WO2012033077A1 - 銅エッチング廃液の処理方法 - Google Patents
銅エッチング廃液の処理方法 Download PDFInfo
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- WO2012033077A1 WO2012033077A1 PCT/JP2011/070225 JP2011070225W WO2012033077A1 WO 2012033077 A1 WO2012033077 A1 WO 2012033077A1 JP 2011070225 W JP2011070225 W JP 2011070225W WO 2012033077 A1 WO2012033077 A1 WO 2012033077A1
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- etching waste
- copper etching
- hydrogen peroxide
- waste liquid
- copper
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/46—Regeneration of etching compositions
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
Definitions
- the present invention relates to a method for treating a copper etching waste liquid containing hydrogen peroxide discharged from a liquid crystal manufacturing process or the like.
- a chemical containing a high concentration of hydrogen peroxide is used for the copper etching process in the liquid crystal manufacturing process. For this reason, a high concentration of hydrogen peroxide is contained in the copper etching waste liquid discharged from the copper etching process, and the hydrogen peroxide concentration is usually 1% by weight or more and may be about 6% by weight.
- activated carbon, catalase, manganese catalyst or the like is used as a method for treating hydrogen peroxide.
- the hydrogen peroxide concentration exceeds 1000 mg / L, the catalyst performance is reduced or the amount of catalyst used is reduced. There are problems such as increase. For this reason, there has been a practical problem in applying such a treatment method to a copper etching waste liquid having a hydrogen peroxide concentration of 1% by weight or more.
- Patent Document 1 As a method for treating hydrogen peroxide contained in a copper etching waste liquid containing hydrogen peroxide at a high concentration, the copper etching waste liquid is heated to 60 to 80 ° C. and maintained in the same temperature range for 0.5 to 10 hours.
- Patent Document 1 A method has been proposed (Patent Document 1).
- this method has the disadvantages that heat energy for heating is required for the decomposition of hydrogen peroxide and that the time required for the decomposition is long.
- the copper etching waste liquid is heated to 80 ° C. and then held for 7 hours to decompose hydrogen peroxide.
- An object of the present invention is to provide a method for efficiently decomposing hydrogen peroxide in a copper etching waste liquid even if it is a copper etching waste liquid containing hydrogen peroxide at a high concentration.
- the present inventors have adjusted the pH of the copper etching waste liquid, which is usually a strongly acidic liquid having a pH of 3 or lower, to 4 or higher.
- SS functions as a hydrogen peroxide decomposition catalyst. Therefore, it is only necessary to adjust the copper etching waste liquid to pH 4 or higher, without the need for dilution or heating. Also, chemicals other than alkaline agents for pH adjustment can be used. It has been found that hydrogen peroxide in a copper etching waste liquid can be efficiently decomposed without need.
- the present invention has been achieved on the basis of such knowledge, and the gist thereof is as follows.
- the method for treating a copper etching waste liquid according to the first aspect includes a step of adjusting the copper etching waste liquid containing hydrogen peroxide to pH 4 or more.
- the method for treating a copper etching waste liquid according to a second aspect includes, in the first aspect, a step of solid-liquid separation of SS generated by adjusting the copper etching waste liquid containing hydrogen peroxide to pH 4 or more. .
- the method for treating a copper etching waste liquid according to the third aspect is characterized in that, in the second aspect, the process includes adding a part or all of the solid-liquid separated SS to a copper etching waste liquid containing hydrogen peroxide.
- the method for treating a copper etching waste liquid according to the fourth aspect is characterized in that, in the second or third aspect, a step of recovering the SS separated into solid and liquid is included.
- the processing method of the copper etching waste liquid according to the fifth aspect includes the hydrogen peroxide in any one of the first to fourth aspects, using the processing water obtained by the processing of the copper etching waste liquid containing hydrogen peroxide as dilution water. It includes a step of adding to a copper etching waste liquid.
- the method for treating a copper etching waste liquid according to a sixth aspect is the method according to any one of the first to fifth aspects, wherein the copper etching waste liquid containing hydrogen peroxide has a hydrogen peroxide concentration of 1% by weight or more and a pH of 3 or less. It is characterized by being.
- the method for treating a copper etching waste liquid according to a seventh aspect is the method according to the sixth aspect, wherein the copper etching waste liquid containing hydrogen peroxide has a hydrogen peroxide concentration of 1 to 10% by weight and a pH of 1 to 3.
- the content of other components is 0.1 to 1.0% by weight of copper, 0.3 to 2.0% by weight of total nitrogen, and 0.5 to 3.0% by weight of TOC.
- the method for treating a copper etching waste liquid according to an eighth aspect is characterized in that, in any one of the first to seventh aspects, an alkaline agent is added to the copper etching waste liquid containing hydrogen peroxide to adjust the pH to 6-9. .
- the method for treating a copper etching waste liquid according to a ninth aspect is the method according to any one of the second to eighth aspects, wherein the copper etching waste liquid containing hydrogen peroxide is adjusted to pH 4 or more and reacted for 0.25 to 2.0 hours. Thereafter, the generated SS is subjected to solid-liquid separation.
- the method for treating a copper etching waste liquid according to a tenth aspect is the method according to any one of the fifth to ninth aspects, wherein the liquid temperature is adjusted to 40 to 70 ° C. by adding the dilution water to the copper etching waste liquid containing hydrogen peroxide. It is characterized by maintaining.
- the copper etching waste liquid treatment apparatus includes a pH adjusting tank into which a copper etching waste liquid containing hydrogen peroxide is introduced, an alkaline agent adding means for adding an alkaline agent to the pH adjusting tank, and a pH in the pH adjusting tank.
- a pH meter for measuring the pH a control means for controlling the alkali agent addition means based on the measured value of the pH meter, a reaction tank into which the effluent of the pH adjustment tank is introduced, and a solid tank into which the effluent of the reaction tank is introduced. It is characterized by comprising a liquid separation means, a means for returning a part of the sludge separated by the solid-liquid separation means to a pH adjusting tank, and a dehydration means for introducing the remainder of the separated sludge.
- the copper etching waste liquid treatment apparatus of the twelfth aspect is characterized in that, in the eleventh aspect, the copper etching waste liquid treatment apparatus has means for adding a part of the treated water separated by the solid-liquid separation means to the pH adjusting tank.
- the present invention it is only necessary to add an alkali agent to the copper etching waste liquid containing hydrogen peroxide to adjust the pH to 4 or higher, and it is necessary to add energy and dilution for heating, addition of chemicals other than the alkali agent, and the like.
- hydrogen peroxide in the copper etching waste liquid can be efficiently decomposed and removed.
- the copper etching waste liquid when the copper etching waste liquid is adjusted to pH 4 or more, SS containing copper is generated.
- the copper contained in the SS functions as a hydrogen peroxide decomposition catalyst.
- the generated SS may be solid-liquid separated and added to the copper etching waste liquid. Further, since this SS is mainly composed of copper, the solid-liquid separated SS may be recovered as a copper raw material, and the copper separated and recovered from the SS may be reused.
- the copper etching waste liquid to be treated according to the present invention is a strongly acidic waste liquid having a high concentration of hydrogen peroxide of 1% by weight or more and having a pH of 3 or less.
- the copper etching waste liquid containing hydrogen peroxide to be treated in the present invention is a copper etching waste liquid containing hydrogen peroxide discharged from a copper etching process using a chemical containing hydrogen peroxide, and usually its peroxidation.
- the hydrogen concentration is about 0.1 to 10% by weight
- the present invention is particularly a copper etching waste solution having a hydrogen peroxide concentration of 1% by weight or more, for example about 1 to 10% by weight, which is difficult to decompose hydrogen peroxide by a conventional method. It is effective for.
- the pH of such copper etching waste liquid is usually 3 or less, for example, about 1 to 3, and the content of components other than hydrogen peroxide is usually as follows. Copper content: 0.1-1.0% by weight Total nitrogen: 0.3-2.0% by weight TOC: 0.5 to 3.0% by weight
- an alkaline agent is added to such a hydrogen peroxide-containing copper etching waste solution to adjust the pH to 4 or more, preferably 6 or more, more preferably 7 to 9.
- the adjusted pH value is 4 or more, hydrogen peroxide can be efficiently decomposed and removed.
- the adjusted pH value is preferably higher from the viewpoint of the decomposition efficiency of hydrogen peroxide, the adjusted pH value is preferably not more than the above upper limit from the viewpoint of reducing the amount of alkali agent used and the safety of the working environment.
- alkali agent used for pH adjustment of copper etching waste liquid 1 type, or 2 or more types of general purpose alkali agents, such as sodium hydroxide and potassium hydroxide, can be used.
- the reaction time after adjusting the pH of the copper etching waste liquid is not particularly limited as long as the hydrogen peroxide in the copper etching waste liquid is sufficiently decomposed and removed, but according to the method of the present invention, the pH Since hydrogen in the liquid is efficiently decomposed and removed in a short time using copper in the SS generated by the adjustment as a catalyst, the reaction time (in the batch system shown in FIG. In the continuous system shown in FIGS. 2 and 3, the residence time in the reaction vessel may be as short as 0.25 to 2.0 hours, particularly 0.5 to 2.0 hours.
- the hydrogen peroxide in the copper etching waste liquid can be efficiently decomposed and removed simply by adjusting the pH of the copper etching waste liquid to 4 or higher.
- the decomposition reaction of hydrogen peroxide is an exothermic reaction
- the copper etching waste liquid which is the water to be treated, is treated with treated water, etc. You may make it process by diluting.
- the decomposition reaction formula of hydrogen peroxide is H 2 O 2 ⁇ H 2 O + 1 / 2O 2.
- the SS generated by adjusting the pH of the copper etching waste liquid is usually an SS mainly composed of copper having a copper content of about 40 to 80% by weight. You may use for a collection process.
- the copper in the SS functions as a decomposition catalyst for hydrogen peroxide
- the solid-liquid separated SS may be added to the copper etching waste solution for pH adjustment. It is possible to increase the decomposition efficiency of hydrogen peroxide by increasing the amount of copper catalyst therein. Addition of the solid-liquid separated SS to the copper etching waste liquid is particularly effective for the treatment of the copper etching waste liquid having a low copper concentration.
- FIG. 1 shows a batch-type treatment method.
- An alkali agent is added to the copper etching waste liquid 2 charged into the reaction tank 1 and stirred in the stirring tank 3.
- the pH of the liquid in the reaction vessel 1 is measured by the pH meter 4, and when the pH value reaches a predetermined pH value, the addition of the alkaline agent is stopped, and the reaction is further completed by stirring for a predetermined time.
- SS is generated in the reaction tank 1 after the reaction, this is solid-liquid separated to obtain treated water, and the separated SS is used for the treatment of the copper etching waste liquid or recovered as a copper raw material.
- FIG. 2 shows a continuous treatment method, in which a copper etching waste liquid is continuously passed through the reaction tank 1 at a predetermined flow rate, and an alkaline agent is added at a predetermined flow rate with stirring.
- the alkaline agent is added by a chemical injection pump 5 interlocked with the pH meter 4 so that the liquid pH in the reaction tank 1 becomes a predetermined pH value.
- the copper etching waste liquid is maintained in the reaction tank 1 for a predetermined residence time by adding an alkali agent.
- the treated water from which hydrogen peroxide has been decomposed and removed by the reaction is taken out from the reaction tank 1 and fed to the next step, where solid-liquid separation of SS, recovery of separated SS, and the like are performed.
- FIG. 3 shows an example of an industrial continuous process, in which the copper etching waste liquid is first introduced into the pH adjusting tank 11 and an alkali agent is added to adjust the pH.
- the addition amount of the alkaline agent is controlled by a chemical injection pump interlocked with a pH meter (not shown) as in FIG.
- the effluent from the pH adjustment tank 11 is then fed to the reaction tank 12, where a reaction is performed for a predetermined time in the reaction tank 12, and the reaction liquid is then fed to the precipitation tank 13 for solid-liquid separation.
- the separated water that has been separated into solid and liquid in the settling tank 13 is taken out as treated water and used for further wastewater treatment or industrial waste treatment.
- a part of the separated sludge is returned to the pH adjustment tank 1 as a return sludge, and the remainder is recovered after being dehydrated by the dehydrator 14.
- the treated water separated in the precipitation tank 13 may be partly returned to the pH adjusting tank 11 to dilute the copper etching waste liquid.
- Example 1 Sodium hydroxide was added to a copper etching waste solution having the same composition as in Comparative Example 1 to adjust the pH to 4 to 10, and the hydrogen peroxide concentration of the copper etching waste solution after 1 hour was measured. The results are shown in Table 1.
- Example 2 About the copper etching waste liquid (pH 2.2, other components are the same as the copper etching waste liquid in Experimental Example 1) having a hydrogen peroxide concentration of 6% by weight and a copper concentration of 0.7% by weight, the pH is adjusted in the same manner as in Example 1. The relationship between the adjusted pH value and the hydrogen peroxide concentration in the copper etching waste solution after 1 hour was examined. The results are shown in Table 2. Table 2 also shows the temperature rise ( ⁇ t) of the copper etching waste liquid after 1 hour.
- Examples 3 and 4 The copper etching waste liquid having the same composition as the copper etching waste liquid treated in Example 2 was used as a stock solution, and the treatment was performed continuously using the reaction tank shown in FIG.
- the reaction tank 1 was filled with treated water in advance, and the stock solution was allowed to flow at a predetermined flow rate.
- Sodium hydroxide was added as an alkaline agent to the reaction tank 1 to adjust the pH of the liquid in the tank to 7 (Example 3) or 8 (Example 4).
- the volume of the reaction tank 1 was twice the flow rate of the stock solution per hour, and the residence time of the stock solution in the reaction tank 1 was 2 hours.
- Table 3 shows the relationship between the liquid passing time and the hydrogen peroxide concentration of the obtained treated water.
- Example 3 adjusted to pH 7, the hydrogen peroxide concentration of the treated water gradually decreased after 1 to 4 hours of liquid passage because the temperature of the reaction vessel increased, so the reaction rate increased and the decomposition efficiency improved. It depends on.
- Example 2 As a result of solid-liquid separation of SS generated in the treatment of Example 4 (pH 8), drying at 105 ° C. for 2 hours, and dissolving in acid, the content of copper (CuO) in this SS was 45% by weight or more. It was confirmed that.
- the following hydrogen peroxide decomposition treatment was performed using this SS.
- An aqueous solution (pH 2.2) having a hydrogen peroxide concentration of 3% by weight was prepared using reagent hydrogen peroxide, and 1% by weight of SS was added to this aqueous hydrogen peroxide solution as a test solution, and no SS was added. Each was adjusted to pH 8 by adding sodium hydroxide, and the hydrogen peroxide concentration in the liquid after 1 hour was measured. The results are shown in Table 4.
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Abstract
Description
しかしながら、この方法では、過酸化水素の分解に加熱のための熱エネルギーを要する上に、分解に要する時間が長いという欠点がある。実際、特許文献1の実施例では、銅エッチング廃液を80℃に加熱した後7時間保持して過酸化水素を分解している。
銅含有量:0.1~1.0重量%
全窒素:0.3~2.0重量%
TOC:0.5~3.0重量%
H2O2→H2O+1/2O2
で表され、分解の反応熱は23.45kcal/molである。従って、例えば6重量%過酸化水素溶液中の過酸化水素をすべて分解する場合には、Δt=41℃の液温の上昇があり、3重量%の過酸化水素溶液中の過酸化水素をすべて分解する場合には、Δt=21℃の液温の上昇がある。従って、実用上は、処理水等でpH調整に供する銅エッチング廃液を希釈し、反応液の温度を40~70℃の範囲に維持するようにすることが好ましい。
下記組成の銅エッチング廃液(pH2.2)をpH調整することなく、そのまま放置し、銅エッチング廃液中の過酸化水素濃度の経時変化を調べたところ、一日経過後の銅エッチング廃液の過酸化水素濃度は2.9重量%であり、過酸化水素濃度は殆ど低下しなかった。即ち、そのままでは銅エッチング廃液中の過酸化水素は分解されないことが分かる。
過酸化水素:3重量%
銅:0.4重量%
全窒素:0.8重量%
TOC:1.1重量%
比較例1におけると同組成の銅エッチング廃液に水酸化ナトリウムを添加して、pH4~10に調整し、1時間経過後の銅エッチング廃液の過酸化水素濃度を測定した。結果を表1に示す。
過酸化水素濃度6重量%、銅濃度0.7重量%の銅エッチング廃液(pH2.2,その他の成分は実験例1における銅エッチング廃液と同様)について、実施例1と同様にpH調整し、調整pH値と1時間経過後の銅エッチング廃液の過酸化水素濃度との関係を調べた。結果を表2に示す。表2には1時間後の銅エッチング廃液の液温の上昇温度(Δt)を併記した。
実施例2で処理した銅エッチング廃液と同組成の銅エッチング廃液を原液として、図2に示す反応槽を用いて、連続式で処理を行った。反応槽1には予め処理水を張り込み、原液を所定の流量で流した。反応槽1にはアルカリ剤として水酸化ナトリウムを添加して、槽内液のpHを7(実施例3)又は8(実施例4)に調整した。反応槽1の容積は1時間当たりの原液通液量の2倍とし、反応槽1での原液の滞留時間は2時間とした。このときの通液時間と得られた処理水の過酸化水素濃度との関係を表3に示す。
実施例4(pH8)の処理で発生したSSを固液分離して、105℃で2時間乾燥後、酸に溶解させて分析した結果、このSSの銅(CuO)含有量は45重量%以上であることが確認された。
このSSを用いて以下の過酸化水素分解処理を行った。
試薬過酸化水素を用いて過酸化水素濃度3重量%の水溶液(pH2.2)を調製し、この過酸化水素水溶液を試験液としてSSを1重量%添加したものと、SS未添加のものとについて、それぞれ水酸化ナトリウムを添加してpH8に調整し、1時間経過後の液中の過酸化水素濃度を測定した。結果を表4に示す。
1 反応槽
2 銅エッチング廃液
3 撹拌機
4 pH計
5 薬注ポンプ
11 pH調整槽
12 反応槽
13 沈殿槽
14 脱水機
なお、本出願は、2010年9月8日付で出願された日本特許出願(特願2010-201158)に基づいており、その全体が引用により援用される。
Claims (12)
- 過酸化水素を含む銅エッチング廃液をpH4以上に調整する工程を含むことを特徴とする銅エッチング廃液の処理方法。
- 請求項1において、前記過酸化水素を含む銅エッチング廃液をpH4以上に調整することにより発生したSSを固液分離する工程を含むことを特徴とする銅エッチング廃液の処理方法。
- 請求項2において、固液分離された前記SSの一部又は全部を過酸化水素を含む銅エッチング廃液に添加する工程を含むことを特徴とする銅エッチング廃液の処理方法。
- 請求項2又は3において、固液分離された前記SSを回収する工程を含むことを特徴とする銅エッチング廃液の処理方法。
- 請求項1ないし4のいずれか1項において、前記過酸化水素を含む銅エッチング廃液の処理で得られた処理水を希釈水として前記過酸化水素を含む銅エッチング廃液に添加する工程を含むことを特徴とする銅エッチング廃液の処理方法。
- 請求項1ないし5のいずれか1項において、前記過酸化水素を含む銅エッチング廃液の過酸化水素濃度が1重量%以上であり、pHが3以下であることを特徴とする銅エッチング廃液の処理方法。
- 請求項6において、前記過酸化水素を含む銅エッチング廃液の過酸化水素濃度が1~10重量%で、pHが1~3であり、過酸化水素以外の成分の含有量が、銅 0.1~1.0重量%、全窒素 0.3~2.0重量%、TOC 0.5~3.0重量%であることを特徴とする銅エッチング廃液の処理方法。
- 請求項1ないし7のいずれか1項において、前記過酸化水素を含む銅エッチング廃液にアルカリ剤を添加してpH6~9に調整することを特徴とする銅エッチング廃液の処理方法。
- 請求項2ないし8のいずれか1項において、前記過酸化水素を含む銅エッチング廃液をpH4以上に調整して0.25~2.0時間反応させた後、発生したSSを固液分離することを特徴とする銅エッチング廃液の処理方法。
- 請求項5ないし9のいずれか1項において、前記過酸化水素を含む銅エッチング廃液に前記希釈水を添加することにより、液温を40~70℃に維持することを特徴とする銅エッチング廃液の処理方法。
- 過酸化水素を含む銅エッチング廃液が導入されるpH調整槽と、pH調整槽にアルカリ剤を添加するアルカリ剤添加手段と、pH調整槽内のpHを測定するpH計と、pH計の測定値に基いてアルカリ剤添加手段を制御する制御手段と、pH調整槽の流出液が導入される反応槽と、反応槽の流出液が導入される固液分離手段と、固液分離手段で分離された汚泥の一部をpH調整槽に返送する手段と、分離汚泥の残部が導入される脱水手段とを備えることを特徴とする銅エッチング廃液の処理装置。
- 請求項11において、前記固液分離手段で分離された処理水の一部を前記pH調整槽に添加する手段を有することを特徴とする銅エッチング廃液の処理装置。
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CN201180043075.2A CN103097302B (zh) | 2010-09-08 | 2011-09-06 | 铜蚀刻废液的处理方法 |
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TW201416330A (zh) * | 2012-10-23 | 2014-05-01 | Mega Union Technology Inc | 廢水處理方法及其設備 |
TWI562957B (en) * | 2013-11-01 | 2016-12-21 | Yu Ming Chia | Methoh of the decomposition of hydrogen peroxide included in sulfuric acid |
CN106103354B (zh) * | 2014-04-10 | 2019-06-04 | 栗田工业株式会社 | 含铜废水的处理方法以及处理装置 |
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JP2005193191A (ja) * | 2004-01-09 | 2005-07-21 | Denki Kagaku Kogyo Kk | 廃水処理方法 |
JP2007038196A (ja) * | 2005-08-04 | 2007-02-15 | Noatech:Kk | 金属エッチング排水の処理方法 |
JP2010077521A (ja) * | 2008-08-25 | 2010-04-08 | Ebara Engineering Service Co Ltd | 銅含有酸性廃液からの銅の回収方法及び装置 |
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JP2012055825A (ja) | 2012-03-22 |
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