JP2002096066A - Method of preparing washing water and washing water - Google Patents
Method of preparing washing water and washing waterInfo
- Publication number
- JP2002096066A JP2002096066A JP2000329666A JP2000329666A JP2002096066A JP 2002096066 A JP2002096066 A JP 2002096066A JP 2000329666 A JP2000329666 A JP 2000329666A JP 2000329666 A JP2000329666 A JP 2000329666A JP 2002096066 A JP2002096066 A JP 2002096066A
- Authority
- JP
- Japan
- Prior art keywords
- water
- mmol
- less
- washing water
- concentration
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/4618—Devices therefor; Their operating or servicing for producing "ionised" acidic or basic water
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、水を電気分解して
得られるアルカリ性の洗浄水の製造方法に関する。The present invention relates to a method for producing alkaline washing water obtained by electrolyzing water.
【０００２】[0002]
【従来の技術】脱脂洗浄にはこれまでフロン１１３や１
・１・１−トリクロロエタンに代表されるハロゲン化炭
化水素系洗浄液が大量に用いられてきたが、オゾン層破
壊や地下水、土壌汚染等の環境破壊が指摘され、多くの
物質が使用禁止となっている。これらに変わる代替洗浄
方法の技術開発が進められ、各種の洗浄方法が提案され
ているが、それぞれに問題を含んでいるのが現状であ
る。2. Description of the Related Art For degreasing cleaning, CFC 113 or 1 has been used.
・ Halogenated hydrocarbon-based cleaning liquids such as 1.1-trichloroethane have been used in large quantities, but environmental destruction such as ozone depletion, groundwater and soil pollution has been pointed out, and the use of many substances has been banned. I have. Technical development of alternative cleaning methods instead of these has been promoted, and various cleaning methods have been proposed, but each of them presents a problem.
【０００３】代替洗浄方法は水系、準水系、非水系に大
別できる。[0003] Alternative cleaning methods can be broadly classified into aqueous, semi-aqueous and non-aqueous.
【０００４】水系は、アルカリ洗剤、中性洗剤等を使用
する方法と、市水あるいは純水のみで洗浄する方法があ
る。しかし、どの水系洗浄方法でも金属、特に鉄鋼を洗
浄する場合は錆の発生が問題になることが多く、乾燥工
程で大量の熱エネルギーを必要となることや、防錆剤を
併用する必要があった。特に、洗剤を使用する方法では
リンス工程が必要となることや、洗剤の濃度管理が必要
となる。また、洗剤に含まれる界面活性剤には内分泌攪
乱作用を疑われる成分（アルキルフェノール、ノニルフ
ェノール等）を含んでいるか、分解によって生成される
危険性が報告されている。また、市水、純水のみの洗浄
では十分な洗浄効果が得られないことがある。[0004] The aqueous system includes a method using an alkaline detergent, a neutral detergent and the like, and a method using only city water or pure water. However, in the case of cleaning metals, particularly steel, with any of the water-based cleaning methods, the generation of rust is often a problem, and a large amount of heat energy is required in the drying process, and it is necessary to use a rust inhibitor in combination. Was. In particular, a method using a detergent requires a rinsing step and a concentration control of the detergent. In addition, it has been reported that surfactants contained in detergents contain components suspected of having an endocrine disrupting effect (such as alkylphenols and nonylphenols), or that they are formed by decomposition. Also, washing with city water and pure water alone may not provide a sufficient washing effect.
【０００５】準水系は、グリコールエーテルやアルコー
ル、エステル等を水と混合した洗浄液を用いるが、引火
の危険性がある。またリンス工程が必要であることや、
防錆についての配慮が必要なのは水系と類似している。[0005] The semi-aqueous system uses a cleaning solution in which glycol ether, alcohol, ester or the like is mixed with water, but there is a risk of ignition. In addition, the rinsing process is necessary,
It is similar to the water system that needs to be considered for rust prevention.
【０００６】非水系は、アルコールや炭化水素等の引火
性溶剤を使用するため、防爆対策が必要である。また、
溶剤の中には乾燥が遅いものもあり、乾燥設備を大型化
する必要がある。[0006] Since non-aqueous systems use flammable solvents such as alcohols and hydrocarbons, explosion-proof measures are required. Also,
Some of the solvents dry slowly, and it is necessary to increase the size of the drying equipment.
【０００７】こういった中で、特開平１０−１９２８６
０号で開示されているような、水を電気分解して得られ
るアルカリ性水を洗浄水として利用する技術が注目され
ている。この方式は、界面活性剤やアルカリ薬剤を使用
せず、一般の市水、工業用水等を原料に電気分解を行い
アルカリ性水とすることで、水の洗浄力を高めるもので
ある。水の安全性を損なうことなく、洗浄力を高められ
るため代替洗浄として有効である。また、アルカリ性イ
オン水は他の水洗浄方式と比較して、発錆を抑止する効
果も有する。しかし、これはすべての金属に長期的な効
果を示すものではなく、水洗浄である以上、防錆対策が
必要であることは他の水洗浄同じである。Under these circumstances, Japanese Patent Application Laid-Open No. 10-19286
No. 0, attention is being paid to a technique of using alkaline water obtained by electrolysis of water as washing water. In this method, the detergency of water is increased by electrolysis using general city water, industrial water or the like as a raw material without using a surfactant or an alkaline agent to make alkaline water. The cleaning power can be increased without impairing the safety of water, which is effective as an alternative cleaning. Further, the alkaline ionized water has an effect of suppressing rusting as compared with other water cleaning methods. However, this does not show a long-term effect on all metals, and since it is water washing, it is the same as other water washing that rust prevention measures are required.
【０００８】[0008]
【発明が解決しようとする課題】特開平９−１３７２８
７号では、電気分解によって得られたアルカリ性水を鉄
加工品の洗浄に用いる場合に、酸性イオン水で洗浄を行
ってからアルカリ性水で洗浄する方法が開示されてい
る。しかし、酸性イオン水は金属腐食性があるため、め
っき等の表面処理がされず鉄素地が露出した鉄鋼・鋳鉄
製品では、酸性イオン水で洗浄を行う段階で錆が発生す
るという問題がある。SUMMARY OF THE INVENTION Japanese Patent Application Laid-Open No. Hei 9-13728
No. 7 discloses a method in which, when alkaline water obtained by electrolysis is used for cleaning a processed iron product, the substrate is washed with acidic ion water and then with alkaline water. However, since acidic ionized water has a metal corrosive property, there is a problem that rust is generated in a step of washing with acidic ionized water in a steel or cast iron product in which a surface treatment such as plating is not performed and an iron base is exposed.
【０００９】また、市水や工業用水を電気分解すると、
その中に含まれるカルシウムイオンやマグネシウムイオ
ンが電気分解によってアルカリ性水側に移動し、これら
のイオン濃度が高くなる。このイオンの一部は炭酸化合
物として、水中のシリカ等と一緒に析出し、配管やバル
ブに付着するため、電解イオン水製造装置の配管内部を
定期的に酸性溶液等で洗浄する必要があった。Further, when city water or industrial water is electrolyzed,
Calcium ions and magnesium ions contained therein move to the alkaline water side by electrolysis, and the concentration of these ions increases. Some of these ions precipitate as carbonate compounds together with the silica in the water and adhere to the pipes and valves. Therefore, it was necessary to periodically wash the inside of the pipes of the electrolytic ionized water producing apparatus with an acidic solution or the like. .
【００１０】さらに、電気分解では陰極側からアルカリ
水が生成されると同時に、陽極側からほぼ同量の酸性水
が生成される。この酸性水は前述の通り金属腐食性があ
るため洗浄には不適であり、通常は排水されるが、ｐＨ
が２．５から５．５程度であるためアルカリ薬剤で中和
して排水する必要があった。Further, in the electrolysis, at the same time as the alkaline water is generated from the cathode side, almost the same amount of acidic water is generated from the anode side. As described above, this acidic water is not suitable for cleaning because of its metal corrosiveness, and is usually drained.
Was about 2.5 to 5.5, so it was necessary to neutralize it with an alkaline agent and drain it.
【００１１】一方、アルミニウムをアルカリ性水で洗浄
する場合、洗浄温度が高く、被洗浄物が洗浄水に接触し
ている時間が長いときにはアルミニウムの表面が、黒褐
色に変色することがあり、アルミニウムの洗浄には適さ
ないことがあった。On the other hand, when aluminum is washed with alkaline water, if the washing temperature is high and the object to be washed is in contact with the washing water for a long time, the surface of the aluminum may turn black-brown and the aluminum may be washed. Was not suitable for
【００１２】本発明は、従来の電気分解によるアルカリ
水よりも高い防錆効果が得られ、安全性と洗浄品質を両
立する洗浄水を提供することを目的としている。An object of the present invention is to provide washing water which has a higher rust prevention effect than conventional alkaline water obtained by electrolysis, and achieves both safety and washing quality.
【００１３】[0013]
【課題を解決するための手段】上記目的を達成するため
に、本発明の第１は、原水中のカルシウムイオン濃度を
１．０ｍｍｏｌ／ｄｍ３以下、及びマグネシウムイオン
濃度を１．０ｍｍｏｌ／ｄｍ３以下にする工程と、この
後に原水中の炭酸ナトリウム濃度を０．１〜１０．０ｍ
ｍｏｌ／ｄｍ３に調整する工程を有し、これを電気分解
してｐＨ値が８．０以上１３．０以下であり、及び／ま
たは、酸化還元電位が−１００ｍＶ〜−１０００ｍＶで
ある洗浄水を得ることを特徴とする洗浄水の製造方法で
ある。In order to achieve the above object, a first aspect of the present invention is to reduce the calcium ion concentration in raw water to 1.0 mmol / dm 3 or less and the magnesium ion concentration to 1.0 mmol / dm 3. And a sodium carbonate concentration in the raw water of 0.1 to 10.0 m
mol / dm 3 , which is electrolyzed to wash water having a pH value of 8.0 or more and 13.0 or less and / or an oxidation-reduction potential of −100 mV to −1000 mV. A method for producing washing water, characterized in that it is obtained.
【００１４】本発明の第２は、原水中の硫酸イオンを
０．２ｍｍｏｌ／ｄｍ３以下、及び／または塩化物イオ
ンを０．５ｍｍｏｌ／ｄｍ３以下、及びカルシウムイオ
ン濃度を１．０ｍｍｏｌ／ｄｍ３以下、及びマグネシウ
ムイオン濃度を１．０ｍｍｏｌ／ｄｍ３以下にする工程
を有し、この後に原水中の炭酸ナトリウム濃度を０．１
〜１０．０ｍｍｏｌ／ｄｍ３に調整する工程を有し、こ
れを電気分解してｐＨ値が８．０以上１３．０以下であ
り、及び／または、酸化還元電位が−１００ｍＶ〜−１
０００ｍＶである洗浄水を得ることを特徴とする洗浄水
の製造方法である。A second aspect of the present invention is that the sulfate ion in raw water is 0.2 mmol / dm 3 or less, and / or the chloride ion is 0.5 mmol / dm 3 or less, and the calcium ion concentration is 1.0 mmol / dm 3. And a step of reducing the magnesium ion concentration to 1.0 mmol / dm 3 or less.
Ｍｍｏｌ10.0 mmol / dm 3 , which is electrolyzed to have a pH value of 8.0 or more and 13.0 or less, and / or an oxidation-reduction potential of −100 mV to −1.
000 mV of cleaning water is obtained.
【００１５】本発明の第３は、上記記載の洗浄水の製造
方法において、製造した洗浄水に水酸化カルシウムを
０．０５ｍｍｏｌ／ｄｍ３〜２ｍｍｏｌ／ｄｍ３の範囲
で添加する工程を有することを特徴とする洗浄水の製造
方法である。According to a third aspect of the present invention, in the above-mentioned method for producing washing water, a step of adding calcium hydroxide to the produced washing water in a range of 0.05 mmol / dm 3 to 2 mmol / dm 3 is provided. This is a characteristic method for producing cleaning water.
【００１６】本発明の第４は、上記記載の洗浄水の製造
方法で製造したアルカリ性水中の溶存水素濃度が０．０
１ｍｇ／ｄｍ３以上であり、溶存酸素濃度が６ｍｇ／ｄ
ｍ３以下であることを特徴とする洗浄水である。A fourth aspect of the present invention is that the concentration of dissolved hydrogen in the alkaline water produced by the above-described method for producing washing water is 0.04% or less.
1 mg / dm 3 or more, and the dissolved oxygen concentration is 6 mg / d
a wash water, characterized in that m 3 or less.
【００１７】以下、本発明について更に詳細に説明す
る。 （第１の発明）電気分解によってアルカリ性水を生成し
洗浄水として用いる場合、電解槽や配管内部に白色のス
ケールが析出して流路を塞ぎ、アルカリ性水の生成量が
減少したり、電解槽を破損したりすることがある。これ
は、原水に含まれるカルシウムイオンやマグネシウムイ
オンが電気分解によってアルカリ性水側に移動し、アル
カリ性水中のカルシウム及びマグネシウムイオン濃度が
高くなり、これらのイオンが炭酸化合物として、水中の
シリカ等と一緒に析出するためである。カルシウムイオ
ン濃度が２．０ｍｍｏｌ／ｄｍ３の場合、電気分解を６
０〜８０時間行うと、配管内にスケールが付着し始め、
１００時間では内径１０ｍｍの配管を塞ぐようになる。Hereinafter, the present invention will be described in more detail. (First invention) When alkaline water is generated by electrolysis and used as washing water, a white scale is deposited in an electrolytic bath or a pipe to block a flow path, thereby reducing the amount of alkaline water generated or an electrolytic bath. May be damaged. This is because calcium ions and magnesium ions contained in the raw water move to the alkaline water side by electrolysis, the calcium and magnesium ion concentrations in the alkaline water increase, and these ions become carbonate compounds together with the silica etc. in the water. This is for precipitation. When the calcium ion concentration is 2.0 mmol / dm 3 ,
When it is performed for 0 to 80 hours, the scale starts to adhere to the piping,
In 100 hours, the pipe having an inner diameter of 10 mm is blocked.
【００１８】そこで、スケールの付着を防止するため、
本発明では電気分解を行う前の原水中のカルシウムイオ
ン濃度を１．０ｍｍｏｌ／ｄｍ３以下、及びマグネシウ
ムイオン濃度を１．０ｍｍｏｌ／ｄｍ３以下にすること
が有効であることを見出した。こうすることにより、電
解槽や配管内での炭酸カルシウムや炭酸マグネシウム等
のスケール化しやすい化合物の生成を防止することがで
きる。Therefore, in order to prevent adhesion of scale,
In the present invention, it has been found that it is effective to set the calcium ion concentration in the raw water before electrolysis to 1.0 mmol / dm 3 or less and the magnesium ion concentration to 1.0 mmol / dm 3 or less. By doing so, it is possible to prevent the formation of easily scalable compounds such as calcium carbonate and magnesium carbonate in the electrolytic cell and the piping.
【００１９】この効果は原水中のカルシウムイオン濃度
とマグネシウムイオン濃度の合計が１．５ｍｍｏｌ／ｄ
ｍ３以下で顕著になり、両イオン濃度がそれぞれ１．０
ｍｍｏｌ／ｄｍ３以下になると、２５０時間以上連続し
て電気分解を行ってもスケールの付着は生じない。The effect is that the sum of the calcium ion concentration and the magnesium ion concentration in the raw water is 1.5 mmol / d
m 3 or less, and both ion concentrations are 1.0
When it is less than 3 mmol / dm 3, no scale adheres even if electrolysis is performed continuously for 250 hours or more.
【００２０】また、アルカリ性水と同時に生成される酸
性水は金属の洗浄に使用すると錆が発生するため、排水
することになるが、ｐＨが低いと、中和して排水してい
る。しかし、本発明者らは、原水に炭酸ナトリウムを添
加し、その濃度を０．１〜１０．０ｍｍｏｌ／ｄｍ３に
調整してから電気分解を行うと、生成される酸性水のｐ
Ｈが５．８から６．５の範囲となり、排水のための中和
の必要が無くなることを見出した。The acidic water produced simultaneously with the alkaline water generates rust when used for washing metals, and is therefore drained. However, when the pH is low, it is neutralized and drained. However, the present inventors add sodium carbonate to raw water, adjust the concentration to 0.1 to 10.0 mmol / dm 3 , and then perform electrolysis.
H was found to be in the range of 5.8 to 6.5, and the need for neutralization for drainage was eliminated.
【００２１】特に、原水中のカルシウムイオンとマグネ
シウムイオン濃度をそれぞれ１．０ｍｍｏｌ／ｄｍ３以
下にしておくことで、添加した炭酸ナトリウムが炭酸塩
として析出することを防止できるため、少量の炭酸ナト
リウムの添加で効果が得られるようになる。In particular, by setting the concentration of calcium ion and magnesium ion in the raw water to 1.0 mmol / dm 3 or less, it is possible to prevent the added sodium carbonate from being precipitated as a carbonate. The effect can be obtained by the addition.
【００２２】このようにイオン成分を調整した原水を電
気分解して、ｐＨ値が８．０以上１３．０以下であり、
及び／または、酸化還元電位が−１００ｍＶ〜−１００
０ｍＶである洗浄水を得ることは従来の方法と比較し
て、装置のメンテナンスや排水処理において、その労力
が大幅に削減できる点で優れている。ただし、炭酸ナト
リウム濃度を１０．０ｍｍｏｌ／ｄｍ３以上にすると、
洗浄品に対する残留イオン成分が多くなり、精密洗浄に
は適さなくなる。The raw water having the ionic components adjusted as described above is electrolyzed to have a pH value of 8.0 or more and 13.0 or less,
And / or a redox potential of -100 mV to -100
Obtaining the cleaning water of 0 mV is superior to the conventional method in that the labor required for maintenance of the apparatus and wastewater treatment can be greatly reduced. However, when the sodium carbonate concentration is 10.0 mmol / dm 3 or more,
Residual ion components in the cleaned product increase, and are not suitable for precision cleaning.
【００２３】（第２の発明）また、原水中のカルシウム
イオンとマグネシウムイオンを低減する工程の前、ある
いは後において、硫酸イオンと塩化物イオンを減少させ
ておくと、得られるアルカリ性水の金属腐食性が大幅に
低減することがわかった。特に硫酸イオンを０．２ｍｍ
ｏｌ／ｄｍ３以下、及び／または塩化物イオンを０．５
ｍｍｏｌ／ｄｍ３以下にした原水を電気分解して得られ
たアルカリ性水と、硫酸イオンと塩化物イオンを低減せ
ずに生成したアルカリ性水とで鋼板を浸漬して錆が発生
するまでの時間を比較すると、イオンを低減した方が３
倍以上長く錆が発生しなかった。また、アルミニウムを
浸漬した場合、硫酸イオン及び／または塩化物イオンを
減少させたアルカリ性水では表面の変色は見られない
が、硫酸イオンと塩化物イオンを低減しなかった方では
表面が黒褐色に変色した。(Second invention) Further, if the sulfate ion and the chloride ion are reduced before or after the step of reducing the calcium ion and the magnesium ion in the raw water, the resulting metal corrosion of alkaline water can be obtained. It was found that the properties were greatly reduced. Especially 0.2mm for sulfate ion
ol / dm 3 or less, and / or 0.5
The time until rust is generated by immersing a steel sheet in alkaline water obtained by electrolyzing raw water having a concentration of 3 mmol / dm 3 or less and alkaline water generated without reducing sulfate ions and chloride ions. By comparison, the ion reduction is 3
Rust did not occur more than twice as long. In addition, when aluminum is immersed, no discoloration of the surface is observed in alkaline water in which sulfate ions and / or chloride ions have been reduced, but the surface discolors blackish brown in those who did not reduce sulfate ions and chloride ions. did.
【００２４】原水中に存在する硫酸イオンや塩化物イオ
ンは、電気分解によって酸性水の方に濃縮するが、一部
はアルカリ性水にも残留する。これらアルカリ性水に含
まれる硫酸イオンや塩化物イオンは、金属表面で局部電
池を形成する際にその腐食を早める傾向が強いために、
これらが多く存在すると発錆しやすくなる。Sulfate ions and chloride ions present in the raw water are concentrated toward the acidic water by electrolysis, but partly remain in the alkaline water. Sulfate ions and chloride ions contained in these alkaline waters have a strong tendency to accelerate the corrosion when forming a local battery on the metal surface,
If these are present in a large amount, rust is likely to occur.
【００２５】このため、あらかじめ原水に含まれる硫酸
イオンや塩化物イオンを低減しておくことは、生成した
アルカリ性水の防錆性を向上する効果がある。For this reason, reducing the sulfate ions and chloride ions contained in the raw water in advance has the effect of improving the rust prevention of the generated alkaline water.
【００２６】（第３の発明）また、このアルカリ性水に
水酸化カルシウムを０．０５ｍｍｏｌ／ｄｍ３〜２ｍｍ
ｏｌ／ｄｍ３の範囲で添加すると、更にアルカリ性水の
防錆性を高めることができる。これは、添加した水酸化
カルシウムのカルシウムイオンがアルカリ性水中の炭酸
水素イオンと結合して炭酸水素カルシウム（Ｃａ（ＨＣ
Ｏ３））を形成し、これがカソードインヒビター的な働
きを示して、金属表面のカソード部分に不溶性皮膜を生
成し、カソード反応の起こる面積を減少させるため、防
錆効果が生じると考えられる。(Third invention) Calcium hydroxide is added to the alkaline water in an amount of 0.05 mmol / dm 3 to 2 mm.
When added in the range of ol / dm 3, the rust prevention of alkaline water can be further enhanced. This is because the calcium ions of the added calcium hydroxide combine with the hydrogen carbonate ions in the alkaline water to form calcium hydrogen carbonate (Ca (HC
O 3 )) is formed, which acts as a cathode inhibitor, generates an insoluble film on the cathode portion of the metal surface, and reduces the area where the cathodic reaction occurs.
【００２７】更に、第１の発明で炭酸ナトリウムを添加
した場合、これに含まれる炭酸イオンは水中で炭酸水素
イオンと平衡状態にあるため、上記の炭酸水素カルシウ
ムの形成に役立つ。Further, when sodium carbonate is added in the first invention, the carbonate ions contained therein are in equilibrium with the hydrogen carbonate ions in water, and thus contribute to the formation of the above-mentioned calcium hydrogen carbonate.
【００２８】ここで添加する水酸化カルシウムの添加量
は、０．０５ｍｍｏｌより少ないと炭酸水素カルシウム
の形成が不十分となり防錆効果が得られず、また、２ｍ
ｍｏｌ／ｄｍ３以上になると、炭酸カルシウムが析出物
として洗浄水中に浮遊し、これが被洗浄物を汚染するこ
とになってしまう。If the amount of calcium hydroxide added is less than 0.05 mmol, the formation of calcium bicarbonate becomes insufficient, so that no rust-preventive effect can be obtained.
If it is at least 3 mol / dm3, calcium carbonate will float in the washing water as a precipitate, and this will contaminate the object to be washed.
【００２９】（第４の発明）電解槽においてアルカリ性
水が生成される陰極では、電極表面で水素過電圧を超え
た場合、水素ガスが発生する。水素ガスが発生すると陰
極室中での水素分圧が上昇し、相対的に酸素分圧が減少
する。すると、ヘンリーの法則によって溶存酸素濃度が
低下することになる。溶存酸素は金属表面を酸化させる
作用が強く、特にその濃度が０から１５ｍｇ／ｄｍ３の
範囲では腐食速度は濃度に比例的に増加する。すなわ
ち、陰極における水素発生によって溶存酸素濃度を低下
させることで、アルカリ性水の防錆性を向上することが
可能であり、本発明においては溶存水素濃度を０．０１
ｍｇ／ｄｍ３以上とし、溶存酸素濃度を６ｍｇ／ｄｍ３
以下としたアルカリ性水の防錆効果が著しく高いことを
見出した。(Fourth Invention) In a cathode where alkaline water is generated in an electrolytic cell, hydrogen gas is generated when a hydrogen overvoltage is exceeded on the electrode surface. When hydrogen gas is generated, the partial pressure of hydrogen in the cathode chamber increases, and the partial pressure of oxygen relatively decreases. Then, the dissolved oxygen concentration is reduced according to Henry's law. The dissolved oxygen has a strong effect of oxidizing the metal surface, and particularly when the concentration is in the range of 0 to 15 mg / dm 3 , the corrosion rate increases in proportion to the concentration. That is, by reducing the dissolved oxygen concentration by generating hydrogen at the cathode, it is possible to improve the rust prevention of alkaline water, and in the present invention, the dissolved hydrogen concentration is reduced to 0.01.
mg / dm 3 or more, and the dissolved oxygen concentration is 6 mg / dm 3
It has been found that the rust-preventing effect of the following alkaline water is extremely high.
【００３０】[0030]
【発明の実施の形態】発明の第１の実施形態を以下に説
明する。ここで使用する実施例１のアルカリ性水は次の
ようにして生成した。原水に水道水（滋賀県東浅井郡び
わ町、硬度６０ｐｐｍ）を用い、これを軟水装置（日本
錬水（株）製ＭＥ−５Ｓ型、使用イオン交換樹脂：スチ
レン系強酸性陽イオン交換樹脂（ナトリウム形））に通
水してカルシウムイオン濃度、及びマグネシウムイオン
濃度を０．００５ｍｍｏｌ／ｄｍ３以下とした。これに
炭酸ナトリウムを添加して炭酸ナトリウム濃度を２．０
ｍｍｏｌ／ｄｍ３とした。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A first embodiment of the present invention will be described below. The alkaline water of Example 1 used here was produced as follows. Tap water is used as raw water (hardness 60 ppm, Biwa-cho, Higashi-Asai-gun, Shiga Prefecture), which is used as a water softener (ME-5S type manufactured by Nippon Rensui Co., Ltd., ion exchange resin used: styrene-based strongly acidic cation exchange resin ( (Sodium form)) to make the calcium ion concentration and the magnesium ion concentration 0.005 mmol / dm 3 or less. Sodium carbonate was added to the mixture to adjust the sodium carbonate concentration to 2.0.
mmol / dm 3 .
【００３１】上記の水を有隔膜電解槽にて電気分解を行
い、アルカリ性水を得てこれを洗浄水とした。電気分解
の条件は印加電圧ＤＣ６０Ｖ、電流密度１．０Ａ／ｄｍ
２、生成量２Ｌ／分である。The water was electrolyzed in a diaphragm electrolyzer to obtain alkaline water, which was used as washing water. Electrolysis conditions were applied voltage DC60V, current density 1.0A / dm.
2. The production amount is 2 L / min.
【００３２】実施例２のアルカリ性水は、原水に水道水
（滋賀県東浅井郡びわ町、硬度６０ｐｐｍ）を用い、こ
れをイオン交換樹脂式純水装置（日本錬水（株）製Ｃ−
２０Ｓ型）に通水してカルシウムイオン濃度、マグネシ
ウムイオン濃度、硫酸イオン濃度、塩素イオン濃度を総
て０．００５ｍｍｏｌ／ｄｍ３以下とした。これに炭酸
ナトリウムを添加して炭酸ナトリウム濃度を２．０ｍｍ
ｏｌ／ｄｍ３とした。これを実施例１と同じ条件で電気
分解を行い、アルカリ性水を得て洗浄水とした。The alkaline water used in Example 2 was tap water (hardness 60 ppm, Biwa-cho, Higashi-Asai-gun, Shiga Prefecture) as raw water, and this was used as an ion-exchange resin-type pure water apparatus (C-Nippon Rensui KK).
(20S type) so that the calcium ion concentration, the magnesium ion concentration, the sulfate ion concentration, and the chloride ion concentration were all 0.005 mmol / dm 3 or less. Sodium carbonate was added to this and the sodium carbonate concentration was 2.0 mm
was ol / dm 3. This was electrolyzed under the same conditions as in Example 1 to obtain alkaline water, which was used as washing water.
【００３３】実施例３−１のアルカリ性水は、実施例１
で得たアルカリ性水に水酸化カルシウムを１．０ｍｍｏ
ｌ／ｄｍ３添加して洗浄水とした。The alkaline water of Example 3-1 was prepared in the same manner as in Example 1
Calcium hydroxide in the alkaline water obtained in 1.0mmo
1 / dm 3 was added to prepare washing water.
【００３４】実施例３−２のアルカリ性水は、実施例２
で得たアルカリ性水に水酸化カルシウムを１．０ｍｍｏ
ｌ／ｄｍ３添加して洗浄水とした。The alkaline water of Example 3-2 was used in Example 2.
Calcium hydroxide in the alkaline water obtained in 1.0mmo
1 / dm 3 was added to prepare washing water.
【００３５】また、比較のため、比較例１、２−１、２
−２、２−３、３−１、３−２、３−３、３−４のアル
カリ性水を生成した。For comparison, Comparative Examples 1, 2-1, and 2
-2, 2-3, 3-1, 3-2, 3-3, 3-4 alkaline water was produced.
【００３６】比較例１のアルカリ性水は、実施例１の中
の軟水装置に通水する工程を省略し、原水中のカルシウ
ムイオン濃度とマグネシウムイオン濃度を調整せずに電
気分解したものである。The alkaline water of Comparative Example 1 was obtained by electrolyzing the raw water without adjusting the calcium ion concentration and the magnesium ion concentration in the raw water, omitting the step of passing through the water softener in Example 1.
【００３７】比較例２−１のアルカリ性水は、実施例１
で炭酸ナトリウムを添加したところを塩化ナトリウムの
添加に変更して電気分解したものである。塩化ナトリウ
ムの添加量は原水中の塩化ナトリウム濃度が４．０ｍｍ
ｏｌ／ｄｍ３になるようにした。これはナトリウムイオ
ン濃度が炭酸ナトリウムの場合と同じになるようにする
ためである。The alkaline water of Comparative Example 2-1 was obtained in Example 1.
In the above, the place where sodium carbonate was added was changed to the addition of sodium chloride and electrolysis was performed. The amount of sodium chloride added was such that the concentration of sodium chloride in the raw water was 4.0 mm.
It was set to ol / dm 3. This is to make the sodium ion concentration the same as in the case of sodium carbonate.
【００３８】比較例２−２のアルカリ性水は、実施例１
の炭酸ナトリウム濃度を０．０５ｍｍｏｌ／ｄｍ３とし
て電気分解を行い、アルカリ性水を得て洗浄水とした。The alkaline water of Comparative Example 2-2 was obtained in Example 1.
Was electrolyzed at a sodium carbonate concentration of 0.05 mmol / dm 3 to obtain alkaline water, which was used as washing water.
【００３９】比較例２−３のアルカリ性水は、実施例１
の炭酸ナトリウム濃度を１５．０ｍｍｏｌ／ｄｍ３とし
て電気分解を行い、アルカリ性水を得て洗浄水とした。The alkaline water of Comparative Example 2-3 was prepared in Example 1.
Was electrolyzed at a sodium carbonate concentration of 15.0 mmol / dm 3 to obtain alkaline water, which was used as washing water.
【００４０】比較例３−１のアルカリ性水は、実施例１
で得たアルカリ性水に水酸化カルシウムを０．０３ｍｍ
ｏｌ／ｄｍ３添加して洗浄水とした。The alkaline water of Comparative Example 3-1 was obtained in Example 1.
0.03 mm of calcium hydroxide in the alkaline water obtained in
ol / dm 3 was added to prepare washing water.
【００４１】比較例３−２のアルカリ性水は、実施例１
で得たアルカリ性水に水酸化カルシウムを３．０ｍｍｏ
ｌ／ｄｍ３添加して洗浄水とした。The alkaline water of Comparative Example 3-2 was prepared in Example 1.
3.0 mmol of calcium hydroxide in the alkaline water obtained in
1 / dm 3 was added to prepare washing water.
【００４２】比較例３−３のアルカリ性水は、実施例２
で得たアルカリ性水に水酸化カルシウムを０．０３ｍｍ
ｏｌ／ｄｍ３添加して洗浄水とした。The alkaline water of Comparative Example 3-3 was used in Example 2.
0.03 mm of calcium hydroxide in the alkaline water obtained in
ol / dm 3 was added to prepare washing water.
【００４３】比較例３−４のアルカリ性水は、実施例２
で得たアルカリ性水に水酸化カルシウムを３．０ｍｍｏ
ｌ／ｄｍ３添加して洗浄水とした。The alkaline water of Comparative Example 3-4 was used in Example 2.
3.0 mmol of calcium hydroxide in the alkaline water obtained in
1 / dm 3 was added to prepare washing water.
【００４４】上記のアルカリ性水を洗浄水として、以下
に述べるような方法で洗浄性、防錆性、スケール付着防
止性、酸性水のｐＨの比較を行った。被洗浄物は、一般
用冷間圧延鋼板（ＳＰＣＣ）寸法１００×５０×ｔ１ｍ
ｍを用いた。これにプレス加工油（日本工作油株式会社
ＰＧ−３０６６）を塗布し、各洗浄水をスプレー噴射し
て洗浄し、温風乾燥を行い、完全乾燥した後に室内放置
した。洗浄条件は洗浄水温度６０℃、スプレー圧０．５
ＭＰａ、洗浄時間２分、洗浄水量１５Ｌ／分である。Using the above alkaline water as wash water, the washability, rust prevention, scale adhesion prevention, and pH of acidic water were compared by the methods described below. The object to be cleaned is a general cold-rolled steel plate (SPCC) having a size of 100 × 50 × t1m.
m was used. A press working oil (Nippon Kogyo Oil Co., Ltd. PG-3066) was applied thereto, and each washing water was sprayed and washed, followed by hot air drying, and after complete drying, was left indoors. Washing conditions are: washing water temperature 60 ° C, spray pressure 0.5
MPa, washing time 2 minutes, washing water amount 15 L / min.
【００４５】評価方法は、洗浄性については洗浄後、温
風乾燥を行った被洗浄物を２５％墨汁水溶液に１分間浸
漬して引き上げ、自然乾燥した後に、表面に残った墨汁
の状況を観察して判断した。また、防錆性は墨汁水溶液
に浸漬しなかった被洗浄物を室内放置し、錆の発生状況
を観察した判断した。The evaluation method was as follows. Regarding the washing property, the object to be washed, which had been washed and then dried with warm air, was immersed in a 25% aqueous ink solution for 1 minute, pulled up, air-dried, and then observed the state of the ink remaining on the surface. I decided. The rust-preventing property was determined by leaving the object to be cleaned which was not immersed in the aqueous ink solution in a room and observing the occurrence of rust.
【００４６】電解イオン水生成装置のアルカリ性水配管
に対するスケール付着防止性の評価については、配管ホ
ースの内面に付着したスケールを観察して判断した。ま
た、アルカリ性水と同時に生成される酸性水のｐＨも測
定して、排水可能か判断した。各アルカリ性水のｐＨと
評価結果を表１に示す。The evaluation of the adhesion of scale to the alkaline water pipe of the electrolytic ionized water generator was made by observing the scale attached to the inner surface of the pipe hose. Further, the pH of the acidic water generated simultaneously with the alkaline water was also measured to determine whether or not drainage was possible. Table 1 shows the pH of each alkaline water and the evaluation results.
【００４７】[0047]
【表１】 [Table 1]
【００４８】表１において、洗浄性の○は墨汁の濡れ性
１００％、△８５％以上を示す。防錆性の◎は６０日放
置で錆発生なし、○は６０日放置で錆発生あり、△は４
０日放置で錆発生ありを示す。In Table 1, 洗浄 indicates a wettability of ink of 100% and Δ85% or more. ◎: No rust after 60 days, ○: 60 days, △: 4
It shows that rust is generated when left for 0 days.
【００４９】スケール付着性の○は連続３００時間の電
気分解を行っても配管へのスケール付着なし、△は配管
へのスケール付着はないが、洗浄タンク内にスケール付
着あり、×は６０時間で配管へのスケール付着ありを示
す。酸性水ｐＨの○はｐＨが５．８から６．５であり、
△はｐＨが４．５から５．８であり、×はｐＨが４．４
以下であることを示す。The scale adhesion ○ indicates that no scale adhered to the pipe even after continuous electrolysis for 300 hours, Δ indicates no scale adhered to the pipe, but scale adhered in the washing tank. This indicates that scale has adhered to the piping. The pH of the acidic water indicates that the pH is 5.8 to 6.5,
Δ indicates a pH of 4.5 to 5.8, and X indicates a pH of 4.4.
Indicates that:
【００５０】以上の結果から、実施例１、２、３−１、
３−２は洗浄性、防錆性、スケール付着防止性、酸性水
ｐＨの総ての項目で優れていることがわかる。From the above results, Examples 1, 2, 3-1,
It can be seen that 3-2 is excellent in all the items of washability, rust prevention, scale adhesion prevention, and acidic water pH.
【００５１】なお、本発明の各請求項の洗浄水を用いる
洗浄方法は、前述の材料や方法に限定されるものではな
く、鉄鋼以外の被洗浄物にも有効であり、洗浄方法も、
浸漬攪拌洗浄、浸漬超音波洗浄等でも優れた効果を示
す。The cleaning method using the cleaning water according to each claim of the present invention is not limited to the above-mentioned materials and methods, but is also effective for objects to be cleaned other than steel.
Excellent effects are also obtained in immersion stirring cleaning, immersion ultrasonic cleaning, and the like.
【００５２】次に、発明の第２の実施形態を以下に説明
する。ここで実施例として使用するアルカリ性水は実施
例１と同様の生成条件で製造したものである。Next, a second embodiment of the present invention will be described below. Here, alkaline water used as an example was produced under the same production conditions as in Example 1.
【００５３】比較例４として、溶存水素濃度を低下する
ため電解電圧をＤＣ５Ｖに低下して電気分解して得られ
たアルカリ性水を洗浄水とした。ただし、ｐＨが低下し
ないように炭酸ナトリウムの添加量は１０．０ｍｍｏｌ
／ｄｍ３とした。In Comparative Example 4, alkaline water obtained by electrolysis with the electrolytic voltage lowered to 5 V DC in order to lower the concentration of dissolved hydrogen was used as washing water. However, the amount of sodium carbonate added is 10.0 mmol so that the pH does not decrease.
/ Was dm 3.
【００５４】評価については、洗浄性と防錆性について
行った。評価方法及び表の記号は第１の実施形態と同様
である。The evaluation was made on the detergency and rust prevention. The evaluation method and the symbols in the table are the same as in the first embodiment.
【００５５】各アルカリ性水のｐＨと評価結果を表２に
示す。Table 2 shows the pH of each alkaline water and the evaluation results.
【００５６】[0056]
【表２】 [Table 2]
【００５７】上記の結果から、溶存水素濃度が高く、溶
存酸素濃度が低いほど、防錆効果が高いことがわかる。From the above results, it can be seen that the higher the dissolved hydrogen concentration and the lower the dissolved oxygen concentration, the higher the rust prevention effect.
【００５８】[0058]
【発明の効果】以上のように本発明では、硫酸イオン濃
度、塩化物イオン濃度、溶存酸素濃度が低いことにより
防錆力が高いアルカリ性水を得ることができる。また、
カルシウムイオン濃度、マグネシウムイオン濃度を低く
することで、配管へのスケール付着防止性があるアルカ
リ性水を得ることができる。As described above, according to the present invention, alkaline water having a high rust-preventive effect can be obtained by lowering the sulfate ion concentration, the chloride ion concentration and the dissolved oxygen concentration. Also,
By reducing the calcium ion concentration and the magnesium ion concentration, it is possible to obtain alkaline water having a scale adhesion preventing property to the pipe.
【００５９】更に、酸性水のｐＨ５．８より低くならな
いために、中和せずに排水可能となる。Further, since the pH of the acidic water does not become lower than 5.8, the water can be drained without neutralization.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 廣川 載泰 滋賀県東浅井郡びわ町細江30番地 高橋金 属株式会社内 Ｆターム(参考） 4D025 AA02 AB19 BA09 CA01 DA06 4D061 DA03 DB08 EA02 EB01 EB04 EB12 EB39 FA08 GC05 GC18 4K021 AA01 BA02 BA16 BB01 DB38 DC15 ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Hiroyasu Noriyasu 30th Hosoe, Biwa-cho, Higashi-Asai-gun, Shiga Prefecture F-term within Takahashi Metals Co., Ltd. 4D025 AA02 AB19 BA09 CA01 DA06 4D061 DA03 DB08 EA02 EB01 EB04 EB12 EB39 FA08 GC05 GC18 4K021 AA01 BA02 BA16 BB01 DB38 DC15
Claims (4)
ｍｍｏｌ／ｄｍ３以下、及びマグネシウムイオン濃度を
１．０ｍｍｏｌ／ｄｍ３以下にする工程と、この後に原
水中の炭酸ナトリウム濃度を０．１〜１０．０ｍｍｏｌ
／ｄｍ３に調整する工程を有し、これを電気分解してｐ
Ｈ値が８．０以上１３．０以下であり、及び／または、
酸化還元電位が−１００ｍＶ〜−１０００ｍＶである洗
浄水を得ることを特徴とする洗浄水の製造方法。1. The method according to claim 1, wherein the calcium ion concentration in the raw water is 1.0
mmol / dm 3 or less, and a step of the magnesium ion concentration to 1.0 mmol / dm 3 or less, the sodium carbonate concentration in the raw water after the 0.1~10.0mmol
/ Dm 3 , which is electrolyzed to p
H value is 8.0 or more and 13.0 or less, and / or
A method for producing cleaning water, comprising obtaining cleaning water having an oxidation-reduction potential of -100 mV to -1000 mV.
ｍ３以下、及び／または塩化物イオンを０．５ｍｍｏｌ
／ｄｍ３以下、及びカルシウムイオン濃度を１．０ｍｍ
ｏｌ／ｄｍ３以下、及びマグネシウムイオン濃度を１．
０ｍｍｏｌ／ｄｍ３以下にする工程と、この後に原水中
の炭酸ナトリウム濃度を０．１〜１０．０ｍｍｏｌ／ｄ
ｍ３に調整する工程を有し、これを電気分解してｐＨ値
が８．０以上１３．０以下であり、及び／または、酸化
還元電位が−１００ｍＶ〜−１０００ｍＶである洗浄水
を得ることを特徴とする洗浄水の製造方法。2. Sulfate ions in raw water are reduced to 0.2 mmol / d.
m 3 or less, and / or chloride ions 0.5mmol
/ Dm 3 or less, and calcium ion concentration of 1.0 mm
ol / dm 3 or less, and a magnesium ion concentration of 1.
0 mmol / dm 3 or less, and thereafter, the sodium carbonate concentration in the raw water is adjusted to 0.1 to 10.0 mmol / d.
having a step of adjusting the pH to m 3 and electrolyzing it to obtain washing water having a pH value of 8.0 or more and 13.0 or less and / or an oxidation-reduction potential of -100 mV to -1000 mV. A method for producing washing water.
造方法において、製造した洗浄水に水酸化カルシウムを
０．０５ｍｍｏｌ／ｄｍ３〜２ｍｍｏｌ／ｄｍ３の範囲
で添加する工程を有することを特徴とする洗浄水の製造
方法。3. The method for producing washing water according to claim 1, further comprising a step of adding calcium hydroxide to the produced washing water in a range of 0.05 mmol / dm 3 to 2 mmol / dm 3. A method for producing washing water.
造方法で製造したアルカリ性水中の溶存水素濃度が０．
０１ｍｇ／ｄｍ３以上であり、溶存酸素濃度が６ｍｇ／
ｄｍ３以下であることを特徴とする洗浄水。4. The concentration of dissolved hydrogen in alkaline water produced by the method for producing washing water according to claim 1 is 0.
01 mg / dm 3 or more, and the dissolved oxygen concentration is 6 mg / dm 3
dm 3 or less.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000329666A JP4025903B2 (en) | 2000-09-21 | 2000-09-21 | Washing water production method and washing water |
| KR10-2001-0007772A KR100398443B1 (en) | 2000-09-21 | 2001-02-16 | A method of producing a wash, and a wash itself |
| CNB011419156A CN1220636C (en) | 2000-09-21 | 2001-09-21 | Process for producing cleaning water and cleaning water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000329666A JP4025903B2 (en) | 2000-09-21 | 2000-09-21 | Washing water production method and washing water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2002096066A true JP2002096066A (en) | 2002-04-02 |
| JP4025903B2 JP4025903B2 (en) | 2007-12-26 |
Family
ID=18806306
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000329666A Expired - Fee Related JP4025903B2 (en) | 2000-09-21 | 2000-09-21 | Washing water production method and washing water |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP4025903B2 (en) |
| KR (1) | KR100398443B1 (en) |
| CN (1) | CN1220636C (en) |
Cited By (3)
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|---|---|---|---|---|
| WO2003042112A1 (en) * | 2001-11-13 | 2003-05-22 | Radical Waters (Ip) (Pty) Limited | Electrochemically activated carbonate and bicarbonate salt solutions |
| WO2004040981A1 (en) * | 2002-10-23 | 2004-05-21 | Radical Waters (Ip) (Pty) Limited | Method for enriching co2 concentrations in a plant environment |
| WO2009008318A1 (en) * | 2007-07-10 | 2009-01-15 | Prefectural University Of Hiroshima | Electrolytically reduced water, hot water for bathing, and method for suppression of lumpy fat |
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-
2000
- 2000-09-21 JP JP2000329666A patent/JP4025903B2/en not_active Expired - Fee Related
-
2001
- 2001-02-16 KR KR10-2001-0007772A patent/KR100398443B1/en not_active IP Right Cessation
- 2001-09-21 CN CNB011419156A patent/CN1220636C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003042112A1 (en) * | 2001-11-13 | 2003-05-22 | Radical Waters (Ip) (Pty) Limited | Electrochemically activated carbonate and bicarbonate salt solutions |
| WO2004040981A1 (en) * | 2002-10-23 | 2004-05-21 | Radical Waters (Ip) (Pty) Limited | Method for enriching co2 concentrations in a plant environment |
| WO2009008318A1 (en) * | 2007-07-10 | 2009-01-15 | Prefectural University Of Hiroshima | Electrolytically reduced water, hot water for bathing, and method for suppression of lumpy fat |
| JPWO2009008318A1 (en) * | 2007-07-10 | 2010-09-09 | 公立大学法人県立広島大学 | Method for suppressing electrolytically reduced water, hot water for bathing and fat mass |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4025903B2 (en) | 2007-12-26 |
| KR100398443B1 (en) | 2003-09-19 |
| CN1347850A (en) | 2002-05-08 |
| KR20020023632A (en) | 2002-03-29 |
| CN1220636C (en) | 2005-09-28 |
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