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CN111617779A - 一种紫外光辐射分解钴电解液中的铜制备Cu2S光催化剂的方法 - Google Patents

一种紫外光辐射分解钴电解液中的铜制备Cu2S光催化剂的方法 Download PDF

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CN111617779A
CN111617779A CN202010695276.1A CN202010695276A CN111617779A CN 111617779 A CN111617779 A CN 111617779A CN 202010695276 A CN202010695276 A CN 202010695276A CN 111617779 A CN111617779 A CN 111617779A
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copper
photocatalyst
cobalt
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韩超
王广欣
唐坤
程楚
徐盼盼
刘海洋
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Henan University of Science and Technology
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    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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Abstract

本发明公开了一种紫外光辐射分解钴电解液制备Cu2S光催化剂的方法，采用硫代硫酸盐预处理方法得到铜硫代硫酸盐络合物，而后通过紫外光辐射分解制备Cu2S光催化剂的方法，既解决了电解精炼过程中电解液中铜去除的问题，又实现了铜组分的高值化利用，体现了“高效、协调、环保”等特点。

Description

一种紫外光辐射分解钴电解液中的铜制备Cu2S光催化剂的 方法
技术领域
本发明涉及冶金行业电解精炼芯片级高纯钴制备领域，具体为一种紫外光辐射分解钴电解液中的铜制备Cu2S光催化剂的方法。
背景技术
钴是重要的高纯金属材料之一，是制备磁记录介质、磁记录磁头、光电器件和磁传感器和集成电路等元器件的重要材料。大多应用都是将钴制备成纯金属靶材或合金靶材，通过镀膜方式得到符合要求的功能薄膜。
5N及以上纯度的高纯钴则主要用来制造超大规模集成电路行业用溅射靶材。目前限于技术原因，5N及以上高纯钴需要大量进口，因而开发具有自主知识产权的高纯钴制备技术尤为重要。
钴溶液的净化阶段多采用溶剂萃取、萃取色层法、膜分离、离子交换、电解等方式，其目的主要是为了除去钴溶液中的金属杂质(如Fe3+、Ni2+、Cu2+、Zn2+等)，经过除杂之后的钴溶液再通过电解的方法得到金属钴。
专利CN201610786224.9公开了一种用离子交换树脂从钴电解液中深度除铜的方法采用螯合型离子交换树脂动态、静态吸附钴电解液中的铜离子，该方法该方法所使用的树脂价格昂贵，极大的增加了生产成本，并且该种树脂在国内很难买到，货期较长。
专利CN200410056895.7公开了一种钴电解液的除铜方法将硫代硫酸钴加入电解液中，经化学反应生成极难溶解的CuS沉淀，过滤分离除铜，该方法分离出硫化物常常需要加凝絮剂增加沉淀效果，不仅费用较高，分离出来的CuS常带有其他金属离子而难以直接用于铜相关领域的加工。
发明内容
本发明目的在于提供一种紫外光辐射分解钴电解液制备Cu2S光催化剂的方法，采用硫代硫酸盐预处理方法得到铜硫代硫酸盐络合物，而后通过紫外光辐射分解制备Cu2S光催化剂的方法，既解决了电解精炼过程中电解液中铜去除的问题，又实现了铜组分的高值化利用，体现了“高效、协调、环保”等特点。
为实现上述目的，本发明提供如下技术方案：
一种紫外光辐射分解钴电解液中的铜制备Cu2S光催化剂的方法，其特征在于，包括以下步骤：
步骤一：向钴电解液中加入硫代硫酸钠，按照Cu2+/S2O3 2-摩尔比为1:10的比例络合钴电解液中的铜组分，将溶液PH调整为6；
步骤二：将步骤一得到的溶液置于常温下，经由波长254nm的紫外光辐射4h，使得Cu+-S2O3 2-络合物发生分解；
步骤三：将步骤二得到的辐射过后的溶液进行过滤，得到组分为Cu2S粉体、粒径为微纳米级、具备光催化性能的产物；
作为本发明的一种优选技术方案，所述步骤三中得到组分为Cu2S粉体、粒径为微纳米级、具备光催化性能的产物可应用于有机物降解或是分解水制氢等领域。
与现有技术相比，本发明的有益效果是：硫代硫酸盐可以极大的去除钴电解液中的铜离子，得到的沉淀物经过245nm的紫外光辐射，可以得到纯度较高的Cu2S粉体用于有机物降解或者分解水制氢气等领域。
附图说明
图1为铜硫代硫酸盐络合物的吸收光谱；
图2为紫外光分解产物的粒度分析；
图3为紫外光分解产物的X光电子能谱；
具体实施方式
一种紫外光辐射分解钴电解液中的铜制备Cu2S光催化剂的方法，其特征在于，包括以下步骤：
步骤一：向钴电解液中加入硫代硫酸钠，按照Cu2+/S2O3 2-摩尔比为1:10的比例络合钴电解液中的铜组分，将溶液PH调整为6；
步骤二：将步骤一得到的溶液置于常温下，经由波长254nm的紫外光辐射4h，使得Cu+-S2O3 2-络合物发生分解；
步骤三：将步骤二得到的辐射过后的溶液进行过滤，得到组分为Cu2S粉体、粒径为微纳米级、具备光催化性能的产物；
作为本发明的一种优选技术方案，所述步骤三中得到组分为Cu2S粉体、粒径为微纳米级、具备光催化性能的产物可应用于有机物降解或是分解水制氢等领域。
实施例1
向钴电解液中添加硫代硫酸钠，调整溶液PH为6，铜浓度为50mg/L、硫代硫酸钠浓度为0.1mol/L，经紫外光(254nm)4h的照射，最终配合物分解率能达到84％，解产物通过XRD、XPS等一系列检测方法进行表征，结果表明产物中主要是硫化亚铜。
上述实施例均为本发明较佳实例，凡是依据本发明的技术实质对以上实施所做的任何简单修饰、等同变化与修饰、均落入本发明的保护范围内。

Claims (2)

1.一种紫外光辐射分解钴电解液中的铜制备Cu2S光催化剂的方法，其特征在于，包括以下步骤：
步骤一：向钴电解液中加入硫代硫酸钠，按照Cu2+/S2O3 2-摩尔比为1:10的比例络合钴电解液中的铜组分；
步骤二：将步骤一得到的溶液置于常温下，经由波长254nm的紫外光辐射4h，使得Cu+-S2O3 2-络合物发生分解；
步骤三：将步骤二得到的辐射过后的溶液进行过滤，得到组分为Cu2S粉体、粒径为微纳米级、具备光催化性能的产物。
2.根据权利要求1中所述的紫外光辐射分解钴电解液中的铜制备Cu2S光催化剂的方法，其特征在于：步骤三中得到组分为Cu2S粉体、粒径为微纳米级、具备光催化性能的产物可应用于有机物降解或是分解水制氢等领域。
CN202010695276.1A 2020-07-19 2020-07-19 一种紫外光辐射分解钴电解液中的铜制备Cu2S光催化剂的方法 Pending CN111617779A (zh)

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CN104795468A (zh) * 2015-04-20 2015-07-22 岭南师范学院 一种铜锌锡硫薄膜的光化学制备方法及其铜锌锡硫薄膜与铜锌锡硫太阳能电池
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* Cited by examiner, † Cited by third party
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US4088552A (en) * 1976-04-19 1978-05-09 Eastman Kodak Company Recovering silver compounds from solutions containing other silver compounds
CN1598013A (zh) * 2004-08-30 2005-03-23 金川集团有限公司 一种钴电解液的除铜方法
US20130091990A1 (en) * 2011-06-15 2013-04-18 Barrick Gold Corporation Method for recovering precious metals and copper from leach solutions
CN103752329A (zh) * 2014-01-09 2014-04-30 华南师范大学 一种CuS光催化剂的光化学制备方法
CN104795468A (zh) * 2015-04-20 2015-07-22 岭南师范学院 一种铜锌锡硫薄膜的光化学制备方法及其铜锌锡硫薄膜与铜锌锡硫太阳能电池
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