CN105779773B - 一种从电镀污泥中分离镍铜铁的方法 - Google Patents
一种从电镀污泥中分离镍铜铁的方法 Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000009713 electroplating Methods 0.000 title claims abstract description 39
- 239000010802 sludge Substances 0.000 title claims abstract description 38
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 10
- 239000000956 alloy Substances 0.000 title claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000010949 copper Substances 0.000 claims abstract description 28
- 229910052802 copper Inorganic materials 0.000 claims abstract description 27
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 229920001732 Lignosulfonate Polymers 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 229910000570 Cupronickel Inorganic materials 0.000 claims abstract description 4
- 239000000284 extract Substances 0.000 claims abstract 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 239000005864 Sulphur Substances 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 47
- 238000002386 leaching Methods 0.000 abstract description 34
- 229910052759 nickel Inorganic materials 0.000 abstract description 23
- 230000000694 effects Effects 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 description 7
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 5
- 229910001431 copper ion Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910001453 nickel ion Inorganic materials 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 4
- 229920005610 lignin Polymers 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 241000605222 Acidithiobacillus ferrooxidans Species 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- QNCDBCXTXVGGRH-UHFFFAOYSA-N O.O.[O-2].[Fe+2] Chemical compound O.O.[O-2].[Fe+2] QNCDBCXTXVGGRH-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- DPSZMPUXFZOWAC-UHFFFAOYSA-N [S].S=O Chemical compound [S].S=O DPSZMPUXFZOWAC-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 231100000611 venom Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
-
- 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
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- Organic Chemistry (AREA)
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Abstract
一种从电镀污泥中分离镍铜铁的方法。其特征是步骤如下：按电镀污泥:硫酸溶液:木质素磺酸盐质量比1:2~5:0.002~0.005，在电镀污泥中加入硫酸溶液和木质素磺酸盐，通入氧气，在氧分压为0.3~0.7MPa，浸出温度100~150℃，浸出液pH控制在0.5~1.5，浸出时间1~5h，浸出结束后，过滤分离得到浸出液和浸出渣，浸出液提取铜镍，浸出渣堆存。本发明的方法操作简单，能一步实现铜、镍等元素选择性浸出和分离铁的目的。铜、镍等元素浸出率高，分解效果好。本发明的方法适用于电镀污泥的处理利用。
Description
技术领域
本发明涉及一种从电镀污泥中分离镍铜铁的方法。
技术背景
电镀污泥是一种含有铜、镍、铁、钴、锌等重金属、元素硫及氰化物等的有毒有害物质，是一种典型的危险废物，具有存量大、污染严重的城市固体污染废物，同时也是重要的有价资源。
电镀污泥的资源化利用一直是国内外的研究热点，但电镀行业种类繁多，所产生的电镀污泥成分复杂、重金属含量及存在形式有所不同，电镀污泥综合处理技术难度大。目前，电镀污泥的处理主要有简单填埋，焚火法焚烧，电动修复，氧化亚铁硫杆菌或氧化硫硫杆菌的生物技术，利用磷酸、双氧水、硫酸溶液脱除重金属的化学处理及离子交换技术等。
陈凡植等（从铜镍电镀污泥中回收金属铜和硫酸镍,《化学工程》,Vol.29,No.4,P28-33,2001）通过常温硫酸浸出-铁屑置换-多步沉淀净化工艺得到铜粉和工业纯的硫酸镍。程洁红等（氨浸-加压氢还原法回收电镀污泥中的铜和镍,《环境科学与技术》,Vol.33,No.6E,P135-138,2010）以电镀废水处理过程中的电镀污泥为原料，采用氨浸-加压氢还原法从电镀污泥中分离铜、镍，镍、铜、锌，浸出率分别为80.25%、77.42%和91.07%，并制取金属铜粉和镍粉，但铜、镍浸出率还有待提高。
发明内容
本发明的目的旨在提供一种从电镀污泥中分离镍铜铁的方法。采用一步浸出将电镀污泥中的有价金属如铜、镍等有价元素选择性浸出，进入溶液，铁留在浸出渣中，达到分离铜、镍和铁等元素的目的。
本发明所述电镀污泥中含镍为2~20%wt，铜为0.2~20%wt，硫为3~25%wt，铁为0.5~15%wt，镍铜铁以硫化物形式存在。
本发明所述的从电镀污泥中分离镍、铜和铁的方法步骤如下：按电镀污泥:硫酸溶液:木质素磺酸盐质量比1:2~5:0.002~0.005，在电镀污泥中加入硫酸溶液和木质素磺酸盐，通入氧气，在氧分压0.3~0.7MPa，浸出温度100~150℃，浸出液pH控制在0.5~1.5，浸出时间1~5h，浸出结束后，过滤分离得到浸出液和浸出渣，浸出液提取铜镍，浸出渣堆存。
所述硫酸溶液的浓度为90~250g/L。
浸出液为含铜和镍等的硫酸溶液，浸出渣主要为含铁和硫的不溶物。主要反应方程式为：
MeS + Fe2(SO4)3 = MeSO4 + 2FeSO4 + S(Me表示Cu，Ni或Fe)
2FeSO4 + H2SO4 + 1/2O2 = Fe2(SO4)3 + H2O
Fe2(SO4)3 + 3H2O = Fe2O3 + 3H2SO4
本发明采用氧气作为氧化剂，在加热下将镍铜硫化物溶解，同时将硫酸铁转化为氧化铁。该方法操作简单，能一步实现铜、镍等有价元素选择性浸出，同时分离铁的目，解决了浸出液中除铁难，消耗化学试剂等问题。铜、镍等有价元素浸出率高分解效果好，浸出渣过滤性好。本发明的方法适用于电镀污泥的处理利用。
具体实施方式
实施例1
电镀污泥成分：Ni 14.14%、Cu 1.0%、Zn 9.09%、Co 0.24%、Fe 5.21%、Mg 0.09%、Mn0.03%、Al 0.08%、Cd 0.07%、S 23.86%。
将电镀污泥500g与浓度90g/L的硫酸溶液2500g加入反应釜中，加入0.6g木质素磺酸盐，通入工业氧气，保持釜内氧分压0.7MPa，浸出温度150℃，浸出液pH控制在1.5，浸出时间3h，浸出结束后，过滤分离得到浸出液及浸出渣；浸出渣烘干后为97.20g，经分析，浸出渣的产率为19.44%，其中Fe 24.99%、Ni 0.47%、Cu 0.054%、S 68.21%，计算可知，镍和铜浸出率大于98%，铁浸出率25.94%，硫浸出率44.43%。浸出液共计４L，其中镍离子浓度17.56g/L、铜离子浓度1.24g/L。
实施例2
电镀污泥成分与实施例1相同。
将电镀污泥500g与浓度250g/L的硫酸溶液1250g加入反应釜中，加入1.5g木质素磺酸盐，通入工业氧气，保持釜内氧分压0.3MPa，浸出温度150℃，浸出液pH控制在1.4，浸出时间1h，浸出结束后，过滤分离得到浸出液及浸出渣；浸出渣烘干后为157.85g，经分析，浸出渣的产率为31.57%，其中Fe 13.52%、Ni 0.53%、Cu 0.048%、S 56.99%，计算可知，镍和铜浸出率大于98%，铁浸出率18.08%，硫浸出率24.59%。浸出液共计3L，其中镍离子浓度23.29g/L、铜离子浓度1.64g/L。
实施例3
电镀污泥成分与实施例1相同。
将电镀污泥500g与浓度220g/L的硫酸溶液1500g加入反应釜中，加入1.2g木质素磺酸盐，通入工业氧气，保持釜内氧分压0.4MPa，浸出温度110℃，浸出液pH控制在1.0，浸出时间5h，浸出结束后，过滤分离得到浸出液及浸出渣；浸出渣烘干后为134.40g。经分析，浸出渣的产率为26.88%，其中Fe 17.09%、Ni 0.42%、Cu 0.044%、S 61.03%，计算可知，镍和铜浸出率为98%，铁浸出率11.83%，硫浸出率31.25%。浸出液共计3L，其中镍离子浓度23.37g/L、铜离子浓度1.65g/L。
实施例4
电镀污泥成分与实施例1相同。
将电镀污泥500g与浓度90g/L的硫酸溶液2500g加入反应釜中，加入0.6g木质素磺酸盐，通入工业氧气，保持釜内氧分压0.5MPa，浸出温度150℃，浸出液pH控制在1.5，浸出时间5h，浸出结束后，过滤分离得到浸出液及浸出渣；浸出渣烘干后为124.90g。经分析，浸出渣的产率为24.98%，其中Fe 17.63%、Ni 0.58%、Cu 0.052%、S 67.34%，计算可知，镍和铜浸出率大于98%，铁浸出率15.47%，硫浸出率29.50%。浸出液共计4L，其中镍离子浓度17.49g/L、铜离子浓度1.23g/L。
实施例5
电镀污泥成分与实施例1相同。
将电镀污泥500g与浓度240g/L的硫酸溶液2000g加入反应釜中，加入1.5g木质素磺酸盐，通入工业氧气，保持釜内氧分压0.7MPa，浸出温度100℃，浸出液pH控制在0.5，浸出时间5h，浸出结束后，过滤分离得到浸出液及浸出渣；浸出渣烘干后为144.70g。经分析，浸出渣的产率为为28.94%，其中Fe 16.27%、Ni 0.37%、Cu 0.041%、S 52.39%，计算可知，镍和铜浸出率大于98%，铁浸出率9.62%，硫浸出率36.46%。浸出液共计3L，其中镍离子浓度23.39g/L、铜离子浓度1.65g/L。
Claims (2)
1.一种从电镀污泥中分离镍铜铁的方法，所述电镀污泥中含镍为2～20％wt，铜为0.2～20％wt，硫为3～25％wt，铁为0.5～15％wt，镍铜铁以硫化物形式存在,其特征是步骤如下：按电镀污泥:硫酸溶液:木质素磺酸盐质量比1:2～5:0.002～0.005，在电镀污泥中加入硫酸溶液和木质素磺酸盐，通入氧气，在氧分压0.3～0.7MPa，浸出温度100～150℃，浸出液pH控制在0.5～1.5，浸出时间为1～5h，浸出结束后，过滤分离得到浸出液和浸出渣，浸出液提取铜镍,浸出渣堆存。
2.根据权利要求1所述的从电镀污泥中分离镍铜铁的方法，其特征是所述硫酸溶液的浓度为90～250g/L。
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| CN102758091A (zh) * | 2012-07-18 | 2012-10-31 | 中国瑞林工程技术有限公司 | 电镀污泥的处理方法 |
| CN104232924A (zh) * | 2014-09-25 | 2014-12-24 | 河南工信华鑫环保科技有限公司 | 一种铜矿石酸浸出液的提铜除铁方法 |
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