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 PDFInfo
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- 239000010949 copper Substances 0.000 title claims abstract description 39
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 29
- 239000010941 cobalt Substances 0.000 title claims abstract description 29
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000003792 electrolyte Substances 0.000 title claims abstract description 23
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 19
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 11
- 230000005855 radiation Effects 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 7
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 5
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 5
- DHCDFWKWKRSZHF-UHFFFAOYSA-L thiosulfate(2-) Chemical compound [O-]S([S-])(=O)=O DHCDFWKWKRSZHF-UHFFFAOYSA-L 0.000 claims description 5
- 230000015556 catabolic process Effects 0.000 claims description 4
- 238000006731 degradation reaction Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000005416 organic matter Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- ANVWDQSUFNXVLB-UHFFFAOYSA-L copper;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [Cu+2].[O-]S([O-])(=O)=S ANVWDQSUFNXVLB-UHFFFAOYSA-L 0.000 abstract description 3
- 238000007670 refining Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- JUDQOQFKZHGHGW-UHFFFAOYSA-L cobalt(2+);dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [Co+2].[O-]S([O-])(=O)=S JUDQOQFKZHGHGW-UHFFFAOYSA-L 0.000 description 1
- AQMRBJNRFUQADD-UHFFFAOYSA-N copper(I) sulfide Chemical compound [S-2].[Cu+].[Cu+] AQMRBJNRFUQADD-UHFFFAOYSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 238000002186 photoelectron spectrum Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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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
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。
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| 杨艺超 等: "紫外光分解银硫代硫酸盐络合物的研究", 《四川冶金》 * |
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