CN117926349A - 从铜箔制造用阳极去除铅物质的方法 - Google Patents
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- 239000011889 copper foil Substances 0.000 title claims abstract description 45
- 239000000126 substance Substances 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004140 cleaning Methods 0.000 claims abstract description 40
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 239000013522 chelant Substances 0.000 claims description 2
- FZIPCQLKPTZZIM-UHFFFAOYSA-N 2-oxidanylpropane-1,2,3-tricarboxylic acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O.OC(=O)CC(O)(C(O)=O)CC(O)=O FZIPCQLKPTZZIM-UHFFFAOYSA-N 0.000 abstract description 4
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- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 1
- 102100021587 Embryonic testis differentiation protein homolog A Human genes 0.000 description 1
- 101000898120 Homo sapiens Embryonic testis differentiation protein homolog A Proteins 0.000 description 1
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- YADSGOSSYOOKMP-UHFFFAOYSA-N lead dioxide Inorganic materials O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供一种从铜箔制造用阳极去除铅物质的方法。本发明包括清洗液准备工序、阳极洗涤工序以及阳极水洗工序。清洗液准备工序准备由EDTA和柠檬酸(citric acid)水溶液制备的清洗液。这样的清洗液在维持7～9的pH浓度和20～50℃的温度范围的同时进行阳极洗涤工序。另外，阳极洗涤工序通过将表面附着有铅物质的铜箔制造用阳极放入清洗液中来进行EDTA‑Pb螯合。如此操作而使阳极的铅物质移动至清洗液中实质上是将铅物质从阳极去除。然后，用高压洗涤机对去除了铅物质的铜箔制造用阳极进行洗涤。
Description
技术领域
本发明涉及从利用电解反应来制造铜箔的阳极去除铅物质(Lead materials)的方法，更详细而言，涉及利用ETDA和柠檬酸(citric acid)来去除铜箔制造用阳极的铅物质从而使阳极再生的阳极的铅物质去除方法。
背景技术
作为利用电解反应来制造铜箔的现有专利，可举出韩国公开专利第10-2019-0038325号。如果参考这样的现有专利，则如图1所图示的那样，为了制造铜箔，利用由浸渍于电解槽10的电解液12中的不溶性阳极20和鼓状的转鼓形阴极30构成的装置。
以与鼓形阴极30对置的方式设置的不溶性阳极20具有与鼓形阴极30的圆筒形外观相称的凹面形状。如果在这样的不溶性阳极20与鼓形阴极30之间通电，则能够在鼓形阴极30的表面生长金属成分。因此，如果在通电状态下使鼓形阴极30相对于镀覆用电极20旋转，则在鼓形阴极30上基于电解反应而形成铜箔。将如此形成的铜箔从鼓形阴极30剥离，能够连续地获得铜箔。
在这样形成铜箔的过程中，铜箔制造用阳极20会附着并生长铅物质(Leadmaterials)(PbO、PbO2、PbSO4)。如上所述，如果在制造电解铜箔的过程中附着并生长铅物质，则不仅铜箔制造用阳极20的功能减弱，由此还会对铜箔的品质造成不良影响。
因此，需要将阳极20从电解槽分离来将阳极20表面的铅物质去除。为了去除这样的铅物质，可以利用物理性的力，但如此利用物理性的力时，存在阳极的表面可能受到物理损伤的担忧。作为其他方法，可以通过化学方法来去除铅物质，例如，可以考虑利用酸(Acid)来去除铅物质。
但是，如果利用酸，则不仅作业环境恶化，还存在不环保的缺点。另外，处理含有所使用的酸的废水在环境和经济方面不可取也是实际情况。因此，可以说，需要一种能够在充分具有经济性和效率性以及环境亲和性的同时从铜箔制造用阳极20去除铅物质的方法。
发明内容
所要解决的课题
本发明的目的在于，提供一种铜箔制造用阳极的铅物质去除方法，其能够利用EDTA和柠檬酸来有效去除铜箔制造用阳极的铅物质(Lead materials)。
解决课题的方法
根据用于实现如上目的的本发明，作为去除在具有与用于形成铜箔的转鼓形阴极30相对应的凹面形状的铜箔制造用阳极20的表面所附着的铅物质(Lead matirials)的方法，包括清洗液准备工序、阳极洗涤工序以及阳极水洗工序。
这里，清洗液准备工序中，准备包含EDTA和柠檬酸(citric acid)水溶液的清洗液。这样的清洗液是在维持7～9的pH浓度、20～50℃的温度范围的同时进行阳极洗涤工序。并且，阳极洗涤工序是通过将表面附着有铅物质的铜箔制造用阳极放入清洗液来进行洗涤，由此进行EDTA-Pb螯合。如此操作而使铅物质移动至清洗液中后，对去除了铅物质的铜箔制造用阳极进行喷水洗涤。
另外，根据本发明的其他实施例，可以进一步包括对完成上述阳极洗涤工序的EDTA水溶液进行电解，由此通过阴极来回收铅物质的工序。
发明效果
根据如上所述的从本发明的铜箔制造用阳极将铅物质去除的方法，可以期待能够简便且有效去除附着于阳极的铅物质的优势。这实际意味着，通过本发明的方法，能够使铜箔制造用阳极再生至可以进行正常的反应的状态。
并且，根据本发明的其他实施例，通过对去除了铅物质的水溶液再次回收铅成分，可以期待能够再利用昂贵的EDTA水溶液的经济方面的优势。这里，关于清洗液所包含的铅成分的回收，通过电解过程利用阴极来进行回收是有效且优选的。
附图说明
图1是基于现有专利文献的电解铜箔制造装置的例示图。
图2是示出本发明的电解铜箔制造方法的流程图。
符号说明
10.....电解槽
12.....电解液
20.....不溶性阳极
30.....转鼓形阴极
具体实施方式
以下，参照附图中图示的实施例来进一步详细说明本发明。
本发明的铅物质去除方法由准备清洗液的工序S10开始。本发明所使用的清洗液用于去除附着于电解铜箔用阳极的表面的铅物质，利用乙二胺四乙酸(EDTA；Ethylenediaminetetraacetic acid)和柠檬酸(citric acid)水溶液。
本发明中所使用的EDTA是EDTA-4N，以便充分确保水溶性。并且，将EDTA-4N与柠檬酸一起溶于水中来制作清洗液，这样包含的柠檬酸是为了调节清洗液的pH而使用的。即，本发明的清洗液通过将EDTA-4N和柠檬酸溶于水中准备，此时，通过调节柠檬酸的量来使清洗液的pH浓度成为7～9的范围。
如此，将清洗液的pH值尽可能调节成弱碱性是为了使EDTA与金属阳离子能够有效反应。这里，如果pH浓度高于上述范围，则EDTA络合物不稳定，OH-与EDTA竞争，或者沉淀为金属氢氧化物，或者形成没有反应性的络合物，因此不佳。另外，如果pH浓度低于上述范围，则水溶性低的EDTA会被浸出，因此不佳。
可以得出，如上说明的清洗液是包含EDTA-4N和柠檬酸的水，pH浓度处于7-9的范围。如果这样的清洗液的准备S10结束，则之后进行清洗铜箔制造用阳极的电极洗涤工序S12。这样的洗涤工序S12意味着，将铜箔制造用阳极浸渍于上述清洗液中进行洗涤。
当将铜箔制造用阳极浸渍于上述清洗液中时，进行从EDTA-4N转变为EDTA-Pb的螯合。即，曾附着于铜箔制造用阳极的表面的铅物质(Lead materials)中的铅成分在清洗液中发生与EDTA暂时结合的螯合。可以认为这一工序实质上会将铜箔制造用阳极的铅物质从阳极去除。
其中，反应式可以由C10H12N2Na4O8.4H2O+PbO2→EDTA-Pb表示，产物为碱性状态，且螯合成H2EDTA形态，溶解存在于清洗液中。另外，在这样的清洗工序中，清洗液优选维持上述pH浓度，温度维持20～50℃。另外，在清洗工序中，这样的温度范围考虑了上述反应的效率性和形成温水时的便利性。
如果这样的阳极洗涤工序S12结束，则可知是实质上从铜箔制造用阳极去除了铅物质的状态。也即，是铜箔制造用阳极的铅物质被分离，在清洗液中以EDTA-Pb的形态存在的状态。另外，铜箔制造用阳极由于是实质上去除了铅物质的状态，因此可以认为是经由洗涤步骤而能够进行再利用的状态。
这里，作为清洗液的EDTA溶液中存在有铅物质，因此为了再利用昂贵的EDTA溶液，需要去除溶液中的铅物质。如此，为了去除清洗液中的铅物质，进行电解反应工序S14。即，如果使呈EDTA-Pb螯合状态的洗涤液在电解槽中发生电解反应，则这样的电解反应结果铅物质可以通过在阴极上镀覆来回收。这里，无需限定电解槽的形态和构成，且优选由多级阳极和阴极构成。
如此，通过电解反应来使铅物质附着于阴极实质上是从作为清洗液的EDTA溶液中去除铅物质。如果铅物质被这样去除，则能够将昂贵的EDTA溶液再次用作清洗液，因此经济性上必定具备相当大的优势。因此，可知电解反应工序S14实质上是将含有EDTA的清洗液再生的工序。
另外，通过阳极水洗工序S12而去除了铅物质的电解铜箔制造用阳极在水洗工序S16中用高压洗涤机进行洗涤，由此被完全再生。对于本领域的一般技术人员而言显而易见的是，这样的后处理并非限定于用高压洗涤机进行洗涤，能够利用多种多样的方法来进行洗涤。
认为，在如上说明的本发明的基本技术思想范畴内，本领域的一般技术人员能够进行多种多样的变形。并且可以说，本发明的保护范围应当根据专利法的法规宗旨以权利要求书所记载的范围来解释。
Claims (2)
1.一种从铜箔制造用阳极去除铅物质的方法，其特征在于，是去除附着于铜箔制造用阳极(20)的表面的铅物质的方法，所述铜箔制造用阳极(20)具有与用于形成铜箔的转鼓形阴极(30)相对应的凹面形状，所述方法包括：
清洗液准备工序，准备包含EDTA和柠檬酸水溶液的清洗液；
阳极洗涤工序，将表面附着有铅物质的铜箔制造用阳极放入清洗液中，由此进行EDTA-Pb螯合；以及
水洗工序，用高压洗涤机对去除了铅物质的铜箔制造用阳极进行洗涤，
所述清洗液具有7～9的pH浓度和20～50℃的温度范围。
2.根据权利要求1所述的从铜箔制造用阳极去除铅物质的方法，进一步包括：将完成所述阳极洗涤工序的EDTA水溶液进行电解，由此通过阴极来回收铅物质的工序。
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| KR1020220138158A KR20240057678A (ko) | 2022-10-25 | 2022-10-25 | 동박 제조용 양극 재생을 위한 리드물질 제거방법 |
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| US (1) | US20240133067A1 (zh) |
| EP (1) | EP4361315A1 (zh) |
| JP (1) | JP2024062918A (zh) |
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| GB1076979A (en) * | 1963-08-13 | 1967-07-26 | William Russell Tedeschi | Surface treating composition |
| US20080115810A1 (en) * | 2006-11-20 | 2008-05-22 | Permelec Electrode Ltd. | Method of reactivating electrode for electrolysis |
| CA3121766C (en) * | 2014-11-18 | 2023-09-26 | Aqua Metals Inc. | Improved devices and method for smelterless recycling of lead acid batteries |
| JP6946911B2 (ja) | 2017-09-29 | 2021-10-13 | 株式会社大阪ソーダ | めっき用電極および電解金属箔の製造装置 |
| CN114990531B (zh) * | 2022-06-28 | 2022-12-13 | 西安泰金工业电化学技术有限公司 | 一种电解铜箔用钛阳极的清洗及再生修复方法 |
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| US20240133067A1 (en) | 2024-04-25 |
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| KR20240057678A (ko) | 2024-05-03 |
| JP2024062918A (ja) | 2024-05-10 |
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