TWI423934B - Acid copper - containing waste liquid recycling manufacturing electrolytic copper method - Google Patents
Acid copper - containing waste liquid recycling manufacturing electrolytic copper method Download PDFInfo
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- TWI423934B TWI423934B TW100132504A TW100132504A TWI423934B TW I423934 B TWI423934 B TW I423934B TW 100132504 A TW100132504 A TW 100132504A TW 100132504 A TW100132504 A TW 100132504A TW I423934 B TWI423934 B TW I423934B
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- copper
- waste liquid
- containing waste
- acidic
- electrolytic copper
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims description 83
- 229910052802 copper Inorganic materials 0.000 title claims description 83
- 239000010949 copper Substances 0.000 title claims description 83
- 239000007788 liquid Substances 0.000 title claims description 52
- 239000002699 waste material Substances 0.000 title claims description 35
- 238000000034 method Methods 0.000 title claims description 16
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 238000004064 recycling Methods 0.000 title claims description 8
- 239000002253 acid Substances 0.000 title claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 16
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 14
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 14
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 13
- 239000003729 cation exchange resin Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 7
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 6
- 229910001431 copper ion Inorganic materials 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 4
- 125000000542 sulfonic acid group Chemical group 0.000 claims description 3
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 18
- 239000010802 sludge Substances 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 6
- 238000007747 plating Methods 0.000 description 5
- 238000005341 cation exchange Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- YXLXNENXOJSQEI-UHFFFAOYSA-L Oxine-copper Chemical compound [Cu+2].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 YXLXNENXOJSQEI-UHFFFAOYSA-L 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 108010054404 Adenylyl-sulfate kinase Proteins 0.000 description 1
- 102100039024 Sphingosine kinase 1 Human genes 0.000 description 1
- 150000001768 cations Chemical group 0.000 description 1
- 229920001429 chelating resin Polymers 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Water Treatment By Electricity Or Magnetism (AREA)
- Electrolytic Production Of Metals (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Description
本發明有關於一種酸性含銅廢液回收製造電解銅方法，尤指一種針對印刷電路板製程中所產生之鍍銅水洗液、微蝕槽洗槽液等混合液進行回收處理，並且製造出電解銅。The invention relates to a method for producing electrolytic copper by recycling an acidic copper-containing waste liquid, in particular to a mixture of a copper plating water washing liquid and a micro etching tank washing liquid generated in a process of a printed circuit board, and manufacturing the electrolytic solution. copper.
隨著電子產品的快速發展，已相對提升相關之高密度封裝技術。而印刷電路板為承載電子產品之主要裝置，因此需要能製作輕薄的印刷電路板，並具有細線寬、微孔，以及高密度設計之製造技術。目前印刷電路板的製造程序包括壓置一金屬薄膜在一基板上，藉由旋轉塗佈一光阻層，然後執行以下的步驟：遮罩曝光、顯影、蝕刻、鑽孔與烘烤、疊層與鍍膜等。With the rapid development of electronic products, the related high-density packaging technology has been relatively improved. The printed circuit board is the main device for carrying electronic products, so it is required to be able to manufacture thin and light printed circuit boards, and has a manufacturing technique of thin line width, micro holes, and high density design. At present, the manufacturing process of the printed circuit board includes pressing a metal film on a substrate, spin coating a photoresist layer, and then performing the following steps: mask exposure, development, etching, drilling and baking, lamination With coatings, etc.
目前印刷電路板製程之用水量大，並且會產生大量的酸性含銅廢液，例如：鍍銅水洗液、微蝕槽洗槽液等混合液，由於酸性含銅廢液之銅濃度低於2000ppm，回收效益低，故所有印刷電路板產業所產生的酸性含銅廢液大多排入廢水池中，再採用中和、混凝沉澱處理法，使銅在鹼性條件下，經由混凝、絮凝、沉澱等步驟，以去除銅離子。惟當廢水達到排放標準時，但却相對產生了大量污泥，而且污泥在進行無害化處理時，必須經過乾燥、焚燒等程序，更會造成二次污染，浪費資源，增加碳排放量。因此要如何改善上述問題與缺失，即為印刷電路板產業所極欲研究發展之方向。At present, the printed circuit board process has a large amount of water, and a large amount of acidic copper-containing waste liquid is generated, for example, a mixed solution of a copper-plated water washing liquid and a micro-etching tank washing liquid, and the copper concentration of the acidic copper-containing waste liquid is less than 2000 ppm. The recycling efficiency is low, so most of the acidic copper-containing waste liquid generated by the printed circuit board industry is discharged into the wastewater pool, and then neutralized and coagulated and precipitated, so that the copper can be coagulated and flocculated under alkaline conditions. , precipitation, etc. to remove copper ions. However, when the wastewater reaches the discharge standard, a large amount of sludge is relatively produced, and when the sludge is treated harmlessly, it must be subjected to procedures such as drying and incineration, which may cause secondary pollution, waste resources, and increase carbon emissions. Therefore, how to improve the above problems and lacks is the direction of the research and development of the printed circuit board industry.
本發明之目的在於提供一種酸性含銅廢液回收製造電解銅方法，主要適用於印刷電路板製程中所產生之鍍銅水洗液、微蝕槽洗槽液等混合液進行回收處理，並且製造出電解銅，能夠降低處理費用，不產生污泥，節能減碳，更增進經濟效益。The object of the present invention is to provide a method for producing electrolytic copper by recovering acidic copper-containing waste liquid, which is mainly suitable for recycling and processing a mixed solution of a copper-plated water washing liquid and a micro-etching tank washing liquid generated in a process of a printed circuit board, and is manufactured. Electrolytic copper can reduce the treatment cost, produce no sludge, save energy and reduce carbon, and enhance economic benefits.
為達上揭目的，本發明係對於印刷電路板製程中所產生之酸性含銅廢液進行回收處理，其包含有依序進行以下步驟：以陽離子交換樹脂吸附酸性含銅廢液中之銅離子；將陽離子交換樹脂以硫酸溶液進行再生，使銅解析成硫酸銅溶液；將硫酸銅溶液進行電解提銅處理，以製造出電解銅；當硫酸銅溶液進行電解提銅處理後，其銅濃度下降至600ppm以下時，即可返回作為硫酸溶液重複使用，而不必排放。In order to achieve the above object, the present invention recovers the acidic copper-containing waste liquid generated in the process of the printed circuit board, which comprises the steps of: sequentially adsorbing copper ions in the acidic copper-containing waste liquid by using a cation exchange resin. The cation exchange resin is regenerated with a sulfuric acid solution to resolve copper into a copper sulfate solution; the copper sulfate solution is subjected to electrolytic copper extraction to produce electrolytic copper; when the copper sulfate solution is subjected to electrolytic copper extraction, the copper concentration is decreased. When it is below 600ppm, it can be reused as a sulfuric acid solution without being discharged.
於較佳實施例中，酸性含銅廢液為鍍銅水洗液、微蝕槽洗槽液之至少一種，該酸性含銅廢液之銅濃度小於2000ppm，該硫酸銅溶液之銅濃度為20~25克/公升，以提高電解提銅效益。In a preferred embodiment, the acidic copper-containing waste liquid is at least one of a copper-plated water washing liquid and a micro-etching tank washing liquid. The copper concentration of the acidic copper-containing waste liquid is less than 2000 ppm, and the copper concentration of the copper sulfate solution is 20~. 25 g / liter to improve the efficiency of electrolytic copper extraction.
於較佳實施例中，陽離子交換樹脂為苯乙烯-二乙烯苯共聚，其基體上帶有磺酸基(-SO3H)。In a preferred embodiment, the cation exchange resin is a styrene-divinylbenzene copolymer having a sulfonic acid group (-SO3H) on its substrate.
於較佳實施例中，硫酸溶液濃度為10~20%(重量百分比)。In a preferred embodiment, the concentration of the sulfuric acid solution is from 10 to 20% by weight.
有關本發明為達成上述目的，所採用之技術手段及其功效，茲舉出可行實施例，並且配合圖式說明如下：首先，請參閱第一圖，本發明酸性含銅廢液回收製造電解銅方法係專供印刷電路板產業使用，以用於回收處理印刷電路板製程中所產生之酸性含銅廢液1，其包括鍍銅水洗液、微蝕槽洗槽液等至少一種廢液及/或混合液，將酸性含銅廢液1依序進行陽離子交換、再生、電解提銅等程序，以製造出電解銅8。The technical means and the efficacy thereof for achieving the above object are as follows, and the following is a description of the possible embodiments. First, referring to the first figure, the electrolytic copper-containing waste liquid of the present invention is recycled to produce electrolytic copper. The method is specially designed for use in the printed circuit board industry for recycling and processing the acidic copper-containing waste liquid 1 produced in the printed circuit board process, and includes at least one kind of waste liquid such as copper plating water washing liquid and micro etching tank washing liquid and/or Or the mixed solution, the acidic copper-containing waste liquid 1 is sequentially subjected to procedures such as cation exchange, regeneration, and electrolytic copper extraction to produce electrolytic copper 8.
於第一圖所示之較佳實施例中，本發明酸性含銅廢液回收製造電解銅方法包含有依序進行以下步驟：In the preferred embodiment shown in the first figure, the method for producing electrolytic copper by recycling the acidic copper-containing waste liquid of the present invention comprises the following steps:
首先，回收印刷電路板製程中所產生之酸性含銅廢液1，其包括銅濃度小於2000ppm之鍍銅水洗液、微蝕槽洗槽液等至少一種廢液及/或混合液，一般酸性含銅廢液之濃度大多在2～500ppm，而PH值在1～2之間。First, the acidic copper-containing waste liquid 1 produced in the process of printing a printed circuit board is recovered, and includes at least one waste liquid and/or a mixed liquid such as a copper plating water washing liquid having a copper concentration of less than 2000 ppm, a micro-etching tank washing liquid, and the like, generally acidic. The concentration of the copper waste liquid is mostly between 2 and 500 ppm, and the pH is between 1 and 2.
以陽離子交換樹脂2吸附酸性含銅廢液1中之銅離子，於較佳實施例中，陽離子交換樹脂2為苯乙烯-二乙烯苯共聚，其基體上帶有磺酸基(-SO3H)，例如採用美國Amberrlite IR-120，Dowex-50，或西德Lewatit-100或日本DiaonSK-1等。而銅為陽離子與樹脂交換基交換，以吸附於樹脂上。The copper ion in the acidic copper-containing waste liquid 1 is adsorbed by the cation exchange resin 2. In the preferred embodiment, the cation exchange resin 2 is copolymerized with styrene-divinylbenzene, and the substrate has a sulfonic acid group (-SO3H). For example, American Amberlite IR-120, Dowex-50, or West German Lewatit-100 or Japanese Diaon SK-1 and the like are used. Copper is a cation exchanged with a resin exchange group to adsorb onto the resin.
酸性含銅廢液1之銅離子被吸附於陽離子交換樹脂2上，使其出水3之銅濃度小於0.5ppm，因此可與一般廢水進行廢水混合處理4，以調整PH值在6～9之間，即可達到排放標準。The copper ion of the acidic copper-containing waste liquid 1 is adsorbed on the cation exchange resin 2, so that the copper concentration of the effluent 3 is less than 0.5 ppm, so that the wastewater can be mixed with the general wastewater 4 to adjust the pH between 6 and 9. To meet emission standards.
當陽離子交換樹脂2吸附酸性含銅廢液1中之銅離子達到飽和狀態時，將陽離子交換樹脂2以硫酸溶液5進行再生，硫酸溶液5濃度可為10～20%(重量百分比)，使銅解析成硫酸銅溶液6，並且銅濃度為20～25克/公升。When the cation exchange resin 2 adsorbs the copper ions in the acidic copper-containing waste liquid 1 to a saturated state, the cation exchange resin 2 is regenerated with the sulfuric acid solution 5, and the concentration of the sulfuric acid solution 5 may be 10 to 20% by weight to make copper. The copper sulfate solution 6 was resolved and the copper concentration was 20 to 25 g/liter.
將硫酸銅溶液6送入高效能電解機，以進行電解提銅處理7，而製造出電解銅8。The copper sulfate solution 6 is sent to a high-performance electrolysis machine to perform electrolytic copper plating treatment 7, thereby producing electrolytic copper 8.
當硫酸銅溶液6進行電解提銅處理7，其銅濃度下降至400～600ppm之間或以下時，即可成為再生液，以返回作為硫酸溶液5重複使用，而不必排放。When the copper sulfate solution 6 is subjected to electrolytic copper extraction treatment 7, and the copper concentration is lowered to between 400 and 600 ppm or less, it becomes a regenerating liquid, and is returned to be used as the sulfuric acid solution 5, without being discharged.
茲舉出本發明用於健鼎(無錫)電子有限公司芙蓉廠之實施例，健鼎(無錫)電子有限公司芙蓉廠之製程中所產生的C系酸性含銅廢液，其含銅濃度為300～500ppm，日排水量2500m3 ，實施前每日銅流失約：400ppm×2500m3 =1000公斤，若污泥以含銅4%計算時，約產生25噸污泥。The invention is directed to the embodiment of Jianlong (Wuxi) Electronics Co., Ltd. Furong Factory, the C-based acidic copper-containing waste liquid produced in the process of Jianding (Wuxi) Electronics Co., Ltd. Furong Factory, the copper concentration of which is 300~ 500ppm, daily displacement of 2500m 3 , daily copper loss before implementation: about 400ppm × 2500m 3 = 1000 kg, if the sludge is calculated as 4% copper, about 25 tons of sludge.
實施設備：三支陽離子交換柱，並且各裝設100公升樹脂。電解機一套，其整流器為500A×36V，儲槽為1000公升。Equipment: Three cation exchange columns, each equipped with 100 liters of resin. A set of electrolysis machines, the rectifier is 500A × 36V, and the storage tank is 1000 liters.
本實施例以C系(類)酸性含銅廢液經由收集槽泵送至陽離子交換柱進行吸附，於此特舉出陽離子交換前後之進出水的銅濃度比較表，以及硫酸銅溶液數據表：In this embodiment, the C-series (type) acidic copper-containing waste liquid is pumped to the cation exchange column through the collection tank for adsorption, and the copper concentration comparison table of the inlet and outlet water before and after the cation exchange and the copper sulfate solution data table are specifically listed here:
綜上所述，本發明可解決習知技術之不足與缺失，其關鍵技術在於將印刷電路板製程中所產生之鍍銅水洗液、微蝕槽洗槽液等混合液進行回收處理，並且製造出電解銅，能夠降低處理費用，不產生污泥，節能減碳，更增進經濟效益，爰依法提出發明專利申請。In summary, the present invention can solve the deficiencies and shortcomings of the prior art, and the key technology is to recover and process the mixed solution of the copper plating water washing liquid and the micro etching tank washing liquid generated in the process of the printed circuit board. Electrolytic copper can reduce the processing cost, produce no sludge, save energy and reduce carbon, and enhance economic benefits.
以上所舉實施例僅用為方便說明本發明，而並非加以限制，在不離本發明精神範疇，熟悉此一行業技藝人士所可作之各種簡易變化與修飾，均仍應含括於以下申請專利範圍中。The above embodiments are intended to be illustrative of the present invention and are not intended to be limiting, and the various modifications and modifications which may be made by those skilled in the art are still included in the following claims. In the scope.
1‧‧‧酸性含銅廢液1‧‧‧Acid copper-containing waste liquid
2‧‧‧陽離子交換樹脂2‧‧‧Cation exchange resin
3‧‧‧出水3‧‧‧Water
4‧‧‧廢水混合處理4‧‧‧ Wastewater mixing treatment
5‧‧‧硫酸溶液5‧‧‧ sulfuric acid solution
6‧‧‧硫酸銅溶液6‧‧‧ copper sulfate solution
7‧‧‧電解提銅處理7‧‧‧ Electrolytic copper treatment
8‧‧‧電解銅8‧‧‧electrolytic copper
第一圖係本發明較佳實施例酸性含銅廢液回收製造電解銅方法之方塊圖。The first figure is a block diagram of a method for producing electrolytic copper by recycling an acidic copper-containing waste liquid according to a preferred embodiment of the present invention.
1．．．酸性含銅廢液1. . . Acidic copper-containing waste liquid
2．．．陽離子交換樹脂2. . . Cation exchange resin
3．．．出水3. . . Water
4．．．廢水混合處理4. . . Wastewater mixing treatment
5．．．硫酸溶液5. . . Sulfuric acid solution
6．．．硫酸銅溶液6. . . Copper sulfate solution
7．．．電解提銅處理7. . . Electrolytic copper treatment
8．．．電解銅8. . . Electrolytic copper
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| CN110453245B (en) * | 2018-05-07 | 2021-12-28 | 卫司特科技股份有限公司 | Method for treating and recovering copper ions in copper etching waste liquid |
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|---|---|---|---|---|
| TWI267417B (en) * | 2001-11-29 | 2006-12-01 | Ebara Corp | Method and device for regenerating ion exchanger, and electrolytic processing apparatus |
| TWI347365B (en) * | 2007-07-24 | 2011-08-21 |
-
2011
- 2011-09-09 TW TW100132504A patent/TWI423934B/en not_active IP Right Cessation
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI267417B (en) * | 2001-11-29 | 2006-12-01 | Ebara Corp | Method and device for regenerating ion exchanger, and electrolytic processing apparatus |
| TWI347365B (en) * | 2007-07-24 | 2011-08-21 |
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| TW201311570A (en) | 2013-03-16 |
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