CN113667825A - 镍铁湿法处理方法及其应用 - Google Patents
镍铁湿法处理方法及其应用 Download PDFInfo
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- CN113667825A CN113667825A CN202110818269.0A CN202110818269A CN113667825A CN 113667825 A CN113667825 A CN 113667825A CN 202110818269 A CN202110818269 A CN 202110818269A CN 113667825 A CN113667825 A CN 113667825A
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- 229910000863 Ferronickel Inorganic materials 0.000 title claims abstract description 55
- 238000003672 processing method Methods 0.000 title claims abstract description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 77
- 239000000706 filtrate Substances 0.000 claims abstract description 54
- 238000002386 leaching Methods 0.000 claims abstract description 49
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 37
- 239000002253 acid Substances 0.000 claims abstract description 29
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 230000001590 oxidative effect Effects 0.000 claims abstract description 15
- 239000007800 oxidant agent Substances 0.000 claims abstract description 13
- 230000007797 corrosion Effects 0.000 claims abstract description 12
- 238000005260 corrosion Methods 0.000 claims abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229960004887 ferric hydroxide Drugs 0.000 claims abstract description 11
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims abstract description 11
- 239000001301 oxygen Substances 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000012716 precipitator Substances 0.000 claims abstract description 3
- 239000002002 slurry Substances 0.000 claims abstract description 3
- 239000010949 copper Substances 0.000 claims description 24
- 239000002893 slag Substances 0.000 claims description 23
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 21
- 229910052802 copper Inorganic materials 0.000 claims description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 13
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 6
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000005530 etching Methods 0.000 claims description 4
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims description 3
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 2
- 238000006073 displacement reaction Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims 1
- 235000011121 sodium hydroxide Nutrition 0.000 claims 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 abstract description 19
- 238000000605 extraction Methods 0.000 abstract description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 8
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001569 carbon dioxide Substances 0.000 abstract description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 3
- 229910001447 ferric ion Inorganic materials 0.000 abstract description 3
- 229910001448 ferrous ion Inorganic materials 0.000 abstract description 3
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 8
- 239000012074 organic phase Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000011268 mixed slurry Substances 0.000 description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 5
- 229910001431 copper ion Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910000805 Pig iron Inorganic materials 0.000 description 2
- QUXFOKCUIZCKGS-UHFFFAOYSA-N bis(2,4,4-trimethylpentyl)phosphinic acid Chemical compound CC(C)(C)CC(C)CP(O)(=O)CC(C)CC(C)(C)C QUXFOKCUIZCKGS-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- -1 hydrogen ions Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910000398 iron phosphate Inorganic materials 0.000 description 2
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- KHPLPBHMTCTCHA-UHFFFAOYSA-N ammonium chlorate Chemical compound N.OCl(=O)=O KHPLPBHMTCTCHA-UHFFFAOYSA-N 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- 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
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- C22B1/00—Preliminary treatment of ores or scrap
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- C22B1/24—Binding; Briquetting ; Granulating
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
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- C22B23/043—Sulfurated acids or salts thereof
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- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
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Abstract
本发明公开了一种镍铁湿法处理方法及其应用，该处理方法是在高压氧气环境中，将镍铁粉碎料、硫酸和助蚀剂混合，进行酸浸反应，再将酸浸后浆料进行固液分离，所得滤液加入氧化剂，并加热，除去助蚀剂，再向滤液中加入沉淀剂，并控制滤液的pH，固液分离，得到氢氧化铁沉淀和含镍滤液；含镍滤液经过萃取和反萃取可以制备电池级硫酸镍。本发明通过在高压氧气及酸性条件下，配合助蚀剂，对镍铁进行氧化酸溶，在高压氧气环境中镍铁极易氧化；后续在滤液中加入强氧化剂，不仅保证了滤液中二价铁离子全部转化为三价铁离子，且可对助蚀剂进行氧化，生成无污染的二氧化碳和水，避免了助蚀剂对后续萃取工序的影响。
Description
技术领域
本发明属于冶金技术领域，具体涉及一种镍铁湿法处理方法及其应用。
背景技术
目前有关镍铁增值利用的方法还不多，相关技术公开了一种含镍生铁制备硫酸镍溶液和电池级磷酸铁的方法，包括以下步骤：原料预处理、酸浸处理、沉淀处理、磷酸铁干燥处理、含镍滤液萃取处理和反萃得到硫酸镍溶液。虽然该方法具有工艺简单、含镍生铁回收率高、成本低廉和产品性能好特点，但是在酸浸处理中存在反应慢、时间长，无法大批量应用。
发明内容
本发明旨在至少解决上述现有技术中存在的技术问题之一。为此，本发明提出一种镍铁湿法处理方法及其应用，该方法具有工艺流程短、辅料消耗量低、浸出率高等优势。
根据本发明的一个方面，提出了一种镍铁湿法处理方法，包括以下步骤：
S1：在高压氧气环境中，将镍铁粉碎料、硫酸和助蚀剂混合，进行酸浸反应；
S2：将步骤S1酸浸后浆料进行固液分离，所得滤液加入氧化剂，并加热，除去助蚀剂；
S3：再向滤液中加入沉淀剂，并控制滤液的pH，固液分离，得到氢氧化铁沉淀和含镍滤液。
在本发明的一些实施方式中，步骤S1中，所述助蚀剂为过氧化氢、乙酸、乙酰丙酮、草酸或甘氨酸中的一种或多种。助蚀剂起到加速氧化，快速腐蚀镍铁的作用。
其中，助蚀剂过氧化氢可以加快氧化浸出，助蚀剂乙酰丙酮与甘氨酸可以与镍铁络合，从而加快反应，助蚀剂草酸和乙酸，不仅具备酸性溶解的性能，还具有络合的功能，提升了整个反应的速率。
在本发明的一些实施方式中，步骤S1中，所述硫酸的浓度为3-8mol/L。
在本发明的一些实施方式中，步骤S1中，所述酸浸反应的压力为3.0-6.5MPa，反应的温度为50-90℃。
在本发明的一些实施方式中，步骤S2中，所述氧化剂为氯酸盐、亚硝酸盐、硝酸盐或过硫酸盐中的一种或多种。选择强氧化剂，可将助蚀剂氧化成二氧化碳或水，避免对后续有机萃取的干扰。
在本发明的一些实施方式中，步骤S2中，固液分离所得滤渣可返回步骤S1中继续进行酸浸反应，避免物料的浪费。
在本发明的一些实施方式中，步骤S2中，所述加热的温度为60-95℃。控制加热温度可以加快反应进度，使氧化剂氧化助蚀剂生成的二氧化碳脱出。
在本发明的一些实施方式中，步骤S3中，所述沉淀剂为氨水、氢氧化钠、碳酸钠或碳酸氢钠中的一种或多种。
在本发明的一些实施方式中，步骤S3中，所述pH为3-3.5。该pH下可使氢氧化铁完全沉淀分离，并保留镍离子。
在本发明的一些实施方式中，步骤S3中，还包括：将所述氢氧化铁沉淀经洗涤、加热后制备铁红。
在本发明的一些实施方式中，步骤S2中，所得滤液可加入镍铁进行置换还原浸出，过滤得到镍铁渣和除铜的浸出液，所述镍铁渣返回步骤S1进行酸浸，所述浸出液加入所述氧化剂进行后续处理。置换还原浸出反应在常压下即可，无需氧气参与，高压酸浸后的滤液中含有大量的氢离子、三价铁离子，还有少量铜离子，加入镍铁反应，实现二次浸出，并将铜置换出来，得到二价铁离子，再继续后续加氧化剂的操作。二次浸出主要发生置换还原反应，可以提升镍、铁离子浓度，并除去铜离子。此外，镍铁渣返回上一步酸浸会导致铜越来越多，但由于镍铁中铜含量很少，可以循环很多次，铜会逐渐积累在二次浸出的镍铁渣中，对镍铁渣检测，当铜含量较高时，采用常压酸浸，选择性的浸出镍和铁，产生的浸出液返回步骤S1高压酸浸，浸出渣送去铜厂处理。
本发明还提出所述的方法得到的含镍滤液在制备电池级硫酸镍中的应用。具体为，所述含镍滤液加入萃取剂萃取镍，静置，分离得到含镍萃取有机相和含杂质萃余液，再用3-5mol/L的H2SO4溶液从含镍萃取有机相中反萃取镍，得到电池级硫酸镍溶液。
在本发明的一些实施方式中，萃取剂选自P204、P507、DEHPA或Cyanex272中的一种或多种。
根据本发明的一种优选的实施方式，至少具有以下有益效果：
本发明通过在高压氧气及酸性条件下，配合助蚀剂，对镍铁进行氧化酸溶；在高压氧气环境中，镍铁极易氧化，并在助蚀剂的作用加快反应速率。后续在滤液中加入氯酸盐、亚硝酸盐、硝酸盐、过硫酸盐等强氧化剂，不仅保证了滤液中二价铁离子全部转化为三价铁离子，且可对助蚀剂进行氧化，生成无污染的二氧化碳和水，避免了助蚀剂对后续萃取工序的影响。整个反应过程，较为迅速，在助蚀剂和氧化剂的双重配合下，浸出效率很高，浸出率可高达97％以上，且不会释放有毒气体，避免了环境污染。
附图说明
下面结合附图和实施例对本发明做进一步的说明，其中：
图1为本发明实施例1的工艺流程图。
具体实施方式
以下将结合实施例对本发明的构思及产生的技术效果进行清楚、完整地描述，以充分地理解本发明的目的、特征和效果。显然，所描述的实施例只是本发明的一部分实施例，而不是全部实施例，基于本发明的实施例，本领域的技术人员在不付出创造性劳动的前提下所获得的其他实施例，均属于本发明保护的范围。
实施例1
一种镍铁湿法处理方法，结合图1，具体过程为：
(1)原料预处理，将镍含量为22.35％的镍铁破碎成粉状或颗粒状；
(2)一段高压酸浸，在密闭压力为6.5MPa、温度为90℃的高压氧气环境中，将步骤(1)所得粉碎料采用浓度为3mol/L的硫酸酸浸，并加入乙酸，得到混合浆料，混合浆料的固液比为1:100g/mL，反应时间3h；
(3)过滤处理，步骤(2)反应结束后，过滤得到滤液和滤渣，向滤液中加入镍铁粉碎料进行二段浸出，使滤液中少量铜离子置换出来，再次过滤得到镍铁渣和除铜的滤液，镍铁渣返回步骤(2)的一段高压酸浸，循环若干次后检测到镍铁渣的含铜量较高时，将镍铁渣进行常压浸出，产生的浸出液返回一段高压酸浸，浸出渣送去铜厂处理；
(4)沉淀处理，向步骤(3)除铜后的滤液中加入氯酸铵，对滤液中的二价铁进行氧化，并进行加热，控制加热温度为60-70℃，除去乙酸，避免干扰后续的萃取过程；
(5)控制沉淀，向步骤(4)所得滤液中继续加入氨水，并控制滤液pH为3-3.5，再次过滤，得到氢氧化铁沉淀和含镍滤液，氢氧化铁沉淀经洗涤、加热后得到铁红。
制备硫酸镍：将含镍滤液用萃取剂P507萃取镍，静置，分离得到含镍萃取有机相和含杂质萃余液；再用5mol/L的H2SO4溶液从含镍萃取有机相中反萃取镍，得到电池级硫酸镍溶液。
蒸发结晶后制得的硫酸镍晶体送化验室分析，分析结果为22.12％Ni、0.021％Co、0.00038％Cu、0.00028％Fe，符合电池级硫酸镍的产品标准。
实施例2
一种镍铁湿法处理方法，具体过程为：
(1)原料预处理，将镍含量为25.85％的镍铁破碎成粉状或颗粒状；
(2)一段高压酸浸，在密闭压力为3.0MPa、温度为50℃的高压氧气环境中，将步骤(1)所得粉碎料采用浓度为8mol/L的硫酸酸浸，并加入乙酰丙酮，得到混合浆料，混合浆料的固液比为1:200g/mL，反应时间1.5h；
(3)过滤处理，步骤(2)反应结束后，过滤得到滤液和滤渣，向滤液中加入镍铁粉碎料进行二段浸出，使滤液中少量铜离子置换出来，再次过滤得到镍铁渣和除铜的滤液，镍铁渣返回步骤(2)的一段高压酸浸，循环若干次后检测到镍铁渣的含铜量较高时，将镍铁渣进行常压浸出，产生的浸出液返回一段高压酸浸，浸出渣送去铜厂处理；
(4)沉淀处理，向步骤(3)除铜后的滤液中加入硝酸铵，对滤液中的二价铁进行氧化，并进行加热，控制加热温度为75-85℃，除去乙酰丙酮，避免干扰后续的萃取过程；
(5)控制沉淀，向步骤(4)所得滤液中继续加入氨水，并控制滤液pH为3-3.5，再次过滤，得到氢氧化铁沉淀和含镍滤液，氢氧化铁沉淀经洗涤、加热后得到铁红。
制备硫酸镍：将含镍滤液用萃取剂Cyanex272萃取镍，静置，分离得到含镍萃取有机相和含杂质萃余液；再用3mol/L的H2SO4溶液从含镍萃取有机相中反萃取镍，得到电池级硫酸镍溶液。
蒸发结晶后制得的硫酸镍晶体送化验室分析，分析结果为22.06％Ni、0.027％Co、0.00031％Cu、0.00012％Fe，符合电池级硫酸镍的产品标准。
实施例3
一种镍铁湿法处理方法，具体过程为：
(1)原料预处理，将镍含量为55.35％的镍铁破碎成粉状或颗粒状；
(2)一段高压酸浸，在密闭压力为5.0MPa、温度为70℃的高压氧气环境中，将步骤(1)所得粉碎料采用浓度为5mol/L的硫酸酸浸，并加入草酸，得到混合浆料，混合浆料的固液比为1:300g/mL，反应时间3h；
(3)过滤处理，步骤(2)反应结束后，过滤得到滤液和滤渣，向滤液中加入镍铁粉碎料进行二段浸出，使滤液中少量铜离子置换出来，再次过滤得到镍铁渣和除铜的滤液，镍铁渣返回步骤(2)的一段高压酸浸，循环若干次后检测到镍铁渣的含铜量较高时，将镍铁渣进行常压浸出，产生的浸出液返回一段高压酸浸，浸出渣送去铜厂处理；
(4)沉淀处理，向步骤(3)除铜后的滤液中加入硝酸铵，对滤液中的二价铁进行氧化，并进行加热，控制加热温度为80-95℃，除去草酸，避免干扰后续的萃取过程；
(5)控制沉淀，向步骤(4)所得滤液中继续加入氨水，并控制滤液pH为3-3.5，再次过滤，得到氢氧化铁沉淀和含镍滤液，氢氧化铁沉淀经洗涤、加热后得到铁红。
制备硫酸镍：将含镍滤液用萃取剂P204和P507的混合液萃取镍，静置，分离得到含镍萃取有机相和含杂质萃余液；再用4mol/L的H2SO4溶液从含镍萃取有机相中反萃取镍，得到电池级硫酸镍溶液。
蒸发结晶后制得的硫酸镍晶体送化验室分析，分析结果为22.18％Ni、0.012％Co、0.00028％Cu、0.00011％Fe，符合电池级硫酸镍的产品标准。
上面结合附图对本发明实施例作了详细说明，但是本发明不限于上述实施例，在所属技术领域普通技术人员所具备的知识范围内，还可以在不脱离本发明宗旨的前提下作出各种变化。此外，在不冲突的情况下，本发明的实施例及实施例中的特征可以相互组合。
Claims (10)
1.一种镍铁湿法处理方法，其特征在于，包括以下步骤：
S1：在高压氧气环境中，将镍铁粉碎料、硫酸和助蚀剂混合，进行酸浸反应；
S2：将步骤S1酸浸后浆料进行固液分离，所得滤液加入氧化剂，并加热，除去助蚀剂；
S3：再向滤液中加入沉淀剂，并控制滤液的pH，固液分离，得到氢氧化铁沉淀和含镍滤液。
2.根据权利要求1所述的镍铁湿法处理方法，其特征在于，步骤S1中，所述助蚀剂为过氧化氢、乙酸、乙酰丙酮、草酸或甘氨酸中的一种或多种。
3.根据权利要求1所述的镍铁湿法处理方法，其特征在于，步骤S1中，所述硫酸的浓度为3-8mol/L。
4.根据权利要求1所述的镍铁湿法处理方法，其特征在于，步骤S1中，所述酸浸反应的压力为3.0-6.5MPa，反应的温度为50-90℃。
5.根据权利要求1所述的镍铁湿法处理方法，其特征在于，步骤S2中，所述氧化剂为氯酸盐、亚硝酸盐、硝酸盐或过硫酸盐中的一种或多种。
6.根据权利要求1所述的镍铁湿法处理方法，其特征在于，步骤S2中，所述加热的温度为60-95℃。
7.根据权利要求1所述的镍铁湿法处理方法，其特征在于，步骤S3中，所述沉淀剂为氨水、氢氧化钠、碳酸钠或碳酸氢钠中的一种或多种。
8.根据权利要求1所述的镍铁湿法处理方法，其特征在于，步骤S3中，所述pH为3-3.5。
9.根据权利要求1所述的镍铁湿法处理方法，其特征在于，步骤S2中，所得滤液可加入镍铁进行置换还原浸出，过滤得到镍铁渣和除铜的浸出液，所述镍铁渣返回步骤S1进行酸浸，所述浸出液加入所述氧化剂进行后续处理。
10.权利要求1-9任一项所述的镍铁湿法处理方法得到的含镍滤液在制备电池级硫酸镍中的应用。
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| CN112941314B (zh) * | 2021-01-29 | 2022-12-13 | 湖南邦普循环科技有限公司 | 一种从镍铁合金中分离镍和铁的方法和应用 |
| CN112941313A (zh) * | 2021-01-29 | 2021-06-11 | 广东邦普循环科技有限公司 | 一种粗制镍铁合金的回收方法和应用 |
| CN113667825B (zh) * | 2021-07-20 | 2022-11-15 | 广东邦普循环科技有限公司 | 镍铁湿法处理方法及其应用 |
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- 2022-06-06 DE DE112022000294.8T patent/DE112022000294B4/de active Active
- 2022-06-06 ES ES202390090A patent/ES2957058A2/es active Pending
- 2022-06-06 WO PCT/CN2022/097183 patent/WO2023000847A1/zh active Application Filing
- 2022-06-06 GB GB2314580.8A patent/GB2622488A/en active Pending
- 2022-06-06 US US18/260,241 patent/US20240034639A1/en active Pending
- 2022-06-06 MA MA61498A patent/MA61498A1/fr unknown
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023000847A1 (zh) * | 2021-07-20 | 2023-01-26 | 广东邦普循环科技有限公司 | 镍铁湿法处理方法及其应用 |
| GB2622488A (en) * | 2021-07-20 | 2024-03-20 | Guangdong Brunp Recycling Technology Co Ltd | Nickel-iron wet treatment method and application thereof |
| WO2023123622A1 (zh) * | 2021-12-29 | 2023-07-06 | 荆门市格林美新材料有限公司 | 一种镍铁合金资源化综合利用方法 |
| CN117003212A (zh) * | 2023-08-07 | 2023-11-07 | 上海天汉环境资源有限公司 | 一种电池级材料的制备方法 |
| CN117003212B (zh) * | 2023-08-07 | 2024-04-05 | 上海天汉环境资源有限公司 | 一种电池级材料的制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| DE112022000294B4 (de) | 2024-02-29 |
| GB202314580D0 (en) | 2023-11-08 |
| ES2957058A2 (es) | 2024-01-09 |
| MA61498A1 (fr) | 2023-11-30 |
| WO2023000847A1 (zh) | 2023-01-26 |
| US20240034639A1 (en) | 2024-02-01 |
| GB2622488A (en) | 2024-03-20 |
| CN113667825B (zh) | 2022-11-15 |
| DE112022000294T5 (de) | 2023-09-14 |
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