CN115573003A - Preparation method of 6N ultra-pure nickel - Google Patents
Preparation method of 6N ultra-pure nickel Download PDFInfo
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- CN115573003A CN115573003A CN202211246511.2A CN202211246511A CN115573003A CN 115573003 A CN115573003 A CN 115573003A CN 202211246511 A CN202211246511 A CN 202211246511A CN 115573003 A CN115573003 A CN 115573003A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 160
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 29
- 239000003792 electrolyte Substances 0.000 claims abstract description 25
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 150000002500 ions Chemical class 0.000 claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 27
- 238000000746 purification Methods 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 7
- 238000005342 ion exchange Methods 0.000 claims description 7
- 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 claims description 6
- 239000003456 ion exchange resin Substances 0.000 claims description 6
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 19
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000007790 solid phase Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910001453 nickel ion Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910001361 White metal Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- RYZCLUQMCYZBJQ-UHFFFAOYSA-H lead(2+);dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Pb+2].[Pb+2].[Pb+2].[O-]C([O-])=O.[O-]C([O-])=O RYZCLUQMCYZBJQ-UHFFFAOYSA-H 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000010969 white metal Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/08—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention relates to a preparation method of 6N ultra-pure nickel, which is characterized in that purified nickel nitrate solution is taken as electrolyte and is filled into an electrolytic bath; then, respectively putting an anode plate and a titanium plate which are made of nickel raw materials into an electrolytic tank as cathode plates, and simultaneously adding an ion diaphragm bag on the anode plate; starting electrolytic reaction, and carrying out direct current electrolysis to obtain 6N ultra-pure nickel on the cathode plate. The invention has lower cost and environmental protection, and can effectively remove impurities in the electrolyte.
Description
Technical Field
The invention relates to a preparation method of high-purity metal, in particular to a preparation method of 6N ultra-pure nickel.
Background
Nickel, having a relative atomic mass of 58.69, is a hard, ductile and ferromagnetic metal that is highly polished and corrosion resistant, has a melting point of 1453 deg.C, a boiling point of 2732 deg.C, and a density of 8.902g/cm 3 . High-purity nickel (nickel purity is more than 4N, namely more than 99.99 percent) contains very few impurities, is glossy silver-white metal, belongs to transition metal, and is widely applied to the fields of sputtering target materials, ion plating, connecting lines for electronic industry, high-purity reagents, high-performance alloys and the like due to hard quality, ductility and excellent processing performance. In recent years, with the development of high-tech industries, the application field of high-purity nickel is increasingly wide.
With the continuous improvement of the purity of the high-purity nickel, the service performance of the high-purity nickel is also continuously improved. The preparation of high-purity nickel generally obtains an intermediate product such as nickel nitrate or nickel chloride from a traditional smelting process, and the intermediate product is extracted with high purity to prepare metal. Electrolytic reduction or hydrogen reduction is used as a main method for preparing high-purity nickel.
The electrolytic refining method is the main method for preparing high-purity nickel, electrolytic nickel and nickel chloride aqueous solutions obtained by the traditional smelting process are respectively used as an anode and an electrolyte, a third-level amine is used as an extracting agent in a clean solution of the electrolyte, and if only from the metal components, 4N-level nickel with the impurity content of 10-20PPm can be easily obtained by refining the electrolytic nickel.
For example, in terms of dissolution of hydrogen, metallic nickel does not dissolve at a high concentration after forming a hydride, but the concentration of hydrogen in electrolytic nickel is generally several tens of PPm, which is much higher than the solubility of metallic iron and metallic cobalt. In addition, electrolytic nickel usually contains tens to hundreds of PPm of oxygen and tens of PPm of nitrogen. Therefore, these gaseous components must be removed to obtain metallic nickel of higher purity. For this purpose, the gas is usually degassed by vacuum melting, but oxygen removal is difficult. In contrast, if heat treatment is performed in hydrogen gas before melting nickel and then vacuum melting degassing is performed, the concentration of oxygen, nitrogen, and hydrogen can be reduced to several PPm. Therefore, the purity of the metallic nickel obtained by the traditional nickel smelting method is more than 4N.
The solid-phase electrolysis is a refining method capable of effectively removing not only metallic impurities but also gaseous impurities. The basic concept of solid phase electrolysis is to use the principle that a metal rod to be extracted at high purity is placed in a high vacuum of 9 to 10 torr, the sample metal is usually heated to a temperature of 100 ℃ below its melting point, one end is used as an anode and the other end is used as a cathode, and several hundred A/CM is introduced 2 Direct current. Then, solute elements such as carbon, oxygen, and nitrogen, whose effective charges are negative, move to the anode side, which is the direction in which electrons flow, and solute elements such as copper, iron, and cobalt, whose effective charges are positive, move to the cathode side. After the electrolysis is completed, the middle part of the sample metal rod is cut out to obtain high-purity metal.
The solid-phase electrolysis method is mainly used for high-purity extraction of rare earth metals, but has few reported examples. Examples of applications of vanadium and thorium other than rare earth metals have been reported. The solid-phase electrolysis method is effective for removing impurity components, particularly gas components. The solid-phase electrolysis method having such characteristics has not been reported to be applied to high-purity extraction of metallic nickel, but is one of the technically effective means.
Chinese patent publication No. CN112359226A, 2/12/2021 discloses a method for preparing high purity nickel, which comprises mixing nickel sulfide ore particles with nickel sulfide ore particles by high temperature negative pressure method to realize primary reduction and desulfurization to obtain crude nickel simple substance, introducing carbon monoxide into the crude nickel simple substance to release heat to obtain Ni (CO) 4 Then heating Ni (CO) 4 Decomposing the nickel by heat absorption, further refining the nickel simple substance, putting the refined nickel simple substance into a hydrochloric acid environment with the pH of 1 to 3, and introducing chlorine gas to prepare high-purity NiCl 2 The solution is then deoiled and purified by anion exchange resin, and finally high-purity nickel simple substance is obtained by electrodeposition, and the method has the advantages that the redox flow is introduced on the basis of the traditional liquid-phase electrolytic electrodeposition preparation of the nickel simple substance, and the method can comprise the steps ofEffectively remove anions doped in the nickel simple substance, thereby obtaining the nickel simple substance with higher purity. However, the technical process is complicated, and the finally produced high-purity nickel is only 5N level, and the purity cannot reach more than 6N.
In summary, the conventional electrolysis technology cannot effectively remove the impurities which are difficult to remove, particularly Ag, co, pb and Fe, so that the impurities and the like in the obtained high-purity nickel are high. Moreover, the product produced by the traditional electrolytic nickel technology can not reach the quality requirement of more than 6N.
Disclosure of Invention
The invention aims to provide a preparation method of 6N ultra-pure nickel for effectively removing impurities in the nickel.
In order to solve the problems, the preparation method of the 6N ultra-pure nickel is characterized by comprising the following steps: the method comprises the steps of taking a purified nickel nitrate solution as electrolyte and filling the electrolyte into an electrolytic cell; then, respectively putting an anode plate and a titanium plate which are made of nickel raw materials into an electrolytic tank as cathode plates, and simultaneously adding an ionic diaphragm bag on the anode plate; starting electrolytic reaction, and carrying out direct current electrolysis to obtain 6N ultra-pure nickel on the cathode plate.
The purified nickel nitrate solution is prepared by carrying out a dissolution reaction on 3N8 electronickel and electronic-grade nitric acid to obtain a nickel nitrate solution; the nickel nitrate solution is subjected to impurity removal by adopting a free amine type ion exchange resin M, the ion exchange liquid passing speed is controlled to be 10L/h, the purification volume ratio is 1.
The temperature of the electrolyte is 15 to 25 ℃.
The anode plate is made of 3N8 nickel raw materials.
The distance between the centers of the anode plate and the cathode plate is 10 to 20cm.
The current density of the direct current electrolysis is 80 to 120A/m 2 。
Compared with the prior art, the invention has the following advantages:
1. in the invention, the anode plate ion diaphragm bag is adopted to isolate the impurities of the anode mud, the ion exchange impurity removal is carried out on the electrolyte, and the impurity content in the electrolyte is greatly reduced by controlling the resin model selection, the purification rate and the purification volume, so that compared with the traditional electrolytic nickel technology, the method can effectively remove the impurities in the electrolyte in the preparation process of the ultra-pure nickel and control the impurity ions separated out from the anode to diffuse to the cathode, thereby enabling the cathode to produce the ultra-pure nickel metal.
2. The invention has the advantages of simple required equipment, large capacity of single set of equipment, low cost and environmental protection.
3. The quality of the ultra-pure nickel product obtained by the method can reach 6N requirements.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a flow chart of the present invention.
Detailed Description
As shown in figure 1, the preparation method of 6N ultra-pure nickel is characterized in that a purified nickel nitrate solution is used as an electrolyte and is filled into an electrolytic tank, and the temperature of the electrolyte is controlled to be 15 to 25 ℃; then, respectively putting an anode plate and a titanium plate which are made of nickel raw materials into an electrolytic tank as a cathode plate, wherein the center distance between electrode plates of the anode plate and the cathode plate is 10-20cm; meanwhile, an ion diaphragm bag is additionally arranged on the anode plate to isolate impurities. Starting an electrolytic reaction, and carrying out direct current electrolysis with the current density of 80 to 120A/m 2 And 6N ultra-pure nickel can be obtained on the cathode plate.
Wherein: the purified nickel nitrate solution is prepared by dissolving 3N8 electronickel and electronic-grade nitric acid for reaction to obtain a nickel nitrate solution; the nickel nitrate solution is subjected to impurity removal by adopting a free amine type ion exchange resin M, the ion exchange liquid passing speed is controlled to be 10L/h, the purification volume ratio (L/L) is 1.
The anode plate is made of 3N8 nickel raw materials, the 3N8 nickel is a common electrolytic nickel plate which is popular in the market, the common electrolytic nickel plate is cut according to the actual requirement of the electrolytic reaction, the common electrolytic nickel plate is cleaned after the size of the common electrolytic nickel plate meets the requirement of the electrolytic production, and then the common electrolytic nickel plate is directly used as a soluble anode of the electrolytic reaction.
The direct current required for electrolysis can be controlled by a rectifier provided with the electrolysis cell.
Example 1
Preparing a nickel nitrate solution as an electrolyte: wherein the concentration of nickel ions is 80g/L, the pH value of the solution is 0.5, and the temperature of the electrolyte is 15 ℃; the method comprises the following steps of (1) physically removing impurities from prepared nickel nitrate electrolyte through three-level mum, removing impurities by adopting free amine type ion exchange resin M, controlling the ion exchange liquid passing speed to be 10L/h, and the purification volume ratio (L/L) to be 1; preparing a 3N8 nickel raw material and a titanium plate into an anode plate and a cathode plate of an electrolytic cell; respectively placing an anode plate and a cathode plate into an electrolytic tank, and simultaneously adding an ion diaphragm bag on the anode plate, wherein the inter-electrode distance is 10cm; starting electrolytic reaction, and performing direct current electrolysis to obtain ultra-pure nickel on the cathode plate with current density of 80A/m 2 。
The ultra-pure nickel is detected by an Element GD glow discharge mass spectrometer (the manufacturer is German Sammerfo, and the model is LH-S-046). Detection conditions of the apparatus: the temperature is 18-28 ℃, and the relative humidity is 30-70%.
The contents of impurity elements in part of the ultrapure nickel sample are shown in Table 1.
TABLE 1 ultra pure nickel GD-MS partial elemental analysis results
Example 2
Preparing a nickel nitrate solution as an electrolyte, wherein the concentration of nickel ions is 100g/L, the pH value of the solution is 2.0, and the temperature of the electrolyte is 20 ℃; the prepared nickel nitrate electrolyte is subjected to three-level mum-level physical impurity removal, free amine type ion exchange resin M is adopted for impurity removal, the ion exchange liquid passing speed is controlled to be 10L/h, and the purification volume ratio (L/L) is 1:5, further reducing the content of main impurities in the nickel nitrate solution and then loading the nickel nitrate solution into an electrolytic bath; preparing an anode plate and a cathode plate of the electrolytic cell from a 3N8 nickel raw material and a titanium plate; respectively mounting anode plate and cathode platePutting into an electrolytic cell, and simultaneously adding an ion diaphragm bag on an anode plate, wherein the inter-electrode distance is 12cm; starting electrolytic reaction, and performing direct current electrolysis to obtain ultra-pure nickel on the cathode plate with current density of 100A/m 2 。
The test conditions of the ultra-pure nickel were the same as in example 1, and the contents of impurity elements in part of the sample were shown in Table 2.
TABLE 2 result of GD-MS analysis of ultra-pure nickel partial element
Example 3
Preparing a nickel nitrate solution as an electrolyte, wherein the concentration of nickel ions is 120g/L, the pH value of the solution is 4.0, and the temperature of the electrolyte is 25 ℃; physically removing impurities from the prepared nickel nitrate electrolyte by three-level mum, removing impurities by adopting free amine type ion exchange resin M, controlling the ion exchange liquid passing speed to be 10L/h and the purification volume ratio (L/L) to be 1, and then loading the nickel nitrate electrolyte into an electrolytic cell after reducing the content of main impurities in the nickel nitrate solution; preparing an anode plate and a cathode plate of the electrolytic cell from a 3N8 nickel raw material and a titanium plate; respectively placing an anode plate and a cathode plate into an electrolytic tank, and simultaneously adding an ion diaphragm bag on the anode plate, wherein the inter-electrode distance is 15cm; starting electrolytic reaction, and performing direct current electrolysis to obtain ultra-pure nickel on the cathode plate with current density of 120A/m 2 。
The testing conditions of the ultra-pure nickel are the same as those of example 1, and the contents of impurity elements in a part of the sample are shown in Table 3.
TABLE 3 result of GD-MS analysis of ultra-pure nickel partial element
Claims (6)
1. A preparation method of 6N ultra-pure nickel is characterized by comprising the following steps: the method comprises the steps of taking a purified nickel nitrate solution as electrolyte and filling the electrolyte into an electrolytic cell; then, respectively putting an anode plate and a titanium plate which are made of nickel raw materials into an electrolytic tank as cathode plates, and simultaneously adding an ion diaphragm bag on the anode plate; starting electrolytic reaction, and carrying out direct current electrolysis to obtain 6N ultra-pure nickel on the cathode plate.
2. The method for preparing 6N ultra-pure nickel according to claim 1, wherein the method comprises the following steps: the purified nickel nitrate solution is prepared by carrying out a dissolution reaction on 3N8 electronickel and electronic-grade nitric acid to obtain a nickel nitrate solution; the nickel nitrate solution is subjected to impurity removal by adopting a free amine type ion exchange resin M, the ion exchange liquid passing speed is controlled to be 10L/h, the purification volume ratio is 1.
3. The method for preparing 6N ultra-pure nickel according to claim 1, wherein the method comprises the following steps: the temperature of the electrolyte is 15 to 25 ℃.
4. The method for preparing 6N ultra-pure nickel according to claim 1, wherein the method comprises the following steps: the anode plate is made of 3N8 nickel raw materials.
5. The method for preparing 6N ultra-pure nickel according to claim 1, wherein the method comprises the following steps: the distance between the centers of the electrode plates of the anode plate and the cathode plate is 10-20cm.
6. The method for preparing 6N ultra-pure nickel according to claim 1, wherein the method comprises the following steps: the current density of the direct current electrolysis is 80 to 120A/m 2 。
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