US3414494A - Method of manufacturing pure nickel hydroxide - Google Patents
Method of manufacturing pure nickel hydroxide Download PDFInfo
- Publication number
- US3414494A US3414494A US502434A US50243465A US3414494A US 3414494 A US3414494 A US 3414494A US 502434 A US502434 A US 502434A US 50243465 A US50243465 A US 50243465A US 3414494 A US3414494 A US 3414494A
- Authority
- US
- United States
- Prior art keywords
- nickel
- compartments
- suspension
- nickel hydroxide
- hydroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 title claims description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 51
- 229910052759 nickel Inorganic materials 0.000 claims description 25
- 239000000725 suspension Substances 0.000 claims description 14
- 239000003792 electrolyte Substances 0.000 claims description 13
- 238000005868 electrolysis reaction Methods 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 239000011593 sulfur Substances 0.000 claims description 9
- 229910052717 sulfur Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 2
- 238000000034 method Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 description 5
- 235000011152 sodium sulphate Nutrition 0.000 description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 4
- 229940053662 nickel sulfate Drugs 0.000 description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 4
- 239000000543 intermediate Substances 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical group 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Definitions
- the present invention relates to a novel method of manufacturing nickel hydroxide by an electrochemical process whereby this substance can be obtained directly from nickel mat (preferably refined by a metallurgical process) and from which any impurities detrimental to its subsequent applications (notably as an additive to nickelplating baths) have been removed.
- high-purity nickel hydroxide is obtained from nickel sulfate or nickel chloride :by lime or soda transfer, the salts, sulfate or chloride themselves being obtained heforehand according to conventional methods notably from pure nickel or nickel oxide.
- pure nickel or nickel oxide may be prepared from nickel mat by applying various known refining processes, whether of the dry or moist type.
- this invention is concerned with a method capable of producing nickel hydroxides having the lowest possible contents of alkaline or alkaline-earth metal residues.
- the present invention relates to a method of producing nickel hydroxide by an electrolytic process comprising the following steps:
- An anodic corrosion of nickel-mat anodes by exerting a direct electrolytic action in the anode compartments of an electrolysis cell divided into compartments and containing as the electrolyte an aqueous solution of a water-soluble chloride or sulfate of an alkaline or alkaline-earth metal such as notably sodium, potassium, magnesium, calcium, to produce a high nickelchloride, or nickel-sulfate, anolyte in an acid medium having a pH value of 2 to 4.
- a water-soluble chloride or sulfate of an alkaline or alkaline-earth metal such as notably sodium, potassium, magnesium, calcium
- this method is carried out continuously.
- the nickel-mat anodes comprise mainly nickel and sulfur, 76% to 83% by Weight of nickel and 23% to 16% by weight of sulfur.
- the contents of elements other than nickel and sulfur lie within the following limits, by weight:
- the corrosion of the immersed portions of the anodes takes place regularly and uniformly. The dissolution is stopped when the current rises. Then, only a stump of anode (undissolved mat) and a sponge of sulfur remain.
- the sulfur sponge contains from 2% to 3% of the total initial nickel.
- a complete method of continuously manufacturing nickel hydroxide according to this invention is described hereinafter, by way of example, by using a sodium sulfate electrolyte.
- Nickel-mat anodes are anodically corroded in anode compartments filled with a sodium sulfate, Na SO electrolyte, the Na SO concentration ranging from to g./liter. This electrolyte becomes charged with Ni to form a mixture of nickel sulfate and sodium sulfate.
- the nickel concentration maintained by continuous circulation ranges from 4 to 8 g./liter of nickel.
- the pH in the anode compartment is kept at a value of 2 to 4.
- the electrolytic dissolution takes place at between 100 to 150 a./sq. m. of anode current density consistent with an adequate anode efficiency and the absence of oxygen release.
- a difference in level of 4 to 6 cm. is maintained between the anode and the cathode compartments by proper partitioning and the use of partition fabric elements, whereby the anolyte will flow continuously towards the cathode compartments.
- the cathode compartment is kept at a pH value of 8 to 10 and the nickel sulfate is precipitated therein in the form of nickel hydroxide within these pH limit values.
- the cathodes consist of stainless steel or nickel sheets and are the seat of a release of hydrogen.
- the bath is kept at a temperature ranging from 45 to 55 C., and the cathode compartment is stirred by using compressed air to keep the hydroxide in suspension and continuously sweeping the cathodes to avoid any undesired or parasitic deposit.
- the hydroxide suspension flowing continuously from the electrolytic cells is decanted in a static decanter in order to raise the nickel concentration to about 25-30 g./liter.
- This suspension is subsequently filtered on a drum-type rotary filter and then washed over the filter.
- three filtration steps are carried out and followed by a Washing step and two inter-mediate repulping steps with water by using 8 to 10 volumes of water per volume of hydroxide.
- These repulping steps should be effected in a minimum time, of the order of half an hour, to ensure an eflicient Washing of the hydroxide, in a lukewarm medium, the same applying to the filtration steps.
- a temperature of 45 to 55 C. is adequate for performing these steps.
- hydroxide manufactured according to the method of this invention by using a Na SO electrolyte and from mat anodes having the composition set forth hereinabove assays as follows (the percentages being by weight):
- the present invention has been described hereinabove with particular reference to the electrolysis of mat anodes in a sodium sulfate electrolyte, but it applies as well to 'any electrolysis of mat anodes in any type of alkaline or alkaline-earth salt electrolyte providing a cathode basic medium having a pH value ranging from 8 to 10.
- a method of manufacturing pure nickel hydroxide which comprises the steps of effecting the anodic corrosion of nickel mat anodes having the following contents by weight: nickel 76% to 83%, sulfur 23% to 16%, cobalt 0.30% to 0.40%, iron 0.04% to 0.08%, copper 0.050% to 0.065%, by direct electrolytic action in anode compartments of an electrolysis cell divided into compartments which contains as an electrolyte an aqueous solution of a water-soluble salt selected from the group consisting of the chlorides and sulfates of sodium, potassium, magnesium and calcium, to form an anolyte having a high-nickel salt content selected from the group consisting of the chloride and sulfate, in an acid medium having a pH value ranging from 2 to 4, diffusing the anolyte towards the anode compartments of the electrolysis cell through fabric partitions separating the anode compartments from the cathode compartments, precipitating the nickel in the cathode compartments in the form of nickel hydroxide,
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Electrolytic Production Of Metals (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR15327A FR1441749A (fr) | 1965-04-30 | 1965-04-30 | Nouveau procédé de fabrication d'hydrate de nickel pur |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3414494A true US3414494A (en) | 1968-12-03 |
Family
ID=8577710
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US502434A Expired - Lifetime US3414494A (en) | 1965-04-30 | 1965-10-22 | Method of manufacturing pure nickel hydroxide |
Country Status (11)
| Country | Link |
|---|---|
| US (1) | US3414494A (it) |
| AT (1) | AT262934B (it) |
| BE (1) | BE672641A (it) |
| CH (1) | CH437235A (it) |
| DE (1) | DE1265153B (it) |
| ES (1) | ES321567A1 (it) |
| FI (1) | FI45649C (it) |
| FR (1) | FR1441749A (it) |
| GB (1) | GB1080119A (it) |
| NL (1) | NL6515547A (it) |
| NO (1) | NO115735B (it) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3979223A (en) * | 1971-03-03 | 1976-09-07 | General Electric Company | Electrochemical impregnation of electrode for rechargeable cell |
| US4265718A (en) * | 1979-01-09 | 1981-05-05 | Societe Metallurgique Le Nickel S. L. N. | Method for producing hydroxylated nickel compounds |
| US4540476A (en) * | 1982-12-10 | 1985-09-10 | At&T Bell Laboratories | Procedure for making nickel electrodes |
| CN1041193C (zh) * | 1994-03-22 | 1998-12-16 | 英科有限公司 | 由元素镍制备氢氧化镍的方法 |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4239295C2 (de) * | 1992-11-23 | 1995-05-11 | Starck H C Gmbh Co Kg | Verfahren zur Herstellung von reinem Nickelhydroxid sowie dessen Verwendung |
| JP2001031429A (ja) * | 1999-07-16 | 2001-02-06 | Matsushita Electric Ind Co Ltd | 水酸化ニッケルの製造方法 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2667454A (en) * | 1948-03-13 | 1954-01-26 | Paul S Roller | Electrolytic methods and apparatus for production of metal hydroxides |
| US3214355A (en) * | 1958-09-03 | 1965-10-26 | Ludwig Kandler | Process for the filling of pores of metallic or metallic coated frames with metallic hydroxides and products thereof |
-
1965
- 1965-04-30 FR FR15327A patent/FR1441749A/fr not_active Expired
- 1965-10-22 US US502434A patent/US3414494A/en not_active Expired - Lifetime
- 1965-11-18 CH CH1588665A patent/CH437235A/fr unknown
- 1965-11-19 NO NO160556A patent/NO115735B/no unknown
- 1965-11-19 GB GB49310/65A patent/GB1080119A/en not_active Expired
- 1965-11-22 BE BE672641D patent/BE672641A/xx unknown
- 1965-11-30 NL NL6515547A patent/NL6515547A/xx unknown
- 1965-12-10 DE DEN27747A patent/DE1265153B/de not_active Withdrawn
- 1965-12-20 AT AT1146065A patent/AT262934B/de active
- 1965-12-29 ES ES0321567A patent/ES321567A1/es not_active Expired
- 1965-12-30 FI FI653119A patent/FI45649C/fi active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2667454A (en) * | 1948-03-13 | 1954-01-26 | Paul S Roller | Electrolytic methods and apparatus for production of metal hydroxides |
| US3214355A (en) * | 1958-09-03 | 1965-10-26 | Ludwig Kandler | Process for the filling of pores of metallic or metallic coated frames with metallic hydroxides and products thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3979223A (en) * | 1971-03-03 | 1976-09-07 | General Electric Company | Electrochemical impregnation of electrode for rechargeable cell |
| US4265718A (en) * | 1979-01-09 | 1981-05-05 | Societe Metallurgique Le Nickel S. L. N. | Method for producing hydroxylated nickel compounds |
| US4540476A (en) * | 1982-12-10 | 1985-09-10 | At&T Bell Laboratories | Procedure for making nickel electrodes |
| CN1041193C (zh) * | 1994-03-22 | 1998-12-16 | 英科有限公司 | 由元素镍制备氢氧化镍的方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| BE672641A (it) | 1966-03-16 |
| FI45649C (fi) | 1972-08-10 |
| FR1441749A (fr) | 1966-06-10 |
| NO115735B (it) | 1968-11-25 |
| FI45649B (it) | 1972-05-02 |
| NL6515547A (it) | 1966-10-31 |
| ES321567A1 (es) | 1966-10-01 |
| DE1265153B (de) | 1968-04-04 |
| GB1080119A (en) | 1967-08-23 |
| CH437235A (fr) | 1967-06-15 |
| AT262934B (de) | 1968-07-10 |
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