JP2023045790A - Treatment method of raw water for purified water production - Google Patents
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
Abstract
Description
本発明は、純水製造用原水の処理方法に係り、特に腐食様有機物を含む純水製造用原水の処理方法に関する。 The present invention relates to a method of treating raw water for pure water production, and more particularly to a method of treating raw water for pure water production containing corrosion-like organic matter.
半導体・電子材料洗浄用の超純水製造装置は、通常、前処理システム、一次純水システム、サブシステム等から構成されている。各システムはそれぞれ濁質、塩類、ＴＯＣなど様々な不純物を除去する装置で成り立っている。 An ultrapure water production system for cleaning semiconductors and electronic materials usually consists of a pretreatment system, a primary pure water system, subsystems, and the like. Each system consists of devices that remove various impurities such as turbidity, salts, and TOC.
図２は超純水製造装置の一例を示すフロー図である。図示の通り、超純水は、前処理装置１０、一次純水製造装置１１、二次純水製造装置（サブシステム）１２から構成される超純水製造設備で原水（工業用水、市水、井水等）を処理することにより製造される。 FIG. 2 is a flowchart showing an example of an ultrapure water production system. As shown in the figure, ultrapure water is produced from raw water (industrial water, city water, well water, etc.).
凝集、加圧浮上（または沈殿）、濾過（例えば膜濾過）装置などよりなる前処理装置１０は、原水中の懸濁物質やコロイド物質の除去を行う。また、この過程では高分子系有機物、疎水性有機物などの除去も可能である。 A pretreatment device 10 comprising a flocculation, pressure flotation (or sedimentation), filtration (eg, membrane filtration) device, etc. removes suspended solids and colloidal substances in the raw water. In this process, it is also possible to remove polymeric organic substances, hydrophobic organic substances, and the like.
逆浸透膜分離装置、脱気装置及びイオン交換装置（混床式又は４床５塔式など）を備える一次純水製造装置１１では、原水中のイオンや有機成分の除去を行う。なお、逆浸透膜分離装置では、塩類を除去すると共に、イオン性、コロイド性のＴＯＣを除去する。イオン交換装置では、塩類を除去すると共にイオン交換樹脂によって吸着又はイオン交換されるＴＯＣ成分の除去を行う。脱気装置では無機系炭素（ＩＣ）、溶存酸素の除去を行う。 A primary pure water production apparatus 11 equipped with a reverse osmosis membrane separation apparatus, a degassing apparatus, and an ion exchange apparatus (mixed bed type, 4-bed 5-tower type, etc.) removes ions and organic components from raw water. In addition, the reverse osmosis membrane separator removes salts as well as ionic and colloidal TOC. The ion exchange device removes salts and TOC components adsorbed or ion-exchanged by the ion exchange resin. The deaerator removes inorganic carbon (IC) and dissolved oxygen.
一次純水製造装置１１からの一次純水は、サブシステム１２において、タンク１４からポンプ１５により熱交換器１６に通水され、次いで紫外線（ＵＶ）照射装置（図４では低圧ＵＶ酸化装置）１７、イオン交換装置１８及び限外濾過（ＵＦ）膜分離装置１９で処理されて、超純水が製造される。低圧ＵＶ酸化装置１７では、ＵＶランプより照射される１８５ｎｍのＵＶによりＴＯＣを有機酸、さらにはＣＯ２まで分解する。分解により生成した有機物及びＣＯ２は後段のイオン交換装置（通常は混床式イオン交換装置）１８で除去される。ＵＦ膜分離装置１９では微粒子が除去され、イオン交換装置１８から流出するイオン交換樹脂の破片等も除去される。
Primary pure water from the primary pure water production device 11 is passed from a
このようにして得られた超純水は、配管２０よりユースポイント２１に送給され、余剰の超純水が配管２２よりタンク１４に戻される。
The ultrapure water obtained in this way is supplied to the point of use 21 through the
地下水、市水など、フミン酸、フルボ酸等の腐食様有機物を含む原水を処理して純水を製造する場合、凝集固液分離によって腐食様有機物を十分に除去する必要がある。 When raw water containing corrosive organic matter such as humic acid and fulvic acid, such as groundwater and city water, is treated to produce pure water, it is necessary to sufficiently remove the corrosive organic matter by solid-liquid separation.
即ち、イオン交換により純水を製造するプロセスにおいて、原水中にフミン酸、フルボ酸などの腐食様有機物が含まれる場合、腐食様有機物による汚染でイオン交換樹脂の交換容量が低下する。そのため、従来では、上記のような原水をイオン交換樹脂に通水する前処理として、ＴＯＣに対して数十倍以上の濃度の凝集剤を用いて凝集および固液分離（加圧浮上や濾過）を行うことにより腐食様有機物を除去する。なお、フミン酸、フルボ酸などの腐食様有機物は、それ自身が凝集効果を低下させる因子にもなる。 That is, in the process of producing pure water by ion exchange, if the raw water contains corrosive organic substances such as humic acid and fulvic acid, contamination with the corrosive organic substances reduces the exchange capacity of the ion exchange resin. Therefore, conventionally, as a pretreatment for passing the above raw water through an ion exchange resin, flocculation and solid-liquid separation (pressure flotation and filtration) using a flocculant with a concentration of several tens of times or more that of TOC to remove corrosion-like organic matter. Corrosion-like organic substances such as humic acid and fulvic acid themselves are also factors that reduce the aggregation effect.
凝集処理により生じたフロックは、加圧浮上や濾過器などの固液分離装置で除去される。この固液分離で発生したスカムや汚泥は、産業廃棄物として処分される場合、処分コストが発生する。 Flocs generated by the flocculation treatment are removed by a solid-liquid separation device such as pressure flotation or a filter. When the scum and sludge generated by this solid-liquid separation are disposed of as industrial waste, disposal costs are incurred.
また、凝集ｐＨは酸性側で行うことが多く、原水の緩衝作用が大きい場合には酸薬品の消費量も多くなる。 In addition, the coagulation pH is often carried out on the acidic side, and when the raw water has a large buffering effect, the consumption of acid chemicals increases.
本発明は、凝集剤やｐＨ調整剤等の薬剤の使用を無くしたり、使用量を少なくしたりしても腐食様有機物を十分に除去し、イオン交換樹脂への悪影響を低減することができる純水製造用原水の処理方法を提供することを課題とする。 The present invention can eliminate the use of agents such as flocculants and pH adjusters, or even if the amount used is reduced, can sufficiently remove corrosion-like organic substances and reduce the adverse effects on ion exchange resins. An object of the present invention is to provide a method for treating raw water for water production.
本発明の純水製造用原水の処理方法は、腐食様有機物を含む原水を処理して純水を製造する純水製造用原水の処理方法において、腐食様有機物を含む原水をオゾン酸化処理した後、イオン交換処理することを特徴とする。 The method for treating raw water for producing pure water according to the present invention is a method for treating raw water for producing pure water by treating raw water containing corrosive-like organic substances to produce pure water. , is characterized by ion exchange treatment.
本発明の一態様では、前記オゾン酸化処理後、還元処理し、その後前記イオン交換処理を行う。 In one aspect of the present invention, after the ozone oxidation treatment, the reduction treatment is performed, and then the ion exchange treatment is performed.
本発明の一態様では、前記オゾン酸化処理を行うに際して、原水中のＴＯＣ１ｍｇ／Ｌに対してオゾンを１～１０ｍｇ／Ｌ添加する。 In one aspect of the present invention, when performing the ozone oxidation treatment, 1 to 10 mg/L of ozone is added to 1 mg/L of TOC in the raw water.
本発明によると、フミン酸、フルボ酸などの腐食様有機物がオゾンにより酸化分解されるので、イオン交換樹脂の汚染が低減される。 According to the present invention, since corrosion-like organic substances such as humic acid and fulvic acid are oxidatively decomposed by ozone, contamination of the ion exchange resin is reduced.
本発明の一態様では、オゾン処理後段で還元処理（活性炭塔への通水や重亜硫酸ソーダの注入など）を行うことにより、イオン交換樹脂に酸化剤が流入することが防止される。 In one aspect of the present invention, reduction treatment (such as passing water through an activated carbon tower or injecting sodium bisulfite) is performed after the ozone treatment, thereby preventing the oxidant from flowing into the ion exchange resin.
以下、図１を参照して実施の形態について説明する。 An embodiment will be described below with reference to FIG.
フミン酸やフルボ酸等の腐食様有機物を含む原水は、オゾン酸化工程１にてオゾン添加により腐食様有機物の分解処理が行われた後、還元処理工程２において残留するオゾンの還元処理が行われ、次いでイオン交換工程３にてイオン交換処理される。
Raw water containing corrosive organic matter such as humic acid and fulvic acid is subjected to decomposition treatment of the corrosive organic matter by addition of ozone in the
原水としては、腐食様有機物を含む地下水、市水、河川水、工業用水、工場排水などが例示されるが、これに限定されない。原水中の腐食様有機物としては、フミン酸やフルボ酸などが例示されるが、これに限定されない。原水のＴＯＣ濃度は０．５～３ｍｇ／Ｌ特に０．８～１．５ｍｇ／Ｌ程度であるが、これよりも少なくても、また多くてもよい。 Examples of raw water include, but are not limited to, groundwater containing corrosive organic matter, city water, river water, industrial water, and factory wastewater. Examples of corrosion-like organic substances in raw water include humic acid and fulvic acid, but are not limited to these. The TOC concentration of raw water is about 0.5-3 mg/L, especially about 0.8-1.5 mg/L, but it may be less or more than this.
なお、必要であれば、原水を凝集及び固液分離処理した後、オゾン酸化工程１に送ってもよい。
If necessary, the raw water may be sent to the
オゾン酸化工程１でのオゾン添加は、原水中のＴＯＣ１ｍｇ／Ｌに対しオゾンを１～１０ｍｇ／Ｌ特に２～６ｍｇ／Ｌ程度の割合で添加するように行われることが好ましい。
The addition of ozone in the
オゾン酸化工程では、原水を反応槽内に下降流で通水し、該反応槽の下部にオゾン含有ガスを散気ノズルによって吹き込むように構成されたオゾン添加手段等によりオゾンが添加される。反応槽内の滞留時間は１～１０ｍｉｎ特に３～７ｍｉｎ程度が好適である。ただし、オゾン添加手段はこれに限定されない。オゾン含有ガスは、空気をオゾン発生器に通気することにより生成させたものが好ましい。 In the ozone oxidation step, raw water is passed through the reaction tank in a downward flow, and ozone is added by an ozone adding means or the like configured to blow an ozone-containing gas into the lower part of the reaction tank through an aeration nozzle. The residence time in the reaction tank is preferably about 1 to 10 minutes, especially about 3 to 7 minutes. However, the ozone adding means is not limited to this. The ozone-containing gas is preferably produced by passing air through an ozone generator.
このオゾン酸化処理により、腐食様有機物が低分子化されるが、ＣＯ２まで酸化される必要はない。 By this ozone oxidation treatment, corrosion-like organic substances are reduced in molecular weight, but they do not need to be oxidized to CO2 .
オゾン酸化処理水中には、オゾンが残留するので、還元処理工程２にてオゾンを還元処理することが好ましい。この還元処理は、活性炭塔への通水、あるいは重亜硫酸ナトリウム等の還元剤の添加などにより行われる。
Since ozone remains in the ozone-oxidized water, it is preferable to reduce the ozone in the
このように腐食様有機物をオゾン酸化処理し、その後必要に応じ還元処理した後、イオン交換工程３にてイオン交換処理することにより純水が製造される。
In this way, the corrosion-like organic substances are subjected to ozone oxidation treatment, and then reduction treatment if necessary, followed by ion exchange treatment in the
イオン交換工程は、被処理水をイオン交換設備に通水することにより行われるのが好ましい。イオン交換設備としては、混床式イオン交換塔、２床３塔式イオン交換装置、３床４塔式イオン交換装置、４床５塔式イオン交換装置などを用いることができる。通水方式としては、上向流式、下向流式のどちらも用いることができる。再生方式としては、並流再生式、向流再生式のどちらも用いることができる。 The ion exchange step is preferably carried out by passing the water to be treated through an ion exchange facility. As the ion exchange equipment, a mixed bed ion exchange tower, a 2-bed 3-tower ion exchanger, a 3-bed 4-tower ion exchange equipment, a 4-bed 5-tower ion exchange equipment and the like can be used. As a water flow system, either an upward flow system or a downward flow system can be used. As a regeneration method, both a cocurrent regeneration method and a countercurrent regeneration method can be used.
かかる本発明の純水製造用原水の処理方法によると、原水中に含まれる腐食様有機物由来のＴＯＣ成分をオゾンにより酸化分解することで、イオン交換樹脂への悪影響を低減することができる。腐食様有機物由来のＴＯＣをＣＯ２まで酸化分解する必要はないため、注入量はＴＯＣ１ｍｇ／Ｌ程度に対して数ｍｇ／Ｌ ａｓ Ｏ３程度でも効果がある。 According to the method for treating raw water for pure water production of the present invention, the TOC component derived from corrosion-like organic matter contained in the raw water is oxidatively decomposed by ozone, thereby reducing adverse effects on the ion exchange resin. Since it is not necessary to oxidatively decompose TOC derived from corrosion-like organic substances into CO 2 , even an injection amount of about several mg/L as O 3 for about 1 mg/L of TOC is effective.
また、本発明の純水製造用原水の処理方法によると、従来法に比べてｐＨ調整剤や凝集剤の添加が不要又は少量となり、薬品コストが低減可能である。また、従来法に比べ汚泥の発生量が少なく、汚泥処理コストが下がる。 Moreover, according to the method of treating raw water for producing pure water according to the present invention, the addition of a pH adjuster or a flocculating agent becomes unnecessary or less than in the conventional method, and chemical costs can be reduced. In addition, the amount of sludge generated is less than that of the conventional method, and the cost of sludge treatment is reduced.
オゾンによる腐食様有機物の分解効果を確認するために、以下の試験を行った In order to confirm the decomposition effect of corrosion-like organic matter by ozone, the following tests were conducted.
［試験方法］
下記水質の井水に対して、空気をオゾン発生器に通気することにより生成させた、オゾン濃度４．５ｖｏｌ％のオゾン含有ガスを散気ノズルから散気することにより添加した。オゾン注入量を０，１，３，５，７ｍｇ／Ｌと変化させて酸化反応させ、その処理水を０．４５μｍのメンブレンフィルターで濾過し、処理水を三次元励起蛍光分光法（ＥＥＭ）により分析した。ＥＥＭでの分析結果をＰＡＲＡＦＡＣ解析（ＥＥＭ－ＰＡＲＡＦＡＣ解析）し、ＴＯＣ成分がイオン交換樹脂へ悪影響を与える度合を数値化した。
＜井水の水質＞
ｐＨ：７．５
導電率：３０ｍＳ／ｍ
濁度：４度
色度：６０度
ＳＳ：３ｍｇ／Ｌ
Ｍアルカリ度：１３０ｍｇ／Ｌ ａｓ ＣａＣＯ３
全硬度：６０ｍｇ／Ｌ
ナトリウム濃度：３０ｍｇ／Ｌ
ＴＯＣ：１．５ｍｇ／Ｌ
ＵＶ２６０：１．３（－ｌｏｇＴ）
[Test method]
An ozone-containing gas having an ozone concentration of 4.5 vol %, which was generated by passing air through an ozone generator, was added to well water having the following water quality by diffusing from an aeration nozzle. The amount of ozone injected was changed to 0, 1, 3, 5, and 7 mg/L for an oxidation reaction, the treated water was filtered through a 0.45 μm membrane filter, and the treated water was subjected to three-dimensional excitation fluorescence spectroscopy (EEM). analyzed. The EEM analysis results were subjected to PARAFAC analysis (EEM-PARAFAC analysis) to quantify the extent to which the TOC components adversely affect the ion exchange resin.
<Well water quality>
pH: 7.5
Conductivity: 30mS/m
Turbidity: 4 degrees Chromaticity: 60 degrees SS: 3 mg/L
M alkalinity: 130mg/L as CaCO3
Total hardness: 60mg/L
Sodium concentration: 30mg/L
TOC: 1.5 mg/L
UV260: 1.3 (-logT)
＜ＴＯＣ成分がイオン交換樹脂へ悪影響を与える度合の測定及び指数値化＞
ＴＯＣ成分がイオン交換樹脂に与える悪影響度を次のようにして測定及び指数値化した。すなわち、イオン交換樹脂に悪影響を与える蛍光性溶存有機物の種類によるピーク出現位置を定義し、測定して得られたピークを成分ごとに分離して解析した。結果は次の通りである。
<Measurement and Indexation of Degree of Adverse Effects of TOC Components on Ion Exchange Resin>
The adverse effect of the TOC component on the ion exchange resin was measured and indexed as follows. That is, the peak appearance positions were defined according to the types of fluorescent dissolved organic substances that adversely affect the ion exchange resin, and the peaks obtained by measurement were separated and analyzed for each component. The results are as follows.
＜悪影響度指数値＞
原水（オゾン処理なし）：５７７
オゾン１ｍｇ／Ｌ注入時：１７１
オゾン３ｍｇ／Ｌ注入時：５２
オゾン５ｍｇ／Ｌ注入時：３１
オゾン７ｍｇ／Ｌ注入時：３１
<Adverse effect index value>
Raw water (no ozone treatment): 577
When
When
When ozone 5 mg/L is injected: 31
When ozone 7mg/L is injected: 31
［考察］
オゾンの添加量が増加するに従い、腐食物質の樹脂への悪影響度の指数は低下した。今回の原水のＴＯＣ濃度は約１．５ｍｇ／Ｌであり、オゾン添加量を約５ｐｐｍ程度添加することで、十分に樹脂の悪影響度が低下することが明らかとなった。
[Discussion]
As the amount of ozone added increased, the index of the degree of adverse effect of corrosive substances on the resin decreased. The TOC concentration of the raw water this time was about 1.5 mg/L, and it was found that adding about 5 ppm of ozone sufficiently reduced the adverse effect of the resin.
１ オゾン酸化工程
２ 還元処理工程
３ イオン交換工程
１０ 前処理装置
１１ 一次純水製造装置
１２ サブシステム
REFERENCE SIGNS
Claims (3)
腐食様有機物を含む原水をオゾン酸化処理した後、イオン交換処理することを特徴とする純水製造用原水の処理方法。 In a method for treating raw water for producing pure water for producing pure water by treating raw water containing corrosive organic matter,
A method for treating raw water for producing pure water, comprising subjecting raw water containing corrosive organic matter to ozone oxidation treatment and then to ion exchange treatment.
3. The method for treating raw water for producing pure water according to claim 1, wherein ozone is added in an amount of 1 to 10 mg/L per 1 mg/L of TOC in the raw water when the ozone oxidation treatment is carried out.
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| PCT/JP2022/025089 WO2023047732A1 (en) | 2021-09-22 | 2022-06-23 | Method for treating raw water for producing purified water |
| TW111124809A TW202313486A (en) | 2021-09-22 | 2022-07-01 | Method for treating raw water for producing purified water |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07241598A (en) * | 1994-03-04 | 1995-09-19 | Nomura Micro Sci Co Ltd | Water treatment apparatus |
| JPH11262783A (en) * | 1998-03-17 | 1999-09-28 | Japan Organo Co Ltd | Removal of organic matter in water |
| JPH11290878A (en) * | 1998-02-16 | 1999-10-26 | Japan Organo Co Ltd | Control method for removing toc component |
-
2021
- 2021-09-22 JP JP2021154361A patent/JP2023045790A/en active Pending
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2022
- 2022-06-23 WO PCT/JP2022/025089 patent/WO2023047732A1/en unknown
- 2022-07-01 TW TW111124809A patent/TW202313486A/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07241598A (en) * | 1994-03-04 | 1995-09-19 | Nomura Micro Sci Co Ltd | Water treatment apparatus |
| JPH11290878A (en) * | 1998-02-16 | 1999-10-26 | Japan Organo Co Ltd | Control method for removing toc component |
| JPH11262783A (en) * | 1998-03-17 | 1999-09-28 | Japan Organo Co Ltd | Removal of organic matter in water |
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| TW202313486A (en) | 2023-04-01 |
| WO2023047732A1 (en) | 2023-03-30 |
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