JP2002210494A - Device for manufacturing extrapure water - Google Patents
Device for manufacturing extrapure waterInfo
- Publication number
- JP2002210494A JP2002210494A JP2001010433A JP2001010433A JP2002210494A JP 2002210494 A JP2002210494 A JP 2002210494A JP 2001010433 A JP2001010433 A JP 2001010433A JP 2001010433 A JP2001010433 A JP 2001010433A JP 2002210494 A JP2002210494 A JP 2002210494A
- Authority
- JP
- Japan
- Prior art keywords
- water
- ion exchange
- membrane
- toc
- ultrapure water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は超純水製造装置に係
り、特に溶存酸素（ＤＯ）、全有機態酸素（ＴＯＣ）及
び過酸化水素（Ｈ２Ｏ２）等の酸化性物質濃度が極めて
低い超純水を製造することができる超純水製造装置に関
する。The present invention relates to relates to ultrapure water production system, particularly the dissolved oxygen (DO), oxidizing agent concentration, such as total organic state oxygen (TOC) and hydrogen peroxide (H 2 O 2) is very The present invention relates to an ultrapure water production device capable of producing low ultrapure water.
【０００２】[0002]
【従来の技術】従来、半導体洗浄用水として用いられて
いる超純水は、図３に示すように前処理システム１、一
次純水システム２及びサブシステム３から構成される超
純水製造装置で原水（工業用水、市水、井水等）を処理
することにより製造されている。図３において、各シス
テムの役割は次の通りである。2. Description of the Related Art Conventionally, ultrapure water used as semiconductor cleaning water is an ultrapure water producing apparatus comprising a pretreatment system 1, a primary pure water system 2 and a subsystem 3, as shown in FIG. It is manufactured by treating raw water (industrial water, city water, well water, etc.). In FIG. 3, the role of each system is as follows.
【０００３】凝集、加圧浮上（沈殿）、濾過装置等より
なる前処理システム１では、原水中の懸濁物質やコロイ
ド物質の除去を行う。逆浸透（ＲＯ）膜分離装置、脱気
装置及びイオン交換装置（混床式、２床３塔式又は４床
５塔式）を備える一次純水システム２では原水中のイオ
ンや有機成分の除去を行う。なお、ＲＯ膜分離装置で
は、塩類除去のほかにイオン性、コロイド性のＴＯＣを
除去する。イオン交換装置では、塩類除去のほかにイオ
ン交換樹脂によって吸着又はイオン交換されるＴＯＣ成
分を除去する。脱気装置（窒素脱気又は真空脱気）では
溶存酸素の除去を行う。[0003] In a pretreatment system 1 including a coagulation, pressure flotation (sedimentation), and a filtration device, suspended substances and colloid substances in raw water are removed. In the primary pure water system 2 equipped with a reverse osmosis (RO) membrane separation device, a degassing device, and an ion exchange device (mixed bed type, two beds three columns type or four beds five columns type), removal of ions and organic components in raw water is performed. I do. The RO membrane separation device removes ionic and colloidal TOC in addition to removing salts. The ion exchange device removes TOC components adsorbed or ion-exchanged by an ion exchange resin in addition to removing salts. In a deaerator (nitrogen deaeration or vacuum deaeration), dissolved oxygen is removed.
【０００４】熱交換器、低圧紫外線（ＵＶ）酸化装置、
混床式イオン交換装置及び限外濾過（ＵＦ）膜分離装置
を備えるサブシステム３では、水の純度をより一層高め
超純水にする。なお、低圧ＵＶ酸化装置では、低圧ＵＶ
ランプより出される波長１８５ｎｍの紫外線によりＴＯ
Ｃを有機酸さらにはＣＯ２まで分解する。分解された有
機物及びＣＯ２は後段のイオン交換樹脂で除去される。
ＵＦ膜分離装置では、微小粒子が除去されイオン交換樹
脂の流出粒子も除去される。Heat exchangers, low pressure ultraviolet (UV) oxidizers,
In the subsystem 3 including the mixed-bed ion exchange device and the ultrafiltration (UF) membrane separation device, the purity of water is further increased to ultrapure water. In the low-pressure UV oxidation device, low-pressure UV
TO with UV of 185nm wavelength emitted from lamp
Decomposing C and organic acids to CO 2. The decomposed organic matter and CO 2 are removed by the subsequent ion exchange resin.
In the UF membrane separation device, the fine particles are removed, and the outflow particles of the ion exchange resin are also removed.
【０００５】特開平９−２９２５１号公報には、このよ
うな超純水製造装置において、サブシステム３の混床式
イオン交換装置とＵＦ膜分離装置との間に膜式脱気装置
を設けることにより、得られる超純水のＤＯを低減する
ことが提案されている。この超純水製造装置であれば、
ＵＶ酸化装置から混床式イオン交換装置を通ることによ
り発生したＤＯを膜式脱気装置で除去することにより、
得られる超純水中のＤＯの値を低下させることができ
る。即ち、水中のＴＯＣに対しＵＶ酸化装置のＵＶ照射
量が過剰になるとＨ２Ｏ２が発生し、生成したＨ２Ｏ２
が後段の混床式イオン交換装置のイオン交換樹脂と接触
して分解され、酸素が生成し、これがＤＯを増加させる
原因となっていることから、特開平９−２９２５１号公
報の超純水製造装置では、混床式イオン交換装置の後段
に膜式脱気装置を設け、この膜式脱気装置でＤＯを除去
する。Japanese Patent Application Laid-Open No. 9-29251 discloses that in such an ultrapure water production apparatus, a membrane deaerator is provided between the mixed bed type ion exchange apparatus of the subsystem 3 and the UF membrane separation apparatus. It has been proposed to reduce the DO of ultrapure water obtained. With this ultrapure water production device,
By removing DO generated by passing through the mixed bed type ion exchange device from the UV oxidation device with the membrane type deaerator,
The value of DO in the obtained ultrapure water can be reduced. That is, when the UV irradiation amount of the UV oxidizing device becomes excessive with respect to the TOC in water, H 2 O 2 is generated, and the generated H 2 O 2
Is decomposed by contact with the ion-exchange resin of the subsequent mixed-bed type ion-exchange device, and oxygen is generated, which causes an increase in DO. Therefore, the production of ultrapure water disclosed in JP-A-9-29251 is disclosed. In the apparatus, a membrane deaerator is provided downstream of the mixed bed ion exchanger, and DO is removed by the membrane deaerator.
【０００６】ところで、ＵＶ酸化装置で発生したＨ２Ｏ
２は混床式イオン交換装置のイオン交換樹脂と接触する
と分解されるが、その際、イオン交換樹脂を劣化させ、
イオン交換樹脂の分解でイオン交換樹脂由来のＴＯＣが
生成し、得られる超純水の水質低下の原因となる。ま
た、混床式イオン交換装置に通水後もなお残留するＨ２
Ｏ２は、混床式イオン交換装置の後段の膜式脱気装置の
脱気膜を劣化させる。[0006] By the way, H 2 O generated by the UV oxidation device
2 is decomposed when it comes into contact with the ion exchange resin of the mixed bed type ion exchange device.
TOC derived from the ion exchange resin is generated by the decomposition of the ion exchange resin, which causes a deterioration in the quality of the obtained ultrapure water. Further, H 2 still remaining after passing water through the mixed bed type ion exchange device.
O 2 degrades the degassing membrane of the membrane degasser located downstream of the mixed bed ion exchange device.
【０００７】そこで、このようなＨ２Ｏ２に起因する問
題を解決するために、ＵＶ酸化装置と混床式イオン交換
装置との間にアニオン交換樹脂を充填したアニオン交換
塔や、炭素系吸着剤を充填した吸着塔を設け、ＵＶ酸化
装置で生成したＨ２Ｏ２を混床式イオン交換装置の前段
で除去した後、混床式イオン交換装置に通水することも
提案されている。[0007] In order to solve such problems caused by H 2 O 2 , an anion exchange tower filled with an anion exchange resin between a UV oxidizer and a mixed bed type ion exchanger has been proposed. It has also been proposed to provide an adsorption tower filled with an agent, remove H 2 O 2 generated by a UV oxidizer at a stage preceding the mixed bed ion exchanger, and then pass water through the mixed bed ion exchanger.
【０００８】[0008]
【発明が解決しようとする課題】アニオン交換塔や吸着
塔を設けて混床式イオン交換装置の前段でＨ２Ｏ２を除
去することにより、Ｈ２Ｏ２に起因する混床式イオン交
換装置のイオン交換樹脂の劣化や膜式脱気装置の脱気膜
の劣化の問題は解消されるが、従来の超純水製造装置で
は、ＴＯＣの発生に対しての十分な配慮がなされていな
いために、ＴＯＣ濃度の低い超純水を得ることができな
いという問題があった。A mixed bed type ion exchange apparatus caused by H 2 O 2 is provided by providing an anion exchange tower or an adsorption tower and removing H 2 O 2 in a stage preceding the mixed bed type ion exchange apparatus. Although the problems of deterioration of the ion exchange resin and deterioration of the deaeration membrane of the membrane deaerator can be solved, the conventional ultrapure water production apparatus does not give sufficient consideration to the generation of TOC. In addition, there is a problem that ultrapure water having a low TOC concentration cannot be obtained.
【０００９】即ち、Ｈ２Ｏ２がアニオン交換樹脂と接触
することにより、Ｈ２Ｏ２が分解除去されるが、これに
より、アニオン交換樹脂の劣化による樹脂由来のＴＯＣ
の溶出の問題がある。また、炭素系吸着剤でもＴＯＣ溶
出の問題がある。また、アニオン交換樹脂や活性炭によ
るＨ２Ｏ２分解では、分解により酸素が生成して後段の
脱気装置の負荷を増加させる問題がある。That is, when H 2 O 2 comes into contact with the anion exchange resin, H 2 O 2 is decomposed and removed.
There is a problem of elution. Further, there is a problem of TOC elution even with a carbon-based adsorbent. In addition, in the decomposition of H 2 O 2 using an anion exchange resin or activated carbon, there is a problem that oxygen is generated by the decomposition and the load on the subsequent deaerator is increased.
【００１０】本発明は上記従来の問題点を解決し、Ｄ
Ｏ、ＴＯＣ、Ｈ２Ｏ２等の酸化性物質濃度が著しく低い
高純度の超純水を製造することができる超純水製造装置
を提供することを目的とする。The present invention solves the above-mentioned conventional problems, and
It is an object of the present invention to provide an ultrapure water production apparatus capable of producing high purity ultrapure water having extremely low concentrations of oxidizing substances such as O, TOC, and H 2 O 2 .
【００１１】[0011]
【課題を解決するための手段】本発明の超純水製造装置
は、１８５ｎｍ付近の波長を有する紫外線を照射する紫
外線酸化装置と、触媒式酸化性物質分解装置と、脱気装
置と、混床式イオン交換装置と、微粒子分離膜装置とを
有し、この順に通水可能としたことを特徴とする。An ultrapure water producing apparatus according to the present invention comprises an ultraviolet oxidizing apparatus for irradiating an ultraviolet ray having a wavelength of about 185 nm, a catalytic oxidizing substance decomposing apparatus, a deaerator and a mixed bed. It has a characteristic ion exchange device and a fine particle separation membrane device, and water can be passed in this order.
【００１２】酸化性物質を触媒で分解する触媒式酸化性
物質分解装置であれば、酸化性物質の分解効率が高く、
しかもＨ２Ｏ２等の酸化性物質と接触することによる劣
化及びＴＯＣ溶出の問題もない。さらに、触媒式酸化性
物質分解装置の場合、Ｈ２Ｏ ２を分解すると水が生成す
るが、酸素は殆ど生成せず、後段の脱気装置の負荷を増
大させることがない。Catalytic oxidization in which oxidizing substances are decomposed with a catalyst
With a substance decomposition device, the decomposition efficiency of oxidizing substances is high,
And H2O2Poor contact with oxidizing substances such as
There is no problem of conversion and TOC elution. In addition, catalytic oxidation
In the case of a material decomposition device, H2O 2Decomposes to produce water
However, almost no oxygen was generated, increasing the load on the downstream degasser.
I won't make it big.
【００１３】また、この触媒を活性炭やイオン交換樹脂
等の担体に担持して用いる場合でも、担体表面に触媒が
担持され、Ｈ２Ｏ２は触媒表面で直ちに分解されるた
め、Ｈ ２Ｏ２により担体が劣化してＴＯＣを溶出させる
こともない。[0013] The catalyst may be activated carbon or ion exchange resin.
Even when used on a carrier such as
Carried, H2O2Is immediately decomposed on the catalyst surface
H 2O2Degrades carrier and elutes TOC
Not even.
【００１４】[0014]
【発明の実施の形態】以下、図面を参照して本発明の超
純水製造装置を詳細に説明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The ultrapure water production apparatus of the present invention will be described below in detail with reference to the drawings.
【００１５】図１は本発明の超純水製造装置の実施の形
態を示す系統図である。FIG. 1 is a system diagram showing an embodiment of an ultrapure water production apparatus according to the present invention.
【００１６】この超純水製造装置では、各種前処理工程
より得られた一次純水（通常の場合、ＴＯＣ濃度２ｐｐ
ｂ以下の純水）をサブタンク１１、ポンプＰ、熱交換器
１２、ＵＶ酸化装置１３、触媒式酸化性物質分解装置１
４、脱気装置１５、混床式イオン交換装置１６及び微粒
子分離膜装置１７に順次に通水し、得られた超純水をユ
ースポイント１８に送る。In this ultrapure water producing apparatus, primary pure water obtained from various pretreatment steps (usually, a TOC concentration of 2 pp
b or less pure water) into a sub-tank 11, a pump P, a heat exchanger 12, a UV oxidizer 13, a catalytic oxidizer 1
4. Water is sequentially passed through the deaerator 15, the mixed bed type ion exchange device 16 and the fine particle separation membrane device 17, and the obtained ultrapure water is sent to the use point 18.
【００１７】ＵＶ酸化装置１３としては、通常、超純水
製造装置に用いられる１８５ｎｍ付近の波長を有するＵ
Ｖを照射するＵＶ酸化装置、例えば低圧水銀ランプを用
いたＵＶ酸化装置を用いることができる。このＵＶ酸化
装置１３で、一次純水中のＴＯＣが有機酸、更にはＣＯ
２に分解される。また、このＵＶ酸化装置１３では過剰
に照射されたＵＶにより、水からＨ２Ｏ２が発生する。As the UV oxidizing device 13, a UV oxidizing device having a wavelength of around 185 nm, which is usually used in
A UV oxidizer that irradiates V, for example, a UV oxidizer using a low-pressure mercury lamp can be used. In this UV oxidizer 13, TOC in the primary purified water is converted into an organic acid,
Decomposed into 2 . Further, in the UV oxidizing apparatus 13, H 2 O 2 is generated from water due to excessively irradiated UV.
【００１８】ＵＶ酸化装置の処理水は、次いで触媒式酸
化性物質分解装置１４に通水される。触媒式酸化性物質
分解装置１４の酸化性物質分解触媒としては、酸化還元
触媒として知られる貴金属触媒、例えば、金属パラジウ
ム、酸化パラジウム、水酸化パラジウム等のパラジウム
（Ｐｄ）化合物又は白金（Ｐｔ）、なかでも還元作用の
強力なパラジウム触媒を好適に使用することができる。
このような貴金属触媒はそのままで用いても良く、二酸
化チタン、アルミナ、活性炭、ゼオライト、イオン交換
樹脂等の担体に担持させて用いても良い。触媒を担体に
担持させる場合、触媒の担持量は通常担体に対する触媒
の担持重量で０．１〜１０重量％とすることが好まし
い。The treated water of the UV oxidizing device is then passed through a catalytic oxidizing substance decomposing device 14. As the oxidizing substance decomposition catalyst of the catalytic oxidizing substance decomposition apparatus 14, a noble metal catalyst known as a redox catalyst, for example, palladium (Pd) compound such as metal palladium, palladium oxide, palladium hydroxide or platinum (Pt), Among them, a palladium catalyst having a strong reducing action can be suitably used.
Such a noble metal catalyst may be used as it is, or may be used by being supported on a carrier such as titanium dioxide, alumina, activated carbon, zeolite, or ion exchange resin. When the catalyst is supported on a carrier, the amount of the supported catalyst is usually preferably 0.1 to 10% by weight based on the weight of the catalyst supported on the carrier.
【００１９】担体としては、ＴＯＣ溶出の恐れが全くな
い二酸化チタン、アルミナ、ゼオライトが好ましいが、
活性炭やイオン交換樹脂を担体として使用した場合で
も、担体表面に触媒が担持され、Ｈ２Ｏ２と接触しても
触媒表面で直ちにＨ２Ｏ２が分解されるため、Ｈ２Ｏ２
が担体を劣化させることは殆どない。As the carrier, titanium dioxide, alumina and zeolite, which have no possibility of TOC elution, are preferable.
Activated carbon or ion exchange resins even when used as a carrier, since the catalyst on the carrier surface is supported immediately H 2 O 2 at the catalyst surface is decomposed on contact with the H 2 O 2, H 2 O 2
Hardly degrades the carrier.
【００２０】なお、アニオン交換樹脂にパラジウムを担
持させるにはアニオン交換樹脂をカラムに充填し、次い
で塩化パラジウムの酸性溶液を通水すればよい。金属パ
ラジウムとして担持させるのであれば、さらにホルマリ
ンなどを加えて還元すればよい。In order to carry palladium on the anion exchange resin, the column may be filled with the anion exchange resin and then an acidic solution of palladium chloride may be passed through. If it is carried as metal palladium, it may be reduced by further adding formalin or the like.
【００２１】触媒の形状は、粉末状、粒状、ベレット状
など何れの形状でも利用できる。粉末状のものを使用す
る場合には、反応槽を設けてこの反応槽に適当量添加す
れば良い。また、粒状又はペレット状のものはカラム等
に充填し、ＵＶ酸化装置１３の処理水を連続的に通水し
て処理することができ、有利である。ただし、粉末状の
ものでも、流動床を形成することによって連続処理に使
用することができる。The catalyst can be used in any shape such as powder, granule, and bellet. When a powdery material is used, a reaction tank may be provided and an appropriate amount may be added to the reaction tank. In addition, the granular or pellet-like material is advantageously packed in a column or the like, and the treated water of the UV oxidation device 13 can be continuously passed through for treatment. However, a powdery material can be used for continuous processing by forming a fluidized bed.
【００２２】この触媒式酸化性物質分解装置１４によ
り、ＴＯＣの溶出の問題を生じることなく、ＵＶ酸化装
置１３で発生したＨ２Ｏ２、その他の酸化性物質が触媒
により効率的に分解除去される。そして、Ｈ２Ｏ２の分
解により、水は生成するが、アニオン交換樹脂や活性炭
のように酸素を生成させることは殆どなく、ＤＯ増加の
原因とならない。The catalytic oxidizing substance decomposing device 14 efficiently decomposes and removes H 2 O 2 and other oxidizing substances generated in the UV oxidizing device 13 without causing the problem of TOC elution. You. Water is generated by the decomposition of H 2 O 2 , but hardly generates oxygen unlike an anion exchange resin or activated carbon, and does not cause an increase in DO.
【００２３】酸化性物質１４の処理水は、次いで脱気装
置１５に通水される。脱気装置１５としては、従来の一
次純水システム２に用いられるような真空脱気装置、窒
素脱気装置や特開平９−２９２５１号公報に記載される
ような膜式脱気装置を用いることができる。The treated water of the oxidizing substance 14 is then passed through a deaerator 15. As the deaerator 15, a vacuum deaerator, a nitrogen deaerator or a membrane deaerator as described in JP-A-9-29251, which is used in the conventional primary pure water system 2, is used. Can be.
【００２４】膜式脱気装置としては、脱気膜の一方の側
に水を流し、他方の側を真空ポンプで排気し、溶存酸素
を膜を透過させて真空側に移行させて除去するようにし
たものが用いられる。なお、この膜の真空側には若干の
水分が脱気膜を透過して出てくるので、この真空側に窒
素等のガスを流し、水分を除去して膜性能の低下を防止
するのが好ましい。Ｎ２流量は一定でも良く、変動させ
ても良い。The membrane type deaerator is configured such that water flows on one side of the deaeration membrane and the other side is evacuated by a vacuum pump, and dissolved oxygen is permeated through the membrane and transferred to the vacuum side for removal. Is used. Since a small amount of moisture permeates through the degassing membrane on the vacuum side of this film, it is necessary to flow a gas such as nitrogen to the vacuum side to remove moisture and prevent the film performance from deteriorating. preferable. N 2 flow rate may be constant or may be varied.
【００２５】脱気膜は、酸素、窒素、蒸気等のガスは通
過するが水は透過しない膜であれば良く、例えば、シリ
コンゴム系、ポリテトラフルオロエチレン系、ポリオレ
フィン系、ポリウレタン系等がある。この脱気膜として
は市販の各種のものを用いることができる。The degassing film may be a film through which gases such as oxygen, nitrogen, steam, etc. pass but water does not permeate. Examples thereof include silicone rubber, polytetrafluoroethylene, polyolefin, and polyurethane. . Various commercially available deaeration membranes can be used.
【００２６】この膜式脱気装置の真空度は４０〜７０Ｔ
ｏｒｒ、Ｎ２等のガスの真空側流量は水流量の５〜２５
％とするのが好ましい。なお、この運転条件は、膜性能
により任意に設定できるが、通常上記のような範囲が好
ましい。真空度が過度に低いと脱気効率が低下し、逆に
過度に大きいと膜を通して水も透過側に出てきて効率が
悪くなる。Ｎ２流量は過度に少ないと水分除去が十分で
なく脱気効率が低下し、大きすぎると真空度が上がらず
脱気効率が低下する。The degree of vacuum of this membrane deaerator is 40 to 70 T
orr, vacuum side flow rate of gas such as N 2 is the water flow rate 5-25
% Is preferable. The operating conditions can be arbitrarily set depending on the membrane performance, but usually the above ranges are preferable. If the degree of vacuum is excessively low, the degassing efficiency is reduced. Conversely, if the degree of vacuum is excessively large, water also comes out to the permeate side through the membrane and the efficiency is reduced. If the N 2 flow rate is excessively small, moisture removal is not sufficient and the deaeration efficiency is reduced. If the N 2 flow rate is too large, the degree of vacuum is not increased and the deaeration efficiency is reduced.
【００２７】この脱気装置１５により、水中のＤＯやＣ
Ｏ２が効率的に除去される。The deaerator 15 allows DO and C in water to be removed.
O 2 is efficiently removed.
【００２８】脱気装置１５の処理水は次いで混床式イオ
ン交換装置１６に通水される。混床式イオン交換装置１
６としては、アニオン交換樹脂とカチオン交換樹脂とを
イオン負荷に応じて混合充填した非再生型混床式イオン
交換装置を用いるのが好ましく、この混床式イオン交換
装置１６により、水中のカチオン及びアニオンが除去さ
れ、水の純度が高められる。The treated water from the deaerator 15 is then passed through a mixed bed type ion exchanger 16. Mixed bed type ion exchanger 1
As 6, it is preferable to use a non-regenerative mixed bed type ion exchange apparatus in which an anion exchange resin and a cation exchange resin are mixed and filled according to the ion load. Anions are removed and water purity is increased.
【００２９】混床式イオン交換装置１６の処理水は次い
で微粒子分離膜装置１７に通水される。微粒子分離膜装
置１７としては、通常の超純水製造装置に用いられるＵ
Ｆ膜分離装置等を用いることができ、この微粒子分離膜
装置１７で水中の微粒子、例えば混床式イオン交換装置
１６からのイオン交換樹脂の流出微粒子等が除去され、
これにより、ＴＯＣ、ＣＯ２、ＤＯ、Ｈ２Ｏ２、イオン
性物質及び微粒子が高度に除去された高純度の超純水が
得られる。The treated water of the mixed bed type ion exchange device 16 is then passed through a fine particle separation membrane device 17. As the fine particle separation membrane device 17, U
An F membrane separation device or the like can be used, and fine particles in water, for example, fine particles of an ion exchange resin flowing out of a mixed bed type ion exchange device 16 are removed by the fine particle separation membrane device 17,
Thereby, high-purity ultrapure water from which TOC, CO 2 , DO, H 2 O 2 , ionic substances, and fine particles are highly removed is obtained.
【００３０】図１の構成は本発明の超純水製造装置の一
例であり、本発明の超純水製造装置は、従来の装置と同
様に前処理システム、一次純水システム、サブシステム
から構成され、その一連の構成単位装置のうちのサブシ
ステムにおいて、ＵＶ酸化装置、触媒式酸化性物質分解
装置、脱気装置、混床式イオン交換装置及び微粒子分離
膜装置をこの順で備えている限り、各種の機器を組み合
わせることができる。例えば、混床式イオン交換装置の
後にＲＯ膜分離装置を設置しても良い。また、原水をｐ
Ｈ４．５以下の酸性下、かつ、酸化剤存在下で加熱分解
処理して原水中の尿素及び他のＴＯＣ成分を分解した
後、脱イオン処理する装置を組み込むこともできる。Ｕ
Ｖ酸化装置や混床式イオン交換装置、脱気装置等は多段
に設置されても良い。また、前処理システム１や一次純
水システム２についても、何ら図３に示すものに限定さ
れるものではなく、他の様々な装置の組み合せを採用し
得る。The configuration shown in FIG. 1 is an example of the ultrapure water production apparatus of the present invention. The ultrapure water production apparatus of the present invention comprises a pretreatment system, a primary pure water system, and subsystems as in the conventional apparatus. As long as the subsystem of the series of constituent unit devices includes a UV oxidizing device, a catalytic oxidizing substance decomposing device, a degassing device, a mixed-bed ion exchange device and a fine particle separation membrane device in this order, , Various devices can be combined. For example, an RO membrane separation device may be installed after the mixed bed type ion exchange device. In addition, raw water
It is also possible to incorporate a device for deionizing after decomposing urea and other TOC components in raw water by heat decomposition treatment under an acid of H4.5 or less and in the presence of an oxidizing agent. U
A V oxidation device, a mixed-bed ion exchange device, a degassing device, and the like may be provided in multiple stages. Further, the pretreatment system 1 and the primary pure water system 2 are not limited to those shown in FIG. 3 at all, and combinations of other various devices can be adopted.
【００３１】[0031]
【実施例】以下に比較例及び実施例を挙げて本発明をよ
り具体的に説明する。The present invention will be described more specifically with reference to comparative examples and examples.
【００３２】実施例１ 水道水（野木町水）を原水として、図１の装置により超
純水を製造した。Example 1 Ultrapure water was produced by using the apparatus shown in FIG. 1 using tap water (Nogimachi water) as raw water.
【００３３】まず、原水を活性炭塔、ＵＦ膜分離装置、
２段ＲＯ膜分離装置、膜式脱気装置及び混床式イオン交
換装置に順次通水して一次純水を得、この一次純水を６
ｍ３／ｈｒの流量で図１に示すサブシステム３に通水し
て超純水を製造した。サブシステム３に用いた各装置の
仕様は次の通りである。 ＵＶ酸化装置（日本フォトサイエンス社製低圧ＵＶ酸化
装置（波長１８５ｎｍ付近、０．３２ｋＷ・ｈｒ／
ｍ３）） 触媒式酸化性物質分解装置（二酸チタンを担体としたパ
ラジウム触媒充填塔） 脱気装置（ヘキスト社製Ｌｉｑｕｉ−Ｃｅｌを充填した
膜式脱気装置） 混床式イオン交換装置（非再生型混床式イオン交換装
置） 微粒子分離膜装置（栗田工業（株）製ＵＦ膜分離装置
「ＫＵ−１５１０」）First, raw water is converted into an activated carbon tower, a UF membrane separation device,
Water is sequentially passed through a two-stage RO membrane separator, a membrane deaerator, and a mixed-bed ion exchanger to obtain primary pure water.
Ultrapure water was produced by passing water through the subsystem 3 shown in FIG. 1 at a flow rate of m 3 / hr. The specifications of each device used in the subsystem 3 are as follows. UV oxidizer (Low pressure UV oxidizer manufactured by Nippon Photo Science Co., Ltd. (wavelength around 185 nm, 0.32 kW · hr /
m 3 )) Catalytic oxidizing substance decomposer (palladium catalyst packed column using titanium dioxide as a carrier) Deaerator (membrane deaerator filled with Hoquist's Liqui-Cel) Mixed bed ion exchanger ( Non-regenerative mixed-bed ion exchange device) Particle separation membrane device (KU-1510 manufactured by Kurita Water Industries Ltd.)
【００３４】なお、触媒式酸化性物質分解装置の通水Ｓ
Ｖは８００ｈｒ−１とし、膜脱気装置の真空度は５０Ｔ
ｏｒｒ、Ｎ２流量は０．９Ｎｍ３／ｈｒとした。また、
混床式イオン交換装置の通水ＳＶは８０ｈｒ−１とし
た。The water flow S of the catalytic oxidizing substance decomposition apparatus
V is 800 hr -1 and the degree of vacuum of the membrane deaerator is 50 T
The flow rate of orr and N 2 was 0.9 Nm 3 / hr. Also,
The flow SV of the mixed bed type ion exchange device was set to 80 hr -1 .
【００３５】この処理において、ＵＶ酸化装置の入口水
及び出口水と得られた超純水（ＵＦ膜分離装置の出口
水）の水質は表１に示す通りであった。In this treatment, the water qualities of the inlet water and outlet water of the UV oxidation apparatus and the obtained ultrapure water (outlet water of the UF membrane separator) were as shown in Table 1.
【００３６】比較例１ 実施例１において図２に示す如く、触媒式酸化性物質分
解装置１４の代りにアニオン交換塔１９を設け、ＵＶ酸
化装置１３の出口水をアニオン交換塔１９にＳＶ５０ｈ
ｒ−１で通水した後、脱気装置１５、混床式イオン交換
装置１６、微粒子分離膜装置１７に順次通水したこと以
外は同様に処理を行ったところ、得られた超純水の水質
は表１に示す通りであった。COMPARATIVE EXAMPLE 1 In Example 1, as shown in FIG. 2, an anion exchange column 19 was provided in place of the catalytic oxidizing substance decomposer 14, and the outlet water of the UV oxidizer 13 was supplied to the anion exchange column 19 by the SV 50 h.
After passing water at r- 1 , the same treatment was performed except that water was sequentially passed through the deaerator 15, the mixed bed type ion exchange device 16, and the fine particle separation membrane device 17, and the resulting ultrapure water was obtained. The water quality was as shown in Table 1.
【００３７】[0037]
【表１】 [Table 1]
【００３８】表１より次のことが明らかである。The following is clear from Table 1.
【００３９】即ち、比較例１では、ＵＶ酸化装置１３の
処理水をアニオン交換塔１９に通水してＨ２Ｏ２を分解
除去し、次いで脱気装置１５で脱気処理するため、Ｈ２
Ｏ２及びＤＯを低減することができるが、Ｈ２Ｏ２等の
酸化性物質とアニオン交換樹脂との反応で樹脂から溶出
するＴＯＣのために、得られる超純水のＴＯＣは十分低
減できない。[0039] That is, in Comparative Example 1, since by passed therethrough treated water UV oxidation apparatus 13 to the anion exchange column 19 H 2 O 2 was decomposed and removed, followed by degassing treatment in the deaerator 15, H 2
Although O 2 and DO can be reduced, the TOC eluted from the resin due to the reaction between the oxidizing substance such as H 2 O 2 and the anion exchange resin cannot be sufficiently reduced due to the TOC eluted from the resin.
【００４０】これに対して、実施例１では、触媒式酸化
性物質分解装置１４でＨ２Ｏ２等の酸化性物質を除去
し、この酸化性物質の除去に当たりＴＯＣの溶出の問題
がないため、Ｈ２Ｏ２、ＤＯ、ＴＯＣがいずれも極低濃
度にまで低減された超純水を得ることができる。特に、
ＴＯＣは比較例１に比べ著しく低減されており、また、
触媒式酸化性物質分解装置で酸素の生成が殆どないた
め、ＤＯも比較例１に比べ一層低減されている。On the other hand, in Example 1, the oxidizing substance such as H 2 O 2 was removed by the catalytic oxidizing substance decomposer 14, and there was no problem of elution of TOC in removing the oxidizing substance. , H 2 O 2 , DO, and TOC can all be obtained to ultra-pure water in which the concentration is reduced to an extremely low concentration. In particular,
TOC is significantly reduced as compared with Comparative Example 1, and
Since almost no oxygen is generated in the catalytic oxidizing substance decomposing apparatus, DO is further reduced as compared with Comparative Example 1.
【００４１】[0041]
【発明の効果】以上詳述した通り、本発明の超純水製造
装置によれば、ＤＯ、ＴＯＣ、Ｈ２Ｏ ２等の酸化性物質
濃度が著しく低い高純度超純水を製造することができ
る。As described in detail above, the production of ultrapure water of the present invention
According to the device, DO, TOC, H2O 2Oxidizing substances such as
High purity ultrapure water with extremely low concentration can be produced.
You.
【図１】本発明の超純水製造装置の実施の形態を示す系
統図である。FIG. 1 is a system diagram showing an embodiment of an ultrapure water production apparatus according to the present invention.
【図２】比較例１の超純水製造装置を示す系統図であ
る。FIG. 2 is a system diagram showing an ultrapure water production apparatus of Comparative Example 1.
【図３】従来の超純水製造装置を示す系統図である。FIG. 3 is a system diagram showing a conventional ultrapure water production apparatus.
１ 前処理システム ２ 一次純水システム ３ サブシステム １１ サブタンク １２ 熱交換器 １３ ＵＶ酸化装置 １４ 触媒式酸化性物質分解装置 １５ 脱気装置 １６ 混床式イオン交換装置 １７ 微粒子分離膜装置 １８ ユースポイント １９ アニオン交換塔 Reference Signs List 1 Pretreatment system 2 Primary pure water system 3 Subsystem 11 Subtank 12 Heat exchanger 13 UV oxidizer 14 Catalytic oxidizing substance decomposer 15 Deaerator 16 Mixed-bed ion exchanger 17 Fine particle separation membrane device 18 Use point 19 Anion exchange tower
─────────────────────────────────────────────────────
────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成１３年１月２４日（２００１．１．２
４）[Submission Date] January 24, 2001 (2001.1.2)
4)
【手続補正１】[Procedure amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１６[Correction target item name] 0016
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００１６】この超純水製造装置では、各種前処理工程
より得られた一次純水（通常の場合、ＴＯＣ濃度２ｐｐ
ｂ以上の純水）をサブタンク１１、ポンプＰ、熱交換器
１２、ＵＶ酸化装置１３、触媒式酸化性物質分解装置１
４、脱気装置１５、混床式イオン交換装置１６及び微粒
子分離膜装置１７に順次に通水し、得られた超純水をユ
ースポイント１８に送る。In this ultrapure water producing apparatus, primary pure water obtained from various pretreatment steps (usually, a TOC concentration of 2 pp
b pure water or more) sub-tank 11, the pump P, the heat exchanger 12, UV oxidation apparatus 13, catalytic oxidizing material decomposition apparatus 1
4. Water is sequentially passed through the deaerator 15, the mixed bed type ion exchange device 16 and the fine particle separation membrane device 17, and the obtained ultrapure water is sent to the use point 18.
【手続補正書】[Procedure amendment]
【提出日】平成１３年１月２５日（２００１．１．２
５）[Submission date] January 25, 2001 (2001.1.2)
5)
【手続補正１】[Procedure amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１６[Correction target item name] 0016
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００１６】この超純水製造装置では、各種前処理工程
より得られた一次純水（通常の場合、ＴＯＣ濃度２ｐｐ
ｂ以上の純水）をサブタンク１１、ポンプＰ、熱交換器
１２、ＵＶ酸化装置１３、触媒式酸化性物質分解装置１
４、脱気装置１５、混床式イオン交換装置１６及び微粒
子分離膜装置１７に順次に通水し、得られた超純水をユ
ースポイント１８に送る。In this ultrapure water producing apparatus, primary pure water obtained from various pretreatment steps (usually, a TOC concentration of 2 pp
b pure water or more) sub-tank 11, the pump P, the heat exchanger 12, UV oxidation apparatus 13, catalytic oxidizing material decomposition apparatus 1
4. Water is sequentially passed through the deaerator 15, the mixed bed type ion exchange device 16 and the fine particle separation membrane device 17, and the obtained ultrapure water is sent to the use point 18.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ０２Ｆ 9/00 ５０２ Ｃ０２Ｆ 9/00 ５０２Ｚ ５０４ ５０４Ｂ ５０４Ｅ Ｂ０１Ｄ 19/00 Ｂ０１Ｄ 19/00 Ｈ Ｃ０２Ｆ 1/20 Ｃ０２Ｆ 1/20 Ａ 1/32 1/32 1/42 1/42 Ａ 1/44 1/44 Ｊ 1/72 １０１ 1/72 １０１ Ｆターム(参考） 4D006 GA06 GA41 KA01 KB04 KB11 KB12 KB17 MC22 MC30 MC53 MC65 PB06 PB62 PB63 PB65 PC02 4D011 AA17 4D025 AA04 BA08 BA13 BA22 BB04 DA01 DA03 DA04 DA10 4D037 AA03 BA18 BA23 CA01 CA03 CA11 CA15 4D050 AA05 BC09 BD06 CA03 CA06 CA08 CA09 ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification code FI Theme coat ゛ (Reference) C02F 9/00 502 C02F 9/00 502Z 504 504B 504E B01D 19/00 B01D 19/00 H C02F 1/20 C02F 1/20 A 1/32 1/32 1/42 1/42 A 1/44 1/44 J 1/72 101 1/72 101 F term (reference) 4D006 GA06 GA41 KA01 KB04 KB11 KB12 KB17 MC22 MC30 MC53 MC65 PB06 PB62 PB63 PB65 PC02 4D011 AA17 4D025 AA04 BA08 BA13 BA22 BB04 DA01 DA03 DA04 DA10 4D037 AA03 BA18 BA23 CA01 CA03 CA11 CA15 4D050 AA05 BC09 BD06 CA03 CA06 CA08 CA09
Claims (1)
照射する紫外線酸化装置と、 触媒式酸化性物質分解装置と、 脱気装置と、 混床式イオン交換装置と、 微粒子分離膜装置とを有し、この順に通水可能とした超
純水製造装置。1. An apparatus for irradiating an ultraviolet ray having a wavelength of about 185 nm with an ultraviolet ray, a catalytic oxidizing substance decomposing apparatus, a degassing apparatus, a mixed bed type ion exchange apparatus, and a fine particle separation membrane apparatus. , An ultrapure water production system that allows water to flow in this order.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001010433A JP4552327B2 (en) | 2001-01-18 | 2001-01-18 | Ultrapure water production equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001010433A JP4552327B2 (en) | 2001-01-18 | 2001-01-18 | Ultrapure water production equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2002210494A true JP2002210494A (en) | 2002-07-30 |
| JP4552327B2 JP4552327B2 (en) | 2010-09-29 |
Family
ID=18877745
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001010433A Expired - Lifetime JP4552327B2 (en) | 2001-01-18 | 2001-01-18 | Ultrapure water production equipment |
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| Country | Link |
|---|---|
| JP (1) | JP4552327B2 (en) |
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| JP2004181369A (en) * | 2002-12-03 | 2004-07-02 | Nomura Micro Sci Co Ltd | Ultrapure water making apparatus |
| WO2005095280A1 (en) * | 2004-03-31 | 2005-10-13 | Kurita Water Industries Ltd. | Apparatus for producing ultrapure water |
| JP2008119658A (en) * | 2006-11-15 | 2008-05-29 | Kurita Water Ind Ltd | Ultraviolet oxidation apparatus and organic matter removal apparatus |
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| JP2010069460A (en) * | 2008-09-22 | 2010-04-02 | Japan Organo Co Ltd | Method for reducing hydrogen peroxide, device for reducing the same, device for manufacturing ultrapure water and cleaning method |
| JP2011167633A (en) * | 2010-02-18 | 2011-09-01 | Kurita Water Ind Ltd | Water treatment method and apparatus |
| JP2011183245A (en) * | 2010-03-04 | 2011-09-22 | Kurita Water Ind Ltd | Method and apparatus for producing ultrapure water |
| JP2011218248A (en) * | 2010-04-05 | 2011-11-04 | Japan Organo Co Ltd | Pure water production method and device |
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| US20180044205A1 (en) * | 2015-02-23 | 2018-02-15 | Kurita Water Industries Ltd. | Device for removing microparticles contained in water and ultrapure-water prouction and supply system |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0217994A (en) * | 1988-07-07 | 1990-01-22 | Toshiba Corp | Ultrapure water producer |
| JPH0818040B2 (en) * | 1991-05-17 | 1996-02-28 | 株式会社荏原総合研究所 | Purification method and device for pure water or ultrapure water |
| JP2500968B2 (en) * | 1991-11-20 | 1996-05-29 | 栗田工業株式会社 | Pure water production equipment |
| JPH1177091A (en) * | 1997-09-03 | 1999-03-23 | Japan Organo Co Ltd | Ultrapure water making apparatus |
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2001
- 2001-01-18 JP JP2001010433A patent/JP4552327B2/en not_active Expired - Lifetime
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004181369A (en) * | 2002-12-03 | 2004-07-02 | Nomura Micro Sci Co Ltd | Ultrapure water making apparatus |
| JP2011194402A (en) * | 2004-03-31 | 2011-10-06 | Kurita Water Ind Ltd | Ultrapure water production plant |
| WO2005095280A1 (en) * | 2004-03-31 | 2005-10-13 | Kurita Water Industries Ltd. | Apparatus for producing ultrapure water |
| JPWO2005095280A1 (en) * | 2004-03-31 | 2008-02-21 | 栗田工業株式会社 | Ultrapure water production equipment |
| JP5045099B2 (en) * | 2004-03-31 | 2012-10-10 | 栗田工業株式会社 | Ultrapure water production apparatus and operation method of ultrapure water production apparatus |
| JP2008119658A (en) * | 2006-11-15 | 2008-05-29 | Kurita Water Ind Ltd | Ultraviolet oxidation apparatus and organic matter removal apparatus |
| JP2009112944A (en) * | 2007-11-06 | 2009-05-28 | Kurita Water Ind Ltd | Ultrapure water production method and apparatus, and washing method and apparatus for electronic component members |
| JP2010069460A (en) * | 2008-09-22 | 2010-04-02 | Japan Organo Co Ltd | Method for reducing hydrogen peroxide, device for reducing the same, device for manufacturing ultrapure water and cleaning method |
| JP2011167633A (en) * | 2010-02-18 | 2011-09-01 | Kurita Water Ind Ltd | Water treatment method and apparatus |
| JP2011183245A (en) * | 2010-03-04 | 2011-09-22 | Kurita Water Ind Ltd | Method and apparatus for producing ultrapure water |
| JP2011218248A (en) * | 2010-04-05 | 2011-11-04 | Japan Organo Co Ltd | Pure water production method and device |
| JP2011245380A (en) * | 2010-05-25 | 2011-12-08 | Japan Organo Co Ltd | Method and device for producing pure water |
| US20180044205A1 (en) * | 2015-02-23 | 2018-02-15 | Kurita Water Industries Ltd. | Device for removing microparticles contained in water and ultrapure-water prouction and supply system |
| KR20190089877A (en) * | 2016-12-05 | 2019-07-31 | 쿠리타 고교 가부시키가이샤 | Operation method of ultrapure water producing apparatus and ultrapure water producing apparatus |
| KR102497591B1 (en) * | 2016-12-05 | 2023-02-07 | 쿠리타 고교 가부시키가이샤 | Ultrapure water production device and operation method of ultrapure water production device |
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