US3630862A - Process for regenerating electrolytic solutions obtained in the electrolytic production of manganese dioxide - Google Patents
Process for regenerating electrolytic solutions obtained in the electrolytic production of manganese dioxide Download PDFInfo
- Publication number
- US3630862A US3630862A US11513A US3630862DA US3630862A US 3630862 A US3630862 A US 3630862A US 11513 A US11513 A US 11513A US 3630862D A US3630862D A US 3630862DA US 3630862 A US3630862 A US 3630862A
- Authority
- US
- United States
- Prior art keywords
- electrolytic
- electrolyte
- manganese
- solution
- calcium
- 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
- 239000008151 electrolyte solution Substances 0.000 title abstract description 28
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 title abstract description 28
- 238000004519 manufacturing process Methods 0.000 title abstract description 12
- 238000000034 method Methods 0.000 title description 23
- 230000001172 regenerating effect Effects 0.000 title description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 38
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 abstract description 31
- 239000000243 solution Substances 0.000 abstract description 19
- 229940099596 manganese sulfate Drugs 0.000 abstract description 9
- 239000011702 manganese sulphate Substances 0.000 abstract description 9
- 235000007079 manganese sulphate Nutrition 0.000 abstract description 9
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 abstract description 9
- 238000005868 electrolysis reaction Methods 0.000 abstract description 8
- 239000003792 electrolyte Substances 0.000 description 43
- 210000004027 cell Anatomy 0.000 description 36
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 13
- 229910052748 manganese Inorganic materials 0.000 description 13
- 239000011572 manganese Substances 0.000 description 13
- 238000001816 cooling Methods 0.000 description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 8
- 239000011575 calcium Substances 0.000 description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 7
- 229910052791 calcium Inorganic materials 0.000 description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 6
- 238000006386 neutralization reaction Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 229940043430 calcium compound Drugs 0.000 description 4
- 150000001674 calcium compounds Chemical class 0.000 description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 4
- 239000000920 calcium hydroxide Substances 0.000 description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000003472 neutralizing effect Effects 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 229910052925 anhydrite Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 229960003390 magnesium sulfate Drugs 0.000 description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 3
- 235000019341 magnesium sulphate Nutrition 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 229940021013 electrolyte solution Drugs 0.000 description 2
- 239000013505 freshwater Substances 0.000 description 2
- 238000011081 inoculation Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(iii) oxide Chemical compound O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 230000004043 responsiveness Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 240000001972 Gardenia jasminoides Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- GZMKWMMWAHQTHD-UHFFFAOYSA-L [Mn++].OS([O-])(=O)=O.OS([O-])(=O)=O Chemical compound [Mn++].OS([O-])(=O)=O.OS([O-])(=O)=O GZMKWMMWAHQTHD-UHFFFAOYSA-L 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229940091250 magnesium supplement Drugs 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
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 description 1
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229940028444 muse Drugs 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- GMVPRGQOIOIIMI-DWKJAMRDSA-N prostaglandin E1 Chemical compound CCCCC[C@H](O)\C=C\[C@H]1[C@H](O)CC(=O)[C@@H]1CCCCCCC(O)=O GMVPRGQOIOIIMI-DWKJAMRDSA-N 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
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
- C25B1/01—Products
- C25B1/21—Manganese oxides
Definitions
- Aqueous electrolytic solutions containing manganese sulfate, calcium sulfate and sulfuric acid, obtained in the electrolytic production of manganese (1V)-oxide at elevated temperatures in electrolytic cells are regenerated.
- the electrolytic solution is withdrawn from the electrolytic cell, cooled down to temperatures at least 5 centigrade degrees lower than the electrolysis temperature, precipitated matter is isolated therefrom after a period of at least 15 minutes, and the solution is recycled to the electrolytic cell.
- the present invention relates to a process for regenerating aqueous electrolytic solutions containing manganese sulfate, calcium sulfate and sulfuric acid, obtained in the electrolytic production of manganese IV)-oxide at elevated temperatures.
- Manganese dioxide is normally precipitated electrolytivally from a sulfuric acid manganese sulfate solution, at temperatures of between 80 and 98 C.
- cell electrolyte a sulfuric acid manganese sulfate solution
- an electrolyte portion to be withdrawn therefrom and to be neutralized by means of commercial manganese (III) -oxide prepared from crude manganese ore.
- the resulting solution which is termed regenerated electrolyte hereinafter, is recycled to the cell electrolyte.
- manganese ore is often found to contain rather considerable proportions of calcium compounds. These may appear in commercial manganese (ID-oxide produced therefrom, in the form of carbonates, sulfates, oxides or even silicates, for example.
- ID-oxide produced therefrom, in the form of carbonates, sulfates, oxides or even silicates, for example.
- cell electrolyte for ore-extraction, the above compounds are decomposed by the sulfuric acid contained in the electrolyte with the resultant formation of an equivalent proportion of calcium sulfate.
- regenerated electrolyte solutions saturated or supersaturated with calcium sulfate are obtained.
- the cell electrolyte and regenerated electrolyte are, however, strongly concentrated electrolytic solutions containing manganese sulfate together with magnesium sul fate and potassium sulfate, depending on the source of origin of the starting material, for example up to 0.5 mol/ liter magnesium sulfate in those cases in which African crude manganese dioxide is the starting material.
- the cell electrolyte contains sulfuric acid in a rather high concentration of between about 0.2 and 1.0 mol/liter. In view of this, the salts and sulfuric acid aforesaid were tested as to their influence upon the temperature responsive solubility of CaSO -2H O.
- FIG. 3 The strong influence of sulfuric acid on the temperature responsiveness of the solubility of CaSO -2H O is illustrated in FIG. 3 of the accompanying diagrams. As shown therein, the presence of H 50 in a concentration of merely 0.1 mol produces at C. a solubility approximately percent higher than that at 20 C.
- the process of the present invention for regenerating an aqueous electrolytic solution containing manganese sulfate, calcium sulfate and sulfuric acid, obtained in the electrolytic production of manganese (IV)-oxide at elevated temperatures in an electrolytic cell comprises more particularly withdrawing the electrolyte solution from the electrolytic cell, cooling the solution down to temperatures at least 5 centigrade degrees, preferably 14 to 40 centigrade degrees lower than the electrolysis temperature, isolating precipitated matter therefrom after a period of at least 15 minutes, preferably 1 to 3 hours, and recycling the said solution to the electrolytic cell.
- a preferred feature of the present invention comprises subjecting the electrolytic solutions, prior to cooling them, to treatment with manganese (II)-oxide or manganese (ID-carbonate to effect partial or complete neutralization of the sulfuric acid therein and, in the case of partial neutralization, neutralizing residual sulfuric acid by means of calcium oxide, calcium hydroxide or calcium carbonate.
- manganese (II)-oxide or manganese (ID-carbonate) to effect partial or complete neutralization of the sulfuric acid therein and, in the case of partial neutralization, neutralizing residual sulfuric acid by means of calcium oxide, calcium hydroxide or calcium carbonate.
- a further preferred feature of the present invention comprises neutralizing the electrolytic solution, freeing it from undissolved solid matter and then cooling it with agitation.
- a still further preferred feature of the present invention provides for the quantities of water evaporated during the electrolysis and regeneration of the electrolyte to be replaced with corresponding quantities of fresh water, the water being added to the electrolytic solution following isolation of precipitated matter and prior to recycling the said solution to the electrolytic cell.
- Room temperature is the lower temperature limit down to which the electrolytic solution should conveniently be cooled. Needless to say it is also possible for the solution to be cooled down to temperatures lower than room temperature, but this would imply the use of efficient cooling means and render the process a commercially less attractive procedure.
- the solubility curves shown in FIG. 5 of the accompanying diagrams illustrate the basic idea underlying the process of the present invention.
- the saturation solubility of the cell electrolyte is a function of its temperature (point A)
- the suspension is found to at least cool down to a temperature at which the same saturation concentration is reached (point B).
- the regenerated electrolyte is filtered to free it from undissolved or precipitated matter and recycled then to the cell electrolyte cycle.
- FIG. 5 shows the solubility curves for CaSO -2H O for the electrolyte described in Example 1 hereinafter. As shown therein, the curve of the cell electrolyte is situated below the curve for the regenerated electrolyte. Thus, it is possible by inoculation with CaSO -2H O crystals at a given working temperature to always produce a regenerated electrolyte supersaturated with respect to the cell electrolyte. In other words, a cell electrolyte supersaturated with calcium sulfate would be obtained if the two electrolytes were mixed together.
- EXAMPLE 1 The starting material was a cell electrolyte. It contained 110 grams MnSO 70 grams H grams MgSO and 3.5 kg. K 50 per liter and had a temperature of 95 C. The electrolyte was mixed in an agitator vessel with reduced manganese dioxide until the free sulfuric acid was found to have been substantially neutralized. It was immaterial whether the last residues of the free acid were neutralized with reduced crude manganese dioxide or with a further basic material, for example calcium carbonate, calcium hydroxide or sodium carbonate or a similar compound. The neutralized electrolyte was cooled with agitation, within 3 hours, down to a temperature of C., and filtered. The resulting regenerated electrolyte was recycled to the cell electrolyte cycle. CaSO -2H O could not be found to be precipitated therein.
- EXAMPLE 2 The starting material was a cell electrolyte. It contained 100 grams MnSO 50 grams H 50 and 20 grams MgSO per liter and had a temperature of C.
- the cell electrolyte was treated in the manner set forth in Example 1 using reduced crude manganese dioxide or, e.g. natural rhodochrosite (MnCO and the resulting suspension was conveyed from the agitator vessel to a settling tank, in which it was cooled down to about 40 C. and allowed to stand for some hours. Following filtration, the regenerated electrolyte was ready for use.
- MnCO reduced crude manganese dioxide or, e.g. natural rhodochrosite
- a process for regenerating an aqueous electrolytic solution containing manganese sulfate, calcium sulfate and sulfuric acid, obtained in the electrolytic production of manganese (IV)-oxide at elevated temperatures in an electrolytic cell which comprises withdrawing the electrolytic solution from the electrolytic cell, cooling the said solution down to temperatures at least 5 centigrade degrees lower than the electrolysis temperature, isolating precipitated matter therefrom after a period of at least 15 minutes, and recycling the said solution to the electrolytic cell.
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE1908416A DE1908416C3 (de) | 1969-02-20 | 1969-02-20 | Verfahren zum Regenerieren von wäßrigen mangansulfate calciumsulfat- und schwefelsäurehaltigen Elektrolytlösungen, die bei der elektrolytischen Gewinnung von Mangan(IV)-oxid anfallen |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3630862A true US3630862A (en) | 1971-12-28 |
Family
ID=5725775
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US11513A Expired - Lifetime US3630862A (en) | 1969-02-20 | 1970-02-16 | Process for regenerating electrolytic solutions obtained in the electrolytic production of manganese dioxide |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US3630862A (cs) |
| JP (1) | JPS5518661B1 (cs) |
| BE (1) | BE746290A (cs) |
| CS (1) | CS166253B2 (cs) |
| DE (1) | DE1908416C3 (cs) |
| FR (1) | FR2037112B1 (cs) |
| GB (1) | GB1292218A (cs) |
| NL (1) | NL166730C (cs) |
| NO (1) | NO126313B (cs) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01158293A (ja) * | 1987-12-15 | 1989-06-21 | Tlv Co Ltd | スチームトラップの弁口構造 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1874827A (en) * | 1931-05-12 | 1932-08-30 | Burgess Battery Co | Production of manganese dioxide |
| US2119560A (en) * | 1936-09-10 | 1938-06-07 | Stephen M Shelton | Electrolytic process for the extraction of metallic manganese |
| FR1448939A (fr) * | 1965-06-28 | 1966-08-12 | E J Lavino & Co | Procédé de préparation d'une solution de sulfate de manganèse à partir de ferromanganèse et d'un minerai essentiellement constitué par du bioxyde de manganèse |
-
1969
- 1969-02-20 DE DE1908416A patent/DE1908416C3/de not_active Expired
-
1970
- 1970-02-16 US US11513A patent/US3630862A/en not_active Expired - Lifetime
- 1970-02-18 JP JP1412270A patent/JPS5518661B1/ja active Pending
- 1970-02-18 CS CS1123A patent/CS166253B2/cs unknown
- 1970-02-19 NO NO00596/70A patent/NO126313B/no unknown
- 1970-02-19 GB GB8029/70A patent/GB1292218A/en not_active Expired
- 1970-02-20 FR FR7006152A patent/FR2037112B1/fr not_active Expired
- 1970-02-20 BE BE746290D patent/BE746290A/xx not_active IP Right Cessation
- 1970-02-20 NL NL7002456.A patent/NL166730C/xx not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| NO126313B (cs) | 1973-01-22 |
| DE1908416A1 (de) | 1970-09-10 |
| GB1292218A (en) | 1972-10-11 |
| CS166253B2 (cs) | 1976-02-27 |
| FR2037112A1 (cs) | 1970-12-31 |
| DE1908416C3 (de) | 1974-06-12 |
| NL7002456A (cs) | 1970-08-24 |
| FR2037112B1 (cs) | 1974-08-09 |
| BE746290A (fr) | 1970-08-20 |
| JPS5518661B1 (cs) | 1980-05-20 |
| NL166730B (nl) | 1981-04-15 |
| DE1908416B2 (de) | 1973-11-08 |
| NL166730C (nl) | 1981-09-15 |
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