CN106350686B - A kind of method that nickel chloride solution is produced using noble metal leachate as raw material - Google Patents
A kind of method that nickel chloride solution is produced using noble metal leachate as raw material Download PDFInfo
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- CN106350686B CN106350686B CN201610738596.4A CN201610738596A CN106350686B CN 106350686 B CN106350686 B CN 106350686B CN 201610738596 A CN201610738596 A CN 201610738596A CN 106350686 B CN106350686 B CN 106350686B
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- noble metal
- extraction
- metal leachate
- nickel
- leachate
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- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 title claims abstract description 16
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 title claims abstract description 16
- 239000002994 raw material Substances 0.000 title claims abstract description 9
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000460 chlorine Substances 0.000 claims abstract description 21
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 21
- 238000000605 extraction Methods 0.000 claims abstract description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 239000000344 soap Substances 0.000 claims abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 4
- 239000003350 kerosene Substances 0.000 claims abstract description 4
- 238000007127 saponification reaction Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract 2
- 239000003085 diluting agent Substances 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 9
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 4
- UUCGKVQSSPTLOY-UHFFFAOYSA-J cobalt(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Co+2].[Ni+2] UUCGKVQSSPTLOY-UHFFFAOYSA-J 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000012797 qualification Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000012074 organic phase Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000033116 oxidation-reduction process Effects 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 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
- 238000007654 immersion Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
- 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
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A kind of method that nickel chloride solution is produced using noble metal leachate as raw material, noble metal leachate be raw material, and the terminal pH requirements of noble metal leachate iron removaling is between 3.5~4.0.After iron removaling during liquid oxidation, in 450 550mv, logical chlorine time control pH value of solution after 4 6h, logical chlorine is adjusted to 3.5 4.0, P for reaction potential control507In extraction process, extractant P507Volume ratio with diluent sulfonated kerosene is 1:3, soda soap saponification rate is 70%, and the volume ratio of extraction organic phase and water phase is 3:1, extraction series is 7 grades, is compared：O:A=4:1, extraction form is counter-current extraction.Beneficial effect：The nickel of noble metal leachate, the nickel chloride solution of output qualification are recycled, satisfaction prepares the requirement of nickel chloride product, reduces the waste of nickel resources.
Description
Technical field
The invention belongs to smelting field of nonferrous metal, it is related to a kind of molten by raw material production nickel chloride of noble metal leachate
The method of liquid.
Background technology
In the production of nickel chloride product, first having to produce nickel chloride solution, the method for producing nickel chloride solution is more,
The method that dissolving with hydrochloric acid electrolytic nickel can be used, the method that dissolving with hydrochloric acid nickelous carbonate, nickel hydroxide can also be used etc., it is various
The raw materials used physics of production method Main Basiss and chemical property determine.Using nickeliferous noble metal leachate due to component
Complexity is, it is necessary to a kind of extracting method recycling nickel.
The content of the invention
The object of the present invention is to provide a kind of method that nickel chloride solution is produced using noble metal leachate as raw material.
Technical scheme：A kind of method that nickel chloride solution is produced using noble metal leachate as raw material, including with
Lower step：
A, by noble metal leachate（Further elements content is shown in Table 1）After thick hydroxide nickel cobalt adjusting pH value to 3.5-4.0
Filtered, filter residue is scum, removes the Fe elements in noble metal leachate.
B, noble metal leachate is heated to being passed through chlorine after 90-110 DEG C by the monovalence copper in noble metal leachate after iron removaling
Ionic oxide formation is bivalent cupric ion, and the necessity of this process is：Due to P507Extractant not extracts univalent copper ion, can only
Extract bivalent cupric ion, therefore, logical chlorine process be by the univalent copper ion complete oxidation in your immersion liquid after iron removaling for cupric from
Son；For logical chlorine process oxidation-reduction potential in 450mv-550mv, it be 4-6h to lead to the chlorine time, leads to after the completion of chlorine and adds thick nickel hydroxide
Solution ph is adjusted to 3.5-4.0, the solution after pH value is adjusted and is filtered through filter press.
C, liquid passes through P after the press filtration of step b outputs507Abstraction impurity removal, cobalt, copper, magnesium, manganese, the zinc etc. removed in leachate are miscellaneous
Matter, obtains liquid after pure nickel chloride extraction, it is ensured that liquid disclosure satisfy that the miscellaneous of the nickel chloride product of production high-quality after the extraction
The purpose of matter content requirement, extraction process use V (P507)：V (sulfonated kerosene)=25%：75%, 70% turn of nickel soap of soda soap saponification rate,
Extraction phase carries out 7 stage countercurrent extractions, Co in liquid after extraction than O/A=3/12+≤ 0.004g/l, Fe3+≤ 0.004g/l, Zn2+≤
0.004g/L, Cu2+≤ 0.004g/L, Mn2+≤ 0.004g/L, Mg2+≤ 0.50g/L, Pb2+≤ 0.004g/l, Na+≤0.8g/
l。
Beneficial effects of the present invention：The nickel of noble metal leachate, the nickel chloride solution of output qualification are recycled, satisfaction prepares chlorine
Change the requirement of nickel product, reduce the waste of nickel resources.Overall process is wet method, and condition is easily-controllable.
Brief description of the drawings
Fig. 1 is the process flow chart of the present invention.
Embodiment
Embodiment 1
A kind of method with noble metal leachate production nickel chloride solution, comprises the following steps：
A, noble metal leachate is measured（Further elements content is shown in Table 1）10L, add thick hydroxide nickel cobalt adjust pH value to
Filtered after 3.5.
B, noble metal leachate is passed through chlorine after being heated to 95 DEG C after iron removaling, leads to chlorine process oxidation-reduction potential in 480mv,
The logical chlorine time is 4.5h, and thick nickel hydroxide is added after the completion of logical chlorine and adjusts solution ph to 3.5, adjusts the solution after pH value through pressure
Filter is filtered.
C, liquid passes through P after the press filtration of step b outputs507Abstraction impurity removal, extraction process use V (P507)：V (sulfonated kerosene)=
25%：75%, 70% turn of nickel soap of soda soap saponification rate, extraction phase carries out 7 stage countercurrent extractions than O/A=3/1.
After testing, Co in raffinate2+≤ 0.004g/l, Fe3+≤ 0.004g/l, Zn2+≤ 0.004g/L, Cu2+≤
0.004g/L, Mn2+≤ 0.004g/L, Mg2+≤ 0.50g/L, Pb2+≤ 0.004g/l, Na+≤ 0.8g/l, raffinate component are shown in
Table 2；
Embodiment 2
2 step process of embodiment is with embodiment 1, and condition is different, specifically：
Step a and the difference of embodiment 1 are, adjust pH value to 3.8.
Step b and the difference of embodiment 1 are that noble metal leachate is passed through chlorine after being heated to 100 DEG C after iron removaling,
For logical chlorine process oxidation-reduction potential in 510mv, it is 5h to lead to the chlorine time.
Step c is identical with the content of embodiment 1.
After testing, Co in raffinate2+≤ 0.004g/l, Fe3+≤ 0.004g/l, Zn2+≤ 0.004g/L, Cu2+≤
0.004g/L, Mn2+≤ 0.004g/L, Mg2+≤ 0.50g/L, Pb2+≤ 0.004g/l, Na+≤ 0.8g/l, raffinate component are shown in
Table 3；
Embodiment 3
2 step process of embodiment is with embodiment 1, specifically：
Step a and the difference of embodiment 1 are, adjust pH value to 4.0.
Step b and the difference of embodiment 1 are that noble metal leachate is passed through chlorine after being heated to 105 DEG C after iron removaling,
For logical chlorine process oxidation-reduction potential in 530mv, it is 6h to lead to the chlorine time.
Step c is identical with the content of embodiment 1.
After testing, Co in raffinate2+≤ 0.004g/l, Fe3+≤ 0.004g/l, Zn2+≤ 0.004g/L, Cu2+≤
0.004g/L, Mn2+≤ 0.004g/L, Mg2+≤ 0.50g/L, Pb2+≤ 0.004g/l, Na+≤ 0.8g/l, raffinate component are shown in
Table 4；
Claims (1)
- A kind of 1. method that nickel chloride solution is produced using noble metal leachate as raw material, using the noble metal leachate containing nickel as original Expect, between the thick hydroxide nickel cobalt adjusting pH value of noble metal leachate addition to 3.5~4.0, ferro element enters in precipitation, and filtering makes Ferro element is removed from noble metal leachate, and noble metal leachate is passed through chlorine and carries out oxygen after iron removaling after being heated to 95-105 DEG C Change, in oxidizing process, in 480-530mv, logical chlorine time control solution after 4.5-6h, logical chlorine adds for reaction potential control Thick nickel hydroxide adjusts pH to 3.5-4.0, adjusts that the solution after pH value is filtered to obtain filtrate, and filtrate is removed by P507 extractions Miscellaneous, in extraction process, the volume ratio of extractant P507 and diluent sulfonated kerosene is 1:3, soda soap saponification rate is 70%, and extraction has The volume ratio of machine phase and water phase is 3:1, extraction series is 7 grades, and extraction form is counter-current extraction, raffinate component content after extraction For：Co2+≤ 0.004g/L, Fe3+≤ 0.004g/L, Zn2+≤ 0.004g/L, Cu2+≤ 0.004g/L, Mn2+≤ 0.004g/L, Mg2 +≤ 0.50g/L, Pb2+≤ 0.004g/L, Na+≤0.8g/L。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610738596.4A CN106350686B (en) | 2016-08-29 | 2016-08-29 | A kind of method that nickel chloride solution is produced using noble metal leachate as raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610738596.4A CN106350686B (en) | 2016-08-29 | 2016-08-29 | A kind of method that nickel chloride solution is produced using noble metal leachate as raw material |
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| Publication Number | Publication Date |
|---|---|
| CN106350686A CN106350686A (en) | 2017-01-25 |
| CN106350686B true CN106350686B (en) | 2018-05-15 |
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| CN201610738596.4A Active CN106350686B (en) | 2016-08-29 | 2016-08-29 | A kind of method that nickel chloride solution is produced using noble metal leachate as raw material |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109917740A (en) * | 2019-03-20 | 2019-06-21 | 金川集团股份有限公司 | A kind of chlorine oxidation removal of impurities intelligence control system and control method |
| CN116065035A (en) * | 2021-10-29 | 2023-05-05 | 长沙鑫康新材料有限公司 | A kind of purification preparation method of high-purity metallic nickel |
Citations (4)
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|---|---|---|---|---|
| CN102031373A (en) * | 2009-09-29 | 2011-04-27 | 惠州市东江环保技术有限公司 | Method for recycling nickel and copper from electroplating sludge |
| CN103060562A (en) * | 2011-10-18 | 2013-04-24 | 上海轻工业研究所有限公司 | Purification method of inorganic highly-acidic nickel salt solution |
| CN104313322A (en) * | 2014-10-17 | 2015-01-28 | 金川集团股份有限公司 | Method for deeply removing copper in hydrochloric acid leaching solution of cobalt nickel hydroxide |
| CN105349788A (en) * | 2015-11-23 | 2016-02-24 | 金川集团股份有限公司 | Method for producing industrial nickel sulfate through copper electrolysis arsenic matte |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6176491B2 (en) * | 2014-03-26 | 2017-08-09 | 住友金属鉱山株式会社 | Method for removing copper from aqueous nickel chloride solution |
-
2016
- 2016-08-29 CN CN201610738596.4A patent/CN106350686B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102031373A (en) * | 2009-09-29 | 2011-04-27 | 惠州市东江环保技术有限公司 | Method for recycling nickel and copper from electroplating sludge |
| CN103060562A (en) * | 2011-10-18 | 2013-04-24 | 上海轻工业研究所有限公司 | Purification method of inorganic highly-acidic nickel salt solution |
| CN104313322A (en) * | 2014-10-17 | 2015-01-28 | 金川集团股份有限公司 | Method for deeply removing copper in hydrochloric acid leaching solution of cobalt nickel hydroxide |
| CN105349788A (en) * | 2015-11-23 | 2016-02-24 | 金川集团股份有限公司 | Method for producing industrial nickel sulfate through copper electrolysis arsenic matte |
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