchange resin, and the water is separated by a filter and discharged from the container, thereby forming ion exchange in the container. Resin layer. In this case, the mixed slurry of the ion exchange resin and water is supplied to the container by the fluid pressure driven pump, and the separated water is discharged, and if the container is filled with the ion exchange resin, the pump discharge pressure becomes high, accompanied by this. The fluid pressure for driving the pump is also increased. Therefore, when the fluid pressure for driving the pump reaches a predetermined pressure, the fluid pressure acting on the pump is released, whereby the pump is stopped and a certain volume of the ion exchange resin layer can be formed in the container. In the eighth to eleventh aspect, the ion exchange resin has an ion exchange resin in pure water (ultra-pure water) until the resin layer does not change, and is generally allowed to stand for 10 to 20 minutes. The capacity measured in the settled state. In the case where a mixed resin such as a cation exchange resin or an anion exchange resin is used as the ion exchange resin, the capacity of the ion exchange resin is a capacity measured by putting a mixed resin into pure water (ultra-pure water) and allowing it to stand still. . In the ion exchange resin, since the mixed slurry is charged in a pressurized state, the density of the ion exchange resin layer formed in the container becomes high, and therefore the resin capacity constituting the ion exchange resin layer is equivalent to the container. The capacity of the resin in the volume is more. In the present invention, the capacity of the ion exchange resin charged in the pressurized state is made constant. The mixed slurry of the ion exchange resin and water is a mixed slurry of the above ion exchange resin and water. If the mixing ratio of the resin becomes high, the fluidity of the slurry becomes low and the resin becomes clogged easily, and if the resin is mixed. Lower -22-201127491 The amount of water separated increases and hinders operability. Therefore, the mixing ratio of the ion exchange resin and water is preferably such that the capacity ratio of the ion exchange resin to water in the state in which the aqueous phase is formed (the state in which the water is not settled and settled in water) is (70: 30)~ (90: 10) 第 In the eighth to eleventh aspect, the mixed slurry of the ion exchange resin and water is pressurized by the fluid pressure driven pump and then introduced into the container. At this time, the supply of the mixed slurry to the container is supplied. The pressure (i.e., the discharge pressure of the pump) is preferably a pressure which is easy to carry out the charging operation of the resin and which can prevent the resin from being broken and uniformly charged. Generally, the pressure in the range of 0.2 to 0.7 MPa can be set. As such a charging pressure, if the pressure of the hydraulic pressure applied to the ion exchange resin layer in the ion exchange device is the same, in the case of the ion exchange resin charging unit used in the unit exchange type ion exchange device, in the ion exchange device After the unit is mounted, it is preferable to start the liquid passage without adjusting the ion exchange resin layer before the liquid is passed. Supplying the mixed slurry to the container under the pump discharge pressure. When the fluid pressure for driving the pump reaches a predetermined pressure, the fluid pressure acting on the pump is released to stop driving the pump, thereby forming a certain volume in the container. In the case of the ion exchange resin layer, there is a case where the charge density is not uniform. It is difficult to form an ion exchange resin layer having a completely uniform charge density by the first charge operation. Therefore, after stopping the driving of the pump in one charging operation, the pump is again driven to supply the slurry, and when the fluid pressure for driving the pump reaches the predetermined pressure again, the fluid pressure acting on the pump is released and the pump is stopped. An ion exchange resin layer having a uniform charge density can be formed. In this case, it is preferable to start the driving of the pump after the initial charging operation and stop driving the pump. Between -23 and 201127491, for example, 1 to 20 minutes, and more preferably 5 to 10 minutes, the driving of the pump is started again. It is only necessary to repeatedly stop and drive the pump in such a manner, but the more uniform the plurality of times, the more uniform the resin can be charged. The fluid pressure-driven pump may have a control mechanism that releases the fluid pressure acting on the pump when the fluid pressure for driving the pump reaches a predetermined pressure. Therefore, when the container is filled with a predetermined amount of ion exchange resin and becomes full, the fluid pressure for pump driving rises as the slurry push pressure increases, so that the fluid pressure for pump driving reaches a predetermined value. At the point of pressure, the fluid pressure acting on the pump is automatically released. This allows the pump to be stopped without excessive or insufficient ion exchange resin charge. In a control mechanism that detects the discharge pressure of the pump and stops the pump, or a mechanism that automatically stops the pump when the discharge pressure of the pump becomes high, it is difficult to use a complicated mechanism and operation in a mixed system of resin and water. However, in such a system, the fluid pressure for pump driving rises sensitively in response to an increase in the discharge pressure of the pump formed by filling the resin, so that as long as the fluid pressure for driving the pump is controlled, it is possible to fill the resin. Let the pump stop. In this case, since the fluid for pump driving does not contain a resin-like solid substance, the construction and operation of the machine can be simplified. In particular, when air is used as the fluid for pump driving, the structure and operation of the machine become more simplistic, and it is easy to take in and discharge with respect to the system, and it is possible to quickly perform correct control. As the fluid pressure driven pump, preferably an air pressure driven pump, the advantages of using air pressure as the fluid pressure include: easy to generate, handle, and discard, and are compressed at the time of action to reduce resin stress. Impact Institute-24- 201127491 Damage occurred, etc. Further, it is preferable to provide a control mechanism for stopping the air pressure of the pump when the pressure of the pump is set to a predetermined pressure, thereby making the control easy, without damaging the resin and ensuring the density of the charge. , and can form a certain volume of ion exchange. As the air pressure driven pump, a reciprocating piston pump may preferably be an air pressure driven diaphragm pump. By using the air pressure to drive the pump', it is possible to reduce the impact on the resin, and it is possible to further reduce the resin and control the ion exchange resin layer which is easily controlled and charged at a correct charge density. As a container, a container having a raw water introduction path (connected to a parameter), a treated water take-out path (connected to a second filter), and a resin is used, for example, an exchange resin charging unit used in a unit exchange type ion exchange device. In this case, the mixed slurry of ionic fat and water is introduced into the container through the resin introduction path, and the water is separated by the first and/or negative device, and then the raw water introduction path and/or the treated water extraction path can be used in the container. An ion exchange resin layer is formed. The container in which the resin layer is formed in this manner can be directly attached to the ion exchange apparatus, and the ion exchange treatment can be carried out by the liquid passing through the treatment liquid. When the container is saturated, the resin is regenerated and then refilled, and can be used repeatedly. In the eighth to eleventh aspect, the ion exchange device for the purpose of forming an ion exchange resin layer pure water production device, such as an ultrapure water production device, a wastewater treatment device, and an attachment device, is restricted in the introduction. It is preferable that the water used for the transportation is formed by using pure water or ultrapure water of a desired purity to form an ion exchange resin, and the drive can be a positive resin layer or the like, but the diaphragm is damaged, and the volume is introduced into the filter. The ion exchange tree of the road; 2 is sprinkled and discharged, and the ion is exchanged, and the charging operation is performed according to the ion gettering quality, and the charging operation is performed in a dusty environment such as -25-201127491 clean room. According to the eighth to eleventh aspect, the mixed slurry of the ion exchange resin and water is introduced into the container, and the water is separated from the container by the filter, thereby filling the container with the ion exchange resin to form the ion exchange resin layer. The method comprises the steps of: supplying a mixed slurry of ion exchange resin and water to a container by a fluid pressure driven pump, and when the fluid pressure for driving the pump reaches a predetermined pressure, releasing the fluid pressure acting on the pump and stopping the driving of the pump Thereby, an ion exchange resin layer is formed, so that a simple mechanism and a simple operation can accurately charge a certain amount of the ion exchange resin to the container in a short time to form an ion exchange resin layer and have the ion exchange resin layer. The ion exchange device can prevent high-density filling and fragmentation of the ion exchange resin, or blockage of piping. Hereinafter, an embodiment of the eighth to eleventh aspects will be described using FIG. In Fig. 3, the container 1 is an ion exchange unit U used in a unit exchange type ion exchange unit, and has the same structure as that of Fig. 2. That is, the ion exchange unit U is a regenerated ion exchange resin layer 2 formed inside the removable container 1. An opening portion 1a is formed in the upper portion of the container 1, and a lid 6 is attached (the resin introduction path 3, the raw water introduction path 4, and the treated water take-out path 5 are integrated). In the lower portion of the raw water introduction path 4 and the treated water take-out path 5, the first filter 4a and the second filter 5a are provided at the distal end portions extending into the container 1, respectively. Further, the adapters 4b and 5b are attached to the upper portions of the raw water introduction path 4 and the treated water extraction path 5, respectively, and the expansion joints 7 and 8 connectable to the resin charging device are formed. The expansion joints 7, 8 are connected to the outer flow paths 1 1 and 1 2 by the joints 9, 10. -26- 201127491 In Fig. 2, the ion exchange resin layer 2 is not filled in the entirety of the container 1, but a water layer is formed on the upper portion of the container 1. In Fig. 3, the ion exchange resin layer 2 is filled. The state is filled with the entirety of the container 1. Further, as the ion exchange resin layer 2, a mixed resin of a cation exchange resin and an anion exchange resin is charged. The structure of the other ion exchange unit U and the basic operation of charging the container 1 with the resin are substantially the same as those described in Fig. 2. The ion exchange unit U in which the ion exchange resin layer 2 is formed is similarly sealed as in the case of Fig. 2, and is sealed and transported to the site in a state where the positions of the connectors 4b and 5b are separated. After being attached to the ion exchange apparatus, the connectors 4b and 5b are connected to the raw water flow path and the treated water flow path (both not shown) corresponding to the ion exchange devices of the external flow paths 1 1 and 12 for ion exchange. The resin introduction path 3 at this time is used for air discharge or the like. In the third embodiment, in order to charge the resin in the container 1, the cation exchange resin regeneration tank 21, the anion exchange resin regeneration tank 22, and the mixing tank 23 are provided, and after the ion exchange resin is separated, regenerated, mixed, or the like. The regenerated resin is introduced into the vessel 1 filled with the ion exchange unit u by the pump 30. Next, when the used ion exchange resin is separated and regenerated from the recovered ion exchange unit U and then mixed and charged, the mixed resin constituting the ion exchange resin layer 2 is taken from the container 1 of the recovered ion exchange unit u. The cation exchange resin regeneration tank 21 is introduced from the line L1, pure water is supplied from the line L2, the resin is subjected to backwash separation, and the separated anion exchange resin is introduced into the anion exchange resin recovery tank 2 from the line L5. Next, the cation exchange resin regeneration tank 21 is passed through a line -27-201127491 L3 to pass a regenerant (acid), and the regeneration discharge liquid is discharged from the line L4 to regenerate the cation exchange resin, and the regenerated cation exchange resin is discharged from the line L6. Transfer to the mixing tank 23. Further, pure water is sent to the anion exchange resin tank 22 from the line L7, and the resin is backwashed. Then, the reconstituted liquid (alkali) is passed through the line L8, and the regenerated liquid is discharged from the line L9 to regenerate the anion exchange resin. The regenerated anion exchange resin is transferred from the line LI 1 to the mixing tank 23. In the mixing tank 23, air and pure water are supplied from the line L1 2, and pure water is supplied from the line L 1 3 to be mixed with the resin to form a mixed slurry of resin and water. The mixed slurry is introduced into the container 1 through the resin introduction path 3 of the ion exchange unit U from the line L1 5 by the suction and pressurization of the line L1 4 by the pump 30, and the water is supplied by the first filter 4a and the first filter 2 After the filter 5a is separated, it is discharged from the external flow paths 1 1 and 12 by the expansion joints 7 and 8, the joints 9, and 10, whereby the ion exchange resin layer 2 is formed. The chestnut 30 is an air pressure driven diaphragm pump. As the air-pressure-driven diaphragm pump, for example, a double diaphragm type chest disclosed in Patent Document 5 (JP-A-2002-221 1 60) or the like is used. The pump 30 is formed by providing the diaphragms 33a and 33b in the two chest chambers 32a and 32b formed adjacent to the casing 31 so as to be joined to the front end of the main shaft 35 (slidable through the intermediate wall 34). And can move back and forth. Drive air chambers 363, 3615 are formed on the opposite sides of the diaphragms 33a, 33b of the pump chambers 32a, 32b (connected to the drive air passages 37 & 3713, respectively). Check valves 38a and 38b are provided in the lower portion of the pump chambers 32a and 32b, and communicate with the line L14 through the slurry suction path 41, respectively. Further, check valves 39a and 39b are provided in the upper portions -28 to 201127491 of the pump chambers 32a and 32b, and communicate with the pipe line L15 through the slurry supply path 42 respectively. The drive air passages 37a and 37b are connected to the switching valve 43 without crossing the slurry supply passage 42. The switching valve 43 is connected to the air supply path 44 and the air discharge path 45. The pump 30 is provided such that when the air pressure for driving the pump reaches a predetermined pressure, the air pressure acting on the pump is released and the control device 50 for driving the pump is stopped. As the control device 50, for example, Patent Document 6 (Japanese Patent Laid-Open Publication No. Hei. No. Hei. The control device 50 is composed of a control valve 51, a three-way valve 52, and a regulating valve 53. The control valve 51 is partitioned into a first fluid chamber 56 and a second fluid chamber 57 by a valve body 54 (adjusted by a regulator 55). A driving air inlet 58 and a driving air outlet 59 are provided in the first fluid chamber 56, and compressed air from the air compressor 60 through the line L16 having the valve 61 enters from the driving air inlet 58, and the driving air outlet 59 passes through the line L17. The air supply path 44 is supplied to the switching valve 43. Further, the first fluid chamber 56 is provided with a control air outlet 62, communicates with the three-way valve 52 through the pipe line L18, and further communicates with the regulator valve 53 through the line L19. A control air inlet 63 is provided in the second fluid chamber 57, and is connected to the regulating valve 53 through a line L21. The regulator 55 can adjust the flow rate of the driving air passing through the first fluid chamber 56 by adjusting the position of the valve body 54. The regulator 64 is provided in the regulator valve 53 to adjust the operating pressure of the regulator valve 53. By providing the switch 6 5 to the three-way valve 52, the flow path of the three-way valve 52 can be switched to discharge the control air, and the control valve 51 can be reset. In the above configuration, the compressed air from the air compressor 60 is adjusted by the flow of the valve 61, and is introduced into the drive air -29-201127491 gas inlet 58 of the control valve 51 through the line L16, and passes through the drive air outlet 59. The line L17 is supplied to the air supply path 44 of the switching valve 43 of the pump 30. In the switching valve 43, the driving air passages 37a, 37b are alternately switched to alternately introduce the driving air into the driving air chambers 36a, 36b, at which time the driving air is discharged toward the air discharge path 45 from the other driving air passages 37b, 37a. Thereby, the diaphragms 33a and 33b are moved in the same direction through the main shaft 35, and the mixed slurry is sucked and pressurized from the line L1 4, and then introduced into the container 1 through the resin introduction path 3 of the ion exchange unit U from the line L1 5 . Fig. 3 shows that the pump 30 introduces driving air from the switching valve 43 through the driving air passage 37b into the driving air chamber 36b, and discharges the driving air of the driving air chamber 36a from the driving air passage 37a through the air discharge path 45 to the outside of the system. status. At this time, the driving air that drives the air chamber 36a is discharged, and the diaphragm 33a is moved toward the intermediate wall 34 side, whereby the mixed slurry of the mixing tank 23 enters the slurry suction path 41 of the pump 30 from the line L14, and passes through the check valve. 38 a is sucked into the pump chamber 32a. At the same time, the diaphragm 33b moves toward the pump chamber 32b side, thereby pressurizing the mixed slurry in the pump chamber 32b, and enters the slurry supply path 42 from the check valve 39b, and passes through the resin of the ion exchange unit U from the line L15. The channel 3 is introduced and introduced into the container 1. At this time, since the check valve 39a is closed, the mixed slurry of the slurry supply path 42 does not enter the pump chamber 32a. Then, the switching valve 43 is switched, and the driving air is introduced into the driving air chamber 36a from the driving air passage 37a, and the driving air of the driving air chamber 36b is discharged from the switching valve 43 through the air discharge path 45 to the outside of the system through the driving air passage 37b. Thereby, the diaphragms 33a and 33b are moved to the right in the first figure, and the slurry of the slurry suction path 41 entering the pump 30 from the mixing tank 23 is sucked into the pump chamber 32b through the check valve 38b. At the same time, the mixed slurry in the pump chamber 32a is pressurized by -30-201127491, from the check valve 39a into the slurry supply path 4 2, and from the line L 1 5 to the container 1 of the ion exchange unit U. The introduction of the mixed slurry toward the container 1 can be continued by the switching valve 43 alternately switching the flow path for driving the air and mixing the slurry. Introducing the mixed slurry of the container 1 from the line L 1 5, wherein the ion exchange resin is filled in the container 1, and the water is separated by the first filter 4a and the second filter 5a, through the expansion joint 7, 8. The joints 9, 1 are discharged from the external flow paths 1 1 and 1 2, whereby the ion exchange resin layer 2 is formed. At the beginning of the filling of the ion exchange resin, the ion exchange resin layer 2 in the container 1 is less 'in the presence of a large amount of water layer', because the water will be separated and discharged, the mixed slurry can be introduced one after another, and by switching The switching of the valve 43 is repeated to supply the mixed slurry. As the ion exchange resin progresses, the mixed slurry becomes inaccessible to the container 1 when the entire body in the container 1 is filled with the ion exchange resin layer 2. As a result, the discharge pressure of the pump 30 becomes high. As the load applied to the diaphragms 3 3 a and 3 3 b increases, the driving air pressure becomes high. A portion of the drive air in the control valve 5 1 'the first fluid chamber 56 is supplied as control air from the control air outlet 6 2 through the line L 1 8 to the three-way valve 5 2 'further supplied through the line L 1 9 The regulating valve 53 opens the regulating valve 53 when the driving air pressure reaches a predetermined pressure. By opening the regulating valve 5 3 ' to control the air from the regulating valve 53 through the line L21, the control air inlet 63 into the second fluid chamber 57' to move the valve body 54 to the right of the first figure, the first fluid chamber 56 Closed. Thereby, the supply of the driving air to the pump 30 is stopped, and the driving air pressure acting on the pump 30 is released to stop the driving of the pump -31 - 201127491 3 〇. Thereby, the pump 30 stops supplying the mixed slurry to the container 1. At this stage, since the container 1 is in a full state, the container 1 is a ion exchange resin layer 2 which forms a certain capacity. In this manner, when the driving air pressure of the pump 30 reaches a predetermined pressure, the driving air pressure acting on the pump 30 is released, and the driving of the pump 30 is stopped, whereby a certain volume of the ion exchange resin layer 2 can be formed in the container 1. However, there is still a case where the density of the charging is not uniform. Therefore, after stopping the driving of the pump 30 in one charging operation, after a certain period of time (for example, 1 to 10 minutes), the pump 30 is again driven to supply the mixed slurry. When the driving air pressure reaches the predetermined pressure again, the air pressure acting on the pump 30 is released to stop the driving of the pump 30, whereby the ion exchange resin layer 2 having a uniform filling density can be formed. When the pump 30 is started to be driven again, the flow path of the three-way valve 52 is switched by the switch 65 provided in the three-way valve 52 to discharge the control air in the second fluid chamber 57, thereby causing the control valve 5 1 The valve body 54 is reset to reset the control valve 51. By stopping and placing the pump 30, the charging stress of the ion exchange resin layer 2 in the container 1 can be released to form a uniform ion exchange resin layer 2, and the water layer can be separated to form a resin inflow space in the container 1. At this time, the control valve 51 is reset and the pump 30 is started again to start the supply of the mixed slurry in the container 1 again. When the driving air pressure reaches the predetermined pressure again, the regulating valve 53 is opened, the air pressure acting on the pump 30 is released, and the driving of the pump 3 0 is stopped. Thereby, the ion exchange resin layer 2 having a more uniform density can be formed. After the ion exchange resin layer 2 is thus formed, or the case where the charge amount of the ion exchange resin layer 2 is not strictly required, the repeated charging operation can be omitted, and the container 1 is replaced and the ion exchange resin is subjected to the next container 1. -32- 201127491 Formation of layer 2. The replacement of the container 1 is separated from the expansion joints 7, 8 by the connectors 4b, 5b, and replaced with a new one. After replacing the new container 1, the control valve 51 is reset by switching the flow path of the three-way valve 52 by the switch 65, thereby supplying the driving air to the first fluid chamber 56 of the control valve 51. The supply of the ion exchange resin layer 2 is carried out by supplying the mixed prize body to the grain device 1 by the pump 30, and filling the ion exchange resin in the same manner as described above. The operating pressure of the regulating valve 53, that is, the driving air pressure when the regulating valve 53 is opened, is set to a pressure in the range of 〇·2 to 7.7 MPa, and the regulator 64 can adjust the pressure to be easy. The charging operation of the resin can avoid the pressure of the resin being broken and uniformly charged. In this case, it is not necessary to measure or adjust the discharge pressure of the pump 30, and if the operating pressure of the regulator valve 53 is adjusted, the control valve 51 can be closed and the air pressure acting on the pump 30 can be released to stop the drive of the pump 30. Examples and comparative examples of the eighth to eleventh aspects will be described below. [Examples 2 to 6] In the apparatus shown in Fig. 3, a cation exchange resin CRM (trademark of Kurita Industrial Co., Ltd.) and an anion exchange resin KR (Kurita Kogyo Co., Ltd.) were used in the container 1 (volume 70 L). The trademark is mixed with a capacity ratio of i:1·6 to form a mixed resin, and a mixed resin and water in a state in which an aqueous phase is formed (the state in which the water is not allowed to stand and the water is separated) is mixed with a capacity ratio of 80:20. The resulting mixed slurry was charged at a set pressure of 0.294 MPa of the pump 30 to form an ion exchange resin layer 2. When the pump 30 reached 0.29 4MP a and stopped, it was left for 10 minutes, and the pump 30 was again driven at a pressure of 294.294 MPa to perform charging. The five containers 1 were replaced in sequence and filled in. -33- 201127491 The results are shown in Table 2. [Table 2] ___ Layer Capacity (L) Too much or insufficient (L) Example 2 70.5 0.5 Example 3 72.0 2.0 Example 4 71.5 1.5 Example 5 _ 71.0 1.0 Example 6 --70.5 0.5 According to Table 2 As a result, the average enthalpy of the excess or deficiency of the ion exchange resin layer 2 in the container 1 is +1.1 L, and the capacity ratio with respect to the reference amount (70 L) is 1.57%. An insufficient example is judged as qualified. [Comparative Examples 2 to 4] Using the same container and mixed slurry as in Examples 2 to 6, a funnel was provided in the resin introduction path 3 of the container 1 shown in Fig. 3, and the mixed slurry was poured into a beaker until it was full. The ion exchange resin layer 2 is formed in the container 1 up to the container 1. The results of sequentially replacing the three containers 1 are shown in Table 3. [Table 3] Layer capacity (L) Vortex or insufficient amount (L) Comparative Example 2 65 -5 Comparative Example 3 60 -10 Comparative Example 4 63 -7 According to the results of Table 3, in each example, in the container 1 Ion exchange tree-34- 201127491 The capacity of the lipid layer 2 is in the range of 5 to 10 L. The 8th to 11th aspect can be used for: containers used in pure water disposal devices, wastewater treatment devices, ion adsorption devices, etc. A method of forming a ion exchange resin layer by mixing a cation exchange resin, an anion mixed resin, or the like with other resins. Various changes can be made using the specific aspects to illustrate the intent and scope of the present invention. 7 It will be understood by those of ordinary skill. This application is based on the June 3C case of June 2009 (Japanese Patent No. 2009-155660) and the application form of 2009 (Special Wish 2009-266401), which will be described in the following figure. A flow chart of a method and apparatus for an aspect of the invention. Figure 2 is a cross-sectional view of an ion exchange device. Fig. 3 is a flow chart showing the ion exchange resin of the embodiment. [Explanation of main component symbols] 1.133: Container 1 a : Opening portion ' and the deviation is large. The device, the ion exchange device manufactured by the ultrapure water, the exchange resin, and the like are filled in the container, but the present application is applied in the technical application of the Japanese application on the 24th of the application. Method for forming a production layer of the sub-exchange device of the present invention and mounting - 35 - 201127491 2 : ion exchange resin 3 : introduction port 4 : raw water introduction path 4 a, 5 a : filter 4b, 5b : connector 5 : treated water Takeout path 6: cover 7, 8: expansion joints 9, 10: joints 1 1 and 1 2 : external flow path 2 1 : cation exchange resin regeneration tank 22 : anion exchange resin regeneration tank 2 3, 1 3 0 : mixing tank 30 , 112, 117, 122, 127, 131: ^ 31 : Housings 32a, 32b: pump chamber 3 3 a, 3 3 b : diaphragm 3 4 : intermediate wall 35: main shafts 36a, 36b: drive air chambers 37a, 37b: Drive air passages 38a, 38b, 39a, 39b: check valve 41: slurry suction passage 42: slurry supply passage - 36 - 201127491 43 : switching valve 4 4 : air supply passage 4 5 : air discharge passage 5 0 : control Device 5 1 : Control valve 5 2 : Three-way valve 5 3 : Regulating valve 5 4 : Valve body 5 5, 6 4 : Regulator 5 6 : 1 Body chamber 5 7 : 2nd fluid chamber 5 8 : Drive air inlet 5 9 : Drive air outlet 6 0 : Air compressor 61 · Valve 62 : Control air outlet 6 3 : Control air inlet 65 : Switch 1 1 1 1 2 1 : storage tanks 129a, 132 113, 115, 118, 119a, 123, 125, 128, 135, 136, 138: piping 1 1 4, 1 2 4: refining tower 1 1 6 , 1 2 6 : storage tank 1 1 9 , 1 2 9 : Metering tank -37- 201127491 1 3 7 : Analyzer 141 : Clean room 142 : Analysis chamber 143 : Clean room Ll~9, LI 1~1 U : Ion exchanger inlet and outlet 9, L21: Pipeline unit -38

Claims (1)

201127491 七、申請專利範圍: 1. 一種離子交換裝置之製作方法,是將精製處理後的 離子交換樹脂充塡於容器來製作離子交換裝置之方法,其 特徵在於: 將離子交換樹脂充塡於該容器之充塡步驟是在無塵室 內進行。 2·如申請專利範圍第1項記載的離子交換裝置之製作 方法’其中’將離子交換樹脂以不接觸大氣的狀態進行精 製處理後’經由配管而以不接觸大氣的狀態朝充塡步驟移 送。 3.如申請專利範圍第〖或2項記載的離子交換裝置之製 作方法’其中’將進行精製處理之精製設備複數個並列設 置’在一個精製設備僅處理同一種類的離子交換樹脂,關 於不同種類之離子交換樹脂’是在不同的精製設備進行處 理。 4 .如申請專利範圍第3項記載的離子交換裝置之製作 方法’其中’將複數種類的離子交換樹脂分別在不同的精 製設備進行精製後,藉由不同的計量槽進行計量之後,在 混合槽混合而充塡於前述容器。 5 _如申請專利範圍第1至4項中任一項記載的離子交換 ^置之製作方法’其中’前述無塵室之潔淨度爲等級 1 0 0 0 0以下〇 6 ·如申g靑專利範圍第1至5項中任—項記載的離子交換 袋置之製作方法,其中,對於充塡離子交換樹脂後之離子 -39- 201127491 交換裝置,在前述無塵室內進行超純水之通 離子交換裝置之流出水以檢查離子交換裝置 7 .如申請專利範圍第6項記載的離子交 方法,其中,前述流出水之分析是在潔淨度 之高潔淨度無塵室內進行。 8 · —種離子交換裝置之製作設備,是將 離子交換樹脂充塡於容器來製作離子交換裝 特徵在於,係具備: 用來進'行將離子交換樹脂充塡於該容器 無塵室。 9.如申請專利範圍第8項記載的離子交 設備,其中,係具備: 將離子交換樹脂以不接觸大氣的狀態進 精製手段、以及 將該精製手段所精製之離子交換樹脂經 接觸大氣的狀態朝充塡步驟移送之移送手段 1 〇 ·如申請專利範圍第8或9項記載的離 製作設備’其中,將進行精製處理之精製設 設置,在一個精製設備僅處理同一種類的離 關於不同種類之離子交換樹脂,是在不同的 處理。 1 1 ·如申請專利範圍第1 0項記載的離子 作設備,其中,將複數種類的離子交換樹脂 精製設備進行精製後,藉由不同的計量槽進 水,分析來自 〇 換裝置之製作 等級1 0 0 0以下 精製處理後的 置之設備,其 之充塡步驟的 換裝置之製作 行精製處理之 由配管而以不 〇 子交換裝置之 備複數個並列 子交換樹脂, 精製設備進行 交換裝置之製 分別在不同的 行計量之後, -40- 201127491 在混合槽混合而充塡於前述容器。 1 2 ·如申請專利範圍第8至1 1項中任一項記載的離子交 換裝置之製作設備,其中,前述無塵室之潔淨度爲等級 1 0 0 0 0以下。 1 3 .如申請專利範圍第8至1 2項中任一項記載的離子交 換裝置之製作設備’其中,係具備檢查手段; 該檢查手段,是對於充塡離子交換樹脂後之離子交換 裝置,在前述無塵室內進行超純水之通水,分析來自離子 交換裝置之流出水以檢查離子交換裝置。 14. 如申請專利範圍第13項記載的離子交換裝置之製 作設備,其中,係具備:用來進行前述流出水之分析之潔 淨度等級1 〇 〇 〇以下之高潔淨度無塵室。 15. —種離子交換裝置,其特徵在於:是藉由如申請 專利範圍第1至7項中任一項的方法所製造之離子交換裝置 〇 16. —種離子交換裝置,其特徵在於:是藉由如申請 專利範圍第8至1 4項中任一項的設備所製造之離子交換裝 置。 1 7. —種離子交換樹脂層之形成方法,是將離子交換 樹脂和水的混合漿體導入容器,將水藉由過濾器分離後從 容器排出,藉此在容器內充塡離子交換樹脂而形成離子交 換樹脂層的方法,其特徵在於: 離子交換樹脂和水的混合漿體是藉由流體壓驅動式栗 供應至容器, -41 - 201127491 當前述泵驅動用的流體壓到達既定壓力的時點,解除 作用於泵之流體壓而停止驅動泵。 1 8 .如申請專利範圍第1 7項記載的離子交換樹脂層之 形成方法,其中,當泵驅動用的流體壓到達既定壓力的時 點解除作用於泵之流體壓而停止驅動泵後,再度開始驅動 泵’當泵驅動用的流體壓再度到達既定壓力的時點,解除 作用於泵之流體壓而停止驅動泵。 1 9 .如申請專利範圍第1 7或1 8項記載的離子交換樹脂 層之形成方法,其中,容器係具備:連接於第1過濾器之 原水導入路、連接於第2過濾器之處理水取出路、以及樹 脂導入路; 通過樹脂導入路將離子交換樹脂和水的混合漿體導入 容器,藉由第1及/或第2過濾器將水分離後從原水導入路 及/或處理水取出路排出,藉此在容器內形成離子交換樹 脂層。 20.如申請專利範圍第17至19項中任一項記載的離子 交換樹脂層之形成方法,其中,流體壓驅動式泵是空氣壓 驅動式泵,且具備:當泵驅動用的空氣壓到達既定壓力的 時點,解除作用於泵之空氣壓而停止驅動泵之控制機構。 2 1.如申請專利範圍第17至20項中任一項記載的離子 交換樹脂層之形成方法,其中,流體壓驅動式泵是空氣壓 驅動式隔膜泵。 2 2 .如申請專利範圍第1 7至2 1項中任一項記載的離子 交換樹脂層之形成方法,其中,離子交換樹脂爲陽離子交 -42- 201127491 換樹脂和陰離子交換樹脂的混合樹脂》 2 3 .—種離子交換樹脂層之形成裝置,是將離子交換 樹脂和水的混合漿體導入容器,將水藉由過濾器分離後從 容器排出’藉此在容器內充塡離子交換樹脂而形成離子交 換樹脂層的裝置,其特徵在於,係具備: 將離子交換樹脂和水的混合漿體供應至容器之流體壓 驅動式泵、以及 當前述泵驅動用的流體壓到達既定壓力的時點,解除 作用於泵之流體壓而停止驅動泵之泵控制手段。 2 4.如申請專利範圍第23項記載的離子交換樹脂層之 形成裝置,其中,前述泵控制手段,當泵驅動用的流體壓 到達既定壓力的時點解除作用於泵之流體壓而停止驅動泵 後,再度開始驅動泵,當泵驅動用的流體壓再度到達既定 壓力的時點,解除作用於泵之流體壓而停止驅動泵。 2 5 .如申請專利範圍第2 3或2 4項記載的離子交換樹脂 層之形成裝置’其中,容器係具備:連接於第1過濾器之 原水導入路、連接於第2過濾器之處理水取出路、以及樹 脂導入路; 通過樹脂導入路將離子交換樹脂和水的混合漿體導入 容器’藉由第1及/或第2過濾器將水分離後從原水導入路 及/或處理水取出路排出,藉此在容器內形成離子交換樹 脂層。 2 6 .如申請專利範圍第2 3至2 5項中任一項記載的離子 交換樹脂層之形成裝置,其中,流體壓驅動式泵是空氣壓 -43- 201127491 驅動式泵; 前述泵控制手段,當泵驅動用的空氣壓到達既定壓力 的時點’解除作用於泵之空氣壓而停止驅動泵。 27. 如申請專利範圍第23至26項中任一項記載的離子 交換樹脂層之形成裝置,其中,流體壓驅動式泵是空氣壓 驅動式隔膜栗。 28. 如申請專利範圍第23至27項中任一項記載的離子 交換樹脂層之形成裝置,其中,離子交換樹脂爲陽離子交 換樹脂和陰離子交換樹脂的混合樹脂。 29. —種離子交換裝置,其特徵在於:係具有藉由如 申5H專利範圍第1 7至2 2項中任一項的方法所形成之離子交 換樹脂層。 3 〇.~種離子交換裝置,其特徵在於:係具有藉由如 申請專利範圍第23至28項中任一項的裝置所形成之離子交 換樹脂層。 -44-201127491 VII. Patent application scope: 1. A method for preparing an ion exchange device, which is a method for preparing an ion exchange device by charging a purified ion exchange resin to a container, wherein: the ion exchange resin is charged to the ion exchange resin. The filling step of the container is carried out in a clean room. 2. The method of producing an ion exchange apparatus according to the first aspect of the invention, wherein the ion exchange resin is subjected to a refining treatment in a state where it is not in contact with the atmosphere, and is transferred to the charging step without being exposed to the atmosphere via a pipe. 3. In the method for producing an ion exchange device according to the above-mentioned patent application, in the above, the 'purification equipment for performing the purification treatment is plural and arranged in parallel'. In one purification equipment, only the same type of ion exchange resin is processed, and different types are used. The ion exchange resin' is processed in different refining equipment. 4. The method for producing an ion exchange apparatus according to claim 3, wherein 'the plurality of types of ion exchange resins are separately purified in different refining apparatuses, and then metered in different metering tanks, and then in the mixing tank. Mix and fill the aforementioned container. _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ The method for producing an ion exchange bag according to any one of the items 1 to 5, wherein, in the ion-39-201127491 exchange device after charging the ion exchange resin, the ion of the ultrapure water is carried out in the dust-free chamber The ion exchange method according to the sixth aspect of the invention, wherein the analysis of the effluent water is performed in a clean room with high cleanliness and cleanliness. 8 - An apparatus for manufacturing an ion exchange apparatus is an apparatus for producing an ion exchange apparatus by charging an ion exchange resin to a container, and is characterized in that: the method is for: charging an ion exchange resin to the clean room of the container. 9. The ion exchange device according to claim 8, wherein the ion exchange resin is supplied to the atmosphere without being exposed to the atmosphere, and the ion exchange resin purified by the purification means is exposed to the atmosphere. Transfer means 1 which is transferred to the charging step 1 如 · As in the manufacturing equipment of the eighth or ninth aspect of the patent application, the purification processing is performed, and only one type of the same type is processed in one refining equipment. The ion exchange resin is treated differently. 1 1 The ion-making apparatus according to claim 10, wherein a plurality of types of ion exchange resin refining equipment are purified, and then water is introduced from different metering tanks to analyze the production level 1 from the tampering device. 0 0 0 The equipment after the refining process is replaced by a plurality of juxtaposed sub-exchange resins, and the refining device is exchanged by a non-twisting device. After the different lines are metered separately, -40-201127491 is mixed in the mixing tank to be filled with the aforementioned container. The apparatus for producing an ion exchange device according to any one of claims 8 to 11, wherein the clean room has a cleanliness level of 1 000 or less. The apparatus for manufacturing an ion exchange apparatus according to any one of the items of the present invention, wherein the inspection apparatus is an ion exchange apparatus after charging the ion exchange resin, The ultrapure water was passed through the clean room, and the effluent water from the ion exchange unit was analyzed to inspect the ion exchange unit. 14. The apparatus for producing an ion exchange apparatus according to claim 13, wherein the high cleanness clean room having a cleanliness level of 1 〇 〇 or less for performing the analysis of the effluent water is provided. An ion exchange apparatus, which is an ion exchange apparatus manufactured by the method of any one of claims 1 to 7, which is characterized in that it is An ion exchange apparatus manufactured by the apparatus of any one of claims 8 to 14. 1 7. A method of forming an ion exchange resin layer by introducing a mixed slurry of an ion exchange resin and water into a vessel, separating the water by a filter, and discharging the mixture from the vessel, thereby charging the vessel with an ion exchange resin. A method of forming an ion exchange resin layer, characterized in that: a mixed slurry of ion exchange resin and water is supplied to a container by a fluid pressure driven pump, -41 - 201127491 when the fluid pressure for driving the pump reaches a predetermined pressure The hydraulic pressure acting on the pump is released and the pump is stopped. The method for forming an ion-exchange resin layer according to the seventh aspect of the invention, wherein when the fluid pressure for pump driving reaches a predetermined pressure, the fluid pressure acting on the pump is released and the pump is stopped, and then starts again. The pump is driven to stop driving the pump when the fluid pressure for driving the pump reaches the predetermined pressure again, releasing the fluid pressure acting on the pump. The method for forming an ion exchange resin layer according to the first or seventh aspect of the invention, wherein the container includes a raw water introduction path connected to the first filter and a treated water connected to the second filter. The path and the resin introduction path are taken out; the mixed slurry of the ion exchange resin and water is introduced into the container through the resin introduction path, and the water is separated by the first and/or second filter, and then taken out from the raw water introduction path and/or the treated water. The road is discharged, thereby forming an ion exchange resin layer in the container. The method of forming an ion exchange resin layer according to any one of claims 17 to 19, wherein the fluid pressure driven pump is an air pressure driven pump and has: when the air pressure for driving the pump reaches At the time of the predetermined pressure, the control mechanism that drives the pump is stopped by releasing the air pressure acting on the pump. The method of forming an ion exchange resin layer according to any one of claims 17 to 20, wherein the fluid pressure driven pump is an air pressure driven diaphragm pump. The method for forming an ion exchange resin layer according to any one of claims 1 to 2, wherein the ion exchange resin is a mixed resin of a cation exchange-42-201127491 resin and an anion exchange resin. A device for forming an ion exchange resin layer is a method in which a mixed slurry of an ion exchange resin and water is introduced into a container, and water is separated by a filter and then discharged from the container, thereby charging the container with an ion exchange resin. An apparatus for forming an ion exchange resin layer, comprising: a fluid pressure driven pump that supplies a mixed slurry of ion exchange resin and water to a container, and a time when the fluid pressure for driving the pump reaches a predetermined pressure, The pump control means for stopping the driving of the pump by releasing the fluid pressure acting on the pump. 2. The apparatus for forming an ion exchange resin layer according to claim 23, wherein the pump control means stops the driving of the pump when the fluid pressure for driving the pump reaches a predetermined pressure. After that, the pump is started again, and when the fluid pressure for driving the pump reaches the predetermined pressure again, the fluid pressure acting on the pump is released and the pump is stopped. The apparatus for forming an ion exchange resin layer according to the above-mentioned patent application, wherein the container includes a raw water introduction path connected to the first filter and a treated water connected to the second filter. The path and the resin introduction path are taken out; the mixed slurry of the ion exchange resin and water is introduced into the container through the resin introduction path. The water is separated by the first and/or second filter, and then taken out from the raw water introduction path and/or the treated water. The road is discharged, thereby forming an ion exchange resin layer in the container. The apparatus for forming an ion exchange resin layer according to any one of claims 2 to 25, wherein the fluid pressure driven pump is an air pressure-43-201127491 driven pump; When the air pressure for pump driving reaches a predetermined pressure, the air pressure applied to the pump is released to stop driving the pump. The apparatus for forming an ion exchange resin layer according to any one of claims 23 to 26, wherein the fluid pressure driven pump is an air pressure driven diaphragm. The apparatus for forming an ion exchange resin layer according to any one of claims 23 to 27, wherein the ion exchange resin is a mixed resin of a cation exchange resin and an anion exchange resin. An ion exchange apparatus comprising an ion exchange resin layer formed by the method according to any one of the items of the above-mentioned. The ion exchange device is characterized in that it has an ion exchange resin layer formed by the apparatus according to any one of claims 23 to 28. -44-
TW099121231A 2009-06-30 2010-06-29 Ion exchange device, method of making the same, and device TWI494166B (en)

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JP2009155660A JP5391874B2 (en) 2009-06-30 2009-06-30 Manufacturing method of ion exchanger
JP2009266401A JP5407801B2 (en) 2009-11-24 2009-11-24 Method for forming ion exchange resin layer

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TWI551336B (en) 2016-10-01
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CN103342404A (en) 2013-10-09
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WO2011001871A1 (en) 2011-01-06

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