CN105923966A - 一种从电镀污泥中浸出镍铜硫的方法 - Google Patents
一种从电镀污泥中浸出镍铜硫的方法 Download PDFInfo
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- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 34
- 239000010802 sludge Substances 0.000 title claims abstract description 33
- 238000002386 leaching Methods 0.000 title claims abstract description 32
- 238000009713 electroplating Methods 0.000 title claims abstract description 31
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000011593 sulfur Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title abstract description 61
- 229910052802 copper Inorganic materials 0.000 title abstract description 33
- 239000010949 copper Substances 0.000 title abstract description 33
- 229910052759 nickel Inorganic materials 0.000 title abstract description 30
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 35
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 22
- 239000001301 oxygen Substances 0.000 claims abstract description 22
- 229920001732 Lignosulfonate Polymers 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims description 21
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 abstract 1
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 229910001882 dioxygen Inorganic materials 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 238000001035 drying Methods 0.000 description 8
- 229910001453 nickel ion Inorganic materials 0.000 description 8
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 7
- 229910001431 copper ion Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000002893 slag Substances 0.000 description 7
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 229910052793 cadmium Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 241000605272 Acidithiobacillus thiooxidans Species 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- 241000158728 Meliaceae Species 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- BWFPGXWASODCHM-UHFFFAOYSA-N copper monosulfide Chemical class [Cu]=S BWFPGXWASODCHM-UHFFFAOYSA-N 0.000 description 1
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010801 sewage sludge Substances 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/06—Treatment of sludge; Devices therefor by oxidation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/10—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/004—Sludge detoxification
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- 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
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- 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
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- 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
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- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C02F2303/06—Sludge reduction, e.g. by lysis
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Abstract
一种从电镀污泥中浸出镍铜硫的方法，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0.6~1.1MPa，浸出温度130~160℃，浸出液pH控制在0.45以下，浸出时间1~5h，浸出结束后，过滤分离得到浸出液和尾渣，浸出液提取镍和铜,浸出渣堆存。本发明方法能一步实现镍、铜和硫等元素的浸出及尾渣减量化，具有操作简单，化学试剂消耗少，镍、铜和硫等元素浸出率高，渣率低等优点。
Description
技术领域
本发明涉及一种从电镀污泥中浸出镍铜硫的方法。
技术背景
电镀污泥是一种典型的危险废物，含有铜、镍、铁、锌等重金属及氰化物等易于引起二次污染，具有存量大、污染性强等特点，同时也是重要的二次有价金属资源。
电镀重金属污泥的资源化利用一直是国内外的研究热点，但由于电镀污泥来源复杂，重金属含量及存在形式有所不同，成分差异较大，给电镀污泥的综合处理增加了技术难度。目前，电镀污泥的处理工艺主要有简单填埋法，焚火法焚烧及湿法冶金等。郑顺（氯盐体系电镀污泥中有价金属选择性提取工艺研究，学位论文，江西理工大学，2014）采用选择性氯化工艺对电镀污泥氯化焙烧，焙烧料弱酸浸出后逐级分离除杂，达到富集有价金属镍的目的。李淑更（微生物淋滤法去除城市污泥中重金属的效果,《生态环境学报》,Vol.18,No.1,P111-115,2009）等以城市污泥作为培养介质，以硫代硫酸钠为生长基质，氧化亚铁硫杆菌和氧化硫硫杆菌淋滤去除污泥中重金属，污泥中铜、锌、镉、镍的去除率分别为67.2%、88.9%、82.4%和68.4%。该生物技术具有环保优势，但其周期长、主要元素去除率有待提高。这些方法没有有效利用电镀污泥中的硫元素，铜镍浸出率低，造成浸出渣产率大，堆存麻烦。
发明内容
本发明旨在提供一种从电镀污泥中浸出镍铜硫的方法，采用加热氧化，浸出铜、镍和硫等元素，达到有效利用和尾渣减量化的目的。
本发明所述电镀污泥中含镍2~30%wt，铜0.2~25%wt，硫3~30%wt，铁0.5~20%wt，镍、铜和铁以硫化物形式存在。
本发明所述的从电镀污泥中浸出镍铜硫的方法步骤如下：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0.6~1.1MPa，浸出温度130~160℃，浸出液pH控制在0.45以下，浸出时间1~5h，浸出结束后，过滤分离得到浸出液和尾渣，浸出液提取镍铜，浸出渣堆存。
所述硫酸溶液的浓度为90~250g/L。
浸出液为含镍、铜等的硫酸溶液，主要反应方程式为：
MeS + 2O2 = MeSO4 (Me表示Cu，Ni或Fe等)。
本发明采用氧气作为氧化剂，在加热下将镍、铜等硫化物溶解，并将硫转化为硫酸根。本发明方法能一步实现镍、铜和硫等元素的浸出及尾渣减量化。具有操作简单，化学试剂消耗少，镍、铜和硫等元素浸出率高，渣率低等优点。
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300g与浓度90g/L H2SO4的硫酸溶液1500g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160℃，浸出液pH控制在0.3，浸出时间5h，浸出结束后，过滤分离得到浸出液及尾渣；尾渣烘干后28.29g，经分析，尾渣的产率为9.43%，其中Fe 2.09%、Ni 0.68%、Cu 0.081%、S 1.52%，计算可知，镍、铜和硫浸出率均在99%以上，铁浸出率大于95%。浸出液共计2L，其中镍离子浓度21.11g/L、铜离子浓度1.49g/L。
实施例2
物料成分与实施例1相同。
将电镀污泥300g与浓度为250g/L H2SO4的硫酸溶液650g加入反应釜中，加入1.5g木质素磺酸盐，通过工业氧气，保持釜内氧分压0.7MPa，浸出温度160℃，浸出液pH控制在0.4，浸出时间1h，浸出结束后，过滤分离得到浸出液及尾渣，尾渣烘干后24.41g，经分析，尾渣的产率为8.14%，其中Fe 0.72 %、Ni 0.48%、Cu 0.044 %、S 0.78%，计算可知，镍、铜和硫浸出率均在99%以上，铁浸出率98%以上。浸出液共计1L，其中镍离子浓度为36.46g/L、铜离子浓度为2.99g/L。
实施例3
物料成分与实施例1相同。
将电镀污泥300g与浓度为200g/L H2SO4的硫酸溶液850g加入反应釜中，加入1.5g木质素磺酸盐，通过工业氧气，保持釜内氧分压0.9MPa，浸出温度150℃，浸出液pH控制在0.3，浸出时间3h，浸出结束后，过滤分离得到浸出液及尾渣，尾渣烘干后18.76g，经分析，尾渣的产率为6.25%，其中Fe 1.02%、Ni 0.25%、Cu 0.033%、S 1.21%，计算可知，镍、铜和硫浸出率均在99%以上，铁浸出率98%以上。浸出液共计2L，其中镍离子浓度为21.19g/L、铜离子浓度为1.20g/L。
实施例4
物料成分与实施例1相同。
将电镀污泥300g与浓度为90g/L H2SO4的硫酸溶液1350g加入反应釜中，加入1.2g木质素磺酸盐，通过工业氧气，保持釜内氧分压1.1MPa，浸出温度160℃，浸出液pH控制在0.2，浸出时间5h，浸出结束后，过滤分离得到浸出液及尾渣，尾渣烘干后8.63g，经分析，尾渣的产率为2.88%，其中Fe 2.24%、Ni 0.72%、Cu 0.075%、S 2.37%，计算可知，镍、铜和硫浸出率均在99%以上，铁浸出率98%以上。浸出液共计2L，其中镍离子浓度为21.18g/L、铜离子浓度为1.20g/L。
实施例5
电镀污泥成分：Ni 10.38%、Cu 0.76%、Zn 8.24%、Co 0.27%、Fe 8.33%、Mg 0.09%、Mn0.03%、Al 0.08%、Cd 0.07%、S 22.43%。
将电镀污泥300g与浓度为98g/L H2SO4的硫酸溶液1350g加入反应釜中，加入1.0g木质素磺酸盐，通过工业氧气，保持釜内氧分压为1.1MPa，浸出温度为160℃，浸出液pH控制在0，浸出时间4h，浸出结束后，过滤分离得到浸出液及尾渣，尾渣烘干后18.09g，经分析，尾渣的产率为6.03%，其中Fe 1.13%、Ni 0.27%、Cu 0.041%、S 2.02%，计算可知，镍、铜、硫和铁浸出率均在99%以上。浸出液共计2L，其中镍离子浓度为15.55g/L、铜离子浓度为1.14g/L。
实施例6
物料成分与实施例5相同。
将电镀污泥300g与浓度为150g/L H2SO4的硫酸溶液1000g加入反应釜中，加入1.0g木质素磺酸盐，通过工业氧气，保持釜内氧分压0.7MPa，浸出温度140℃，浸出液pH控制在0.3，浸出时间4h，浸出结束后，过滤分离得到浸出液及尾渣，尾渣烘干后17.0g，经分析，尾渣的产率为5.67%，其中Fe 0.98 %、Ni 0.19 %、Cu 0.037%、S 1.88 %，计算可知，镍、铜、硫和铁浸出率均在99%以上。浸出液共计2L，其中镍离子浓度为15.55g/L、铜离子浓度为1.14g/L。
实施例7
物料成分与实施例5相同。
将电镀污泥300g与浓度为150g/L H2SO4的硫酸溶液650g加入反应釜中，加入0.6g木质素磺酸盐，通过工业氧气，保持釜内氧分压0.7MPa，浸出温度130℃，浸出液pH控制在0.2，浸出时间5h，浸出结束后，过滤分离得到浸出液及尾渣，尾渣烘干后22.76g，经分析，尾渣的产率为7.56%，其中Fe 1.34%、Ni 0.31%、Cu 0.045%、S 1.93%，计算可知，镍、铜和硫浸出率均在99%以上，铁浸出率98%以上。浸出液共计2L，其中镍离子浓度为15.53g/L、铜离子浓度为1.13/L。
实施例8
物料成分与实施例5相同。
将电镀污泥300g与浓度为198g/L H2SO4的硫酸溶液900g加入反应釜中，加入1.5g木质素磺酸盐，通过工业氧气，保持釜内氧分压0.7MPa，浸出温度150℃，浸出液pH控制在0.4，浸出时间3h，浸出结束后，过滤分离得到浸出液及尾渣，尾渣烘干后为18.42g，经分析，尾渣的产率为6.14%，其中Fe 1.18 %、Ni 0.53%、Cu 0.048%、S 1.97%，计算可知，镍、铜、硫、铁浸出率均在99%以上。浸出液共计2L，其中镍离子浓度为15.52g/L、铜离子浓度为1.14g/L。
Claims (2)
1.一种从电镀污泥中浸出镍铜硫的方法，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0.6~1.1MPa，浸出温度130~160℃，浸出液pH控制在0.45以下，浸出时间1~5h，浸出结束后，过滤分离得到浸出液和尾渣，浸出液提取镍铜，浸出渣堆存。
2.根据权利要求1从电镀污泥中浸出镍铜硫的方法，其特征是所述硫酸溶液的浓度为90~250g/L。
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