US2651611A - Electrowinning of chromium - Google Patents
Electrowinning of chromium Download PDFInfo
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- US2651611A US2651611A US230413A US23041351A US2651611A US 2651611 A US2651611 A US 2651611A US 230413 A US230413 A US 230413A US 23041351 A US23041351 A US 23041351A US 2651611 A US2651611 A US 2651611A
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- United States
- Prior art keywords
- chromium
- grams
- sulfate
- iron
- precipitate
- Prior art date
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title description 20
- 229910052804 chromium Inorganic materials 0.000 title description 17
- 239000011651 chromium Substances 0.000 title description 17
- 238000005363 electrowinning Methods 0.000 title description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 239000002244 precipitate Substances 0.000 description 16
- DSHWASKZZBZKOE-UHFFFAOYSA-K chromium(3+);hydroxide;sulfate Chemical compound [OH-].[Cr+3].[O-]S([O-])(=O)=O DSHWASKZZBZKOE-UHFFFAOYSA-K 0.000 description 15
- 229910000356 chromium(III) sulfate Inorganic materials 0.000 description 14
- 239000011696 chromium(III) sulphate Substances 0.000 description 14
- 235000015217 chromium(III) sulphate Nutrition 0.000 description 14
- 238000000034 method Methods 0.000 description 14
- 229910052742 iron Inorganic materials 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 description 8
- 235000011152 sodium sulphate Nutrition 0.000 description 8
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 7
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 7
- 235000011130 ammonium sulphate Nutrition 0.000 description 7
- 125000004122 cyclic group Chemical group 0.000 description 7
- 229910001430 chromium ion Inorganic materials 0.000 description 6
- 229910000599 Cr alloy Inorganic materials 0.000 description 5
- 239000000788 chromium alloy Substances 0.000 description 5
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 3
- 150000001342 alkaline earth metals Chemical class 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910000604 Ferrochrome Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229940037003 alum Drugs 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PYKNDCILXQWMJP-UHFFFAOYSA-N azane;chromium(3+) Chemical compound N.[Cr+3] PYKNDCILXQWMJP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002288 cocrystallisation Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000013379 molasses Nutrition 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Chemical compound CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- 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
- C25C1/10—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of chromium or manganese
Definitions
- the present invention relates to a cyclic electrowinning process for the preparation of chromium metal fromiron-chromi'um alloys.
- Another known process for the electrowinning of chromium comprises preparing ammonium chromium alum, used as the feed in the process,
- Another object is to produce in. the cyclic process chromium chemicals which may be efficiently used in theelectrowinning step to form chromium metal of high purity.
- the single figure isv a fiow sheet illustrating the steps of the cyclic method of the invention.
- an iron-chromium alloy is digested with a "dilute mineral acid, for example sulfuric acid, at a temperature of between 60 and 105 C. This step is indicated in box I of the flow sheet.
- the resulting pulp is filtered to remove the residue which consists largely of silica. This step is indicated in box 2 of the flow sheet.
- the filtrate is added to a hot aqueous solution of an alkali or an alkaline earth metal base, for example sodium carbonate, under substantially non-oxidizing atmospheric conditions to a final pH below 3.8 to yield a granular basic chrome sulfate precipitate which is easily filtered and washed free of soluble salts.
- the precipitation step is indicated by box 3 and filtering step by box 4 of the flow sheet.
- the temperature of said alkali or Iii Claim. (Cl. 204-105) is indicated by box 8 of the flow sheet.
- this reduced anolyte is used to dissolve-further alkaline earth metal taining of a granular precipitate, since at less than C. the precipitate tends to become gelatinous.
- the hydrated basic chromium sulfate precipitate is dissolved with a portion of the reduced anolyte from the electrolysis step to" give trivalent basic chromium sulfate solutionswhich are used as electrolyte in the electrowinning step. Box 5 of the flow sheet indicatesthis step. "The solution so obtained is then increased incon-- centration by evaporation. This step is -indicated by box 6 of the flow sheet.
- Hydrated basic chromium sulfate precipitate can be completely dissolved with considerably less than the calculated theoretical acid required to neutralize the basic portion of the precipitate to yield a solution containing basic chromium sulfate.
- the hexavalent chromium in theanolyte is reduced to chromium valence-III with a common reducing agent, organic or inorganic.
- This step basic chromium sulfate precipitate to provide cell feed-
- the cyclic use of this reduced anolyte is-indicated by the line connecting box, 8 and box 5; of the flow sheet.
- the remaining reduced anolyte which contains the sulfate portion of the basic chromium sulfate precipitate as sulfuric acid is in excess and can be used to dissolve iron-chromium alloy from which further basic chromium sulfate can be derived.
- the cyclic use of this excess reduced anolyte is shown by the line between box 8 and box I of the flow sheet.
- the basic chromium sulfate was dissolved with 127 cc. of reduced anolyte which consisted of 38.3 grams of trivalent chromium ion, 55.0 grams of ammonium sulfate, 32.0 grams of sodium sulfate, and 460 grams of sulfuric acid. To this solution were added 14 grams of ammonium sulfate and 8.0 grams of sodium sulfate.
- the resultant 3905 cc. of solution contained 318.3 grams of trivalent chromium ion, 69 grams of ammonium sulfate, 40 grams of sodium sulfate, and 0.8 gram of iron. 2300 cc. of water were evaporated off and the resultant solution used as cell feed.
- chromium metal of composition 270.3 grams chromium, 0.8 gram iron, was obtained.
- 1605 cc. of anolyte was produced containing 48 grams of hexavalent chromium ion, 69 grams of ammonium sulfate, 40 grams of sodium sulfate, and 714 grams of sulfuric acid.
- This anolyte was reduced'with 40 grams of molasses to'form455 cc. of reduced anolyte, 328 cc. of which was considered above as being used to leach the ferrochromium, and 127 cc.
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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)
Description
Patented Sept. 8, 1953 Michael C. Carosella and John D. Mettler, Niagara Falls, Y;., assi'gnors to Union Carbide and Carbon Corporation, a corporation of New York.
Application June '1', 1951, Serial No. 230,413
The present invention relates to a cyclic electrowinning process for the preparation of chromium metal fromiron-chromi'um alloys.
Heretofore, one method for the electrowinning of chromium was plating from chromic acid baths. The costly chromic acid required as feed and the high electrical power usage for this method renders it very inefiicicnt.
Another known process for the electrowinning of chromium comprises preparing ammonium chromium alum, used as the feed in the process,
by digesting chromium-ore with anolyte from the electrolysis step plus additional sulfuric acid, crystallizi-ng the iron, aluminum and other impurities from the digest liquors as alums with a resultant consumptionof sulfuric acid and am monium sulfate, and finally recovering a substantially pure chromium alum from the resultant partially purified solutions by repeated crystallizations. Although electrolytic chromium of high purity can be produced by this process, the complexity of the process as well as comparatively lowchromium recoveries'due to cocrystallization of chromium with-the discarded alums detracts from the commercial application of the process.
It is an object of the present invention to ob-' tain a cyclic process by which chromium-metalof high purity may be produced without the inefiiciencies of the processes" used heretofore.
Another object is to produce in. the cyclic process chromium chemicals which may be efficiently used in theelectrowinning step to form chromium metal of high purity.
Other advantages and aims of. the invention will be apparent from the following description. The single figure isv a fiow sheet illustrating the steps of the cyclic method of the invention. .In. accordance with the present. invention an iron-chromium alloy is digested with a "dilute mineral acid, for example sulfuric acid, at a temperature of between 60 and 105 C. This step is indicated in box I of the flow sheet. The resulting pulp is filtered to remove the residue which consists largely of silica. This step is indicated in box 2 of the flow sheet. The filtrate is added to a hot aqueous solution of an alkali or an alkaline earth metal base, for example sodium carbonate, under substantially non-oxidizing atmospheric conditions to a final pH below 3.8 to yield a granular basic chrome sulfate precipitate which is easily filtered and washed free of soluble salts. The precipitation step is indicated by box 3 and filtering step by box 4 of the flow sheet. The temperature of said alkali or Iii Claim. (Cl. 204-105) is indicated by box 8 of the flow sheet.
of this reduced anolyte is used to dissolve-further alkaline earth metal taining of a granular precipitate, since at less than C. the precipitate tends to become gelatinous. The hydrated basic chromium sulfate precipitate is dissolved with a portion of the reduced anolyte from the electrolysis step to" give trivalent basic chromium sulfate solutionswhich are used as electrolyte in the electrowinning step. Box 5 of the flow sheet indicatesthis step. "The solution so obtained is then increased incon-- centration by evaporation. This step is -indicated by box 6 of the flow sheet.
Hydrated basic chromium sulfate precipitate can be completely dissolved with considerably less than the calculated theoretical acid required to neutralize the basic portion of the precipitate to yield a solution containing basic chromium sulfate.
Electrolysis of such basic chromium sulfate solutions, with added neutral salts to increase conductivity, such as ammonium sulfateand sodium sulfate, in a diaphragm cell, where the bath temperature is maintained between 30-60-' 0., and the catholyte pH controlled between 1.5-2.4, results in the formation of chromium metal at the cathode and sulfuric acid'containing some chromic acid at the anode. In this-step free sulfuric acid is added to the catholyte to regulate" the pH. This step is indicated by'box 1of' the flow sheet. g
The hexavalent chromium in theanolyte is reduced to chromium valence-III with a common reducing agent, organic or inorganic. This step basic chromium sulfate precipitate to provide cell feed- The cyclic use of this reduced anolyte is-indicated by the line connecting box, 8 and box 5; of the flow sheet. The remaining reduced anolyte which contains the sulfate portion of the basic chromium sulfate precipitate as sulfuric acid is in excess and can be used to dissolve iron-chromium alloy from which further basic chromium sulfate can be derived. The cyclic use of this excess reduced anolyte is shown by the line between box 8 and box I of the flow sheet.
We have found in the precipitation step, under substantially non-oxidizing conditions, that above a final pH of about 3.8 the percentage of iron in the precipitate increases more rapidly for a given increase in pH. Thus, with the non oxidizing atmospheric condition of operation and the pH control by operating below the designated base should beabove so C. during this step in order" to insure the'ob A portionl pH range, the iron impurities can be effectively reduced to a minimum, thereby resulting in a precipitate that can be easily filtered.
However, it should be noted that as the final pH is reduced to obtain a decrease in iron content in the precipitate, there is a reduction in the percentage of the total chromium that is precipitated. Therefore, efliciency demands that the final pH must not be reduced to too low a value.
In the electrowinning step for a given bath temperature (in the operable range of 304 C.) there is a unique value of catholyte pH (in the range between 1.5 and 2.4), at which a maximum current eiliciency is obtained. In order to secure this maximum emciency the pH should 7 be controlled by adding free sulfuric acid to the catholyte chamber.
An example setting forth quantitatively the constituents at each stepff or one complete cycle of a typical operation under the process of this inventionis as follows 420 grams of high carbon ferrochromium (60.5% Cr, 24.2% Fe) was digested with 966 grams of make-up dilute sulfuric acid and'328 cc. of excess reduced anolyte which was composed of grams of trivalent chromium ion.
14.0 grams of ammonium sulfate, 8.0 grams ofv sodium sulfate, and 118 grams of sulfuric acid. Steam and water were added in the leaching step- The resulting pulp was filtered and 42 grams of residue removedwhich consisted largely of silica, but contained 2 grams of chromium and 1.0 gram of. iron. An analysis of the filtrate showed 296 grams of trivalent chromium ion, 100.8 grams of bivalent iron ion, 14 grams of ammonium sulfate, and 8 grams of sodium sulfate. When the filtrate was added to a hot aqueous solution containing 925 grams of 10% sodium carbonate, under the conditions herein disclosed, the 3382 grams of filtered basic chromium sulfate precipitate so formed were found to contain 2628 grams of water, 280 grams of chromium, 0.8 gram of.iron, and 116 grams of sulfate. The filtrate and washing was found to contain 16 grams of chromium, 14 grams of ammonium sulfate, 1248 grams of sodium sulfate, and 100 grams of iron.
The basic chromium sulfate was dissolved with 127 cc. of reduced anolyte which consisted of 38.3 grams of trivalent chromium ion, 55.0 grams of ammonium sulfate, 32.0 grams of sodium sulfate, and 460 grams of sulfuric acid. To this solution were added 14 grams of ammonium sulfate and 8.0 grams of sodium sulfate. The resultant 3905 cc. of solution contained 318.3 grams of trivalent chromium ion, 69 grams of ammonium sulfate, 40 grams of sodium sulfate, and 0.8 gram of iron. 2300 cc. of water were evaporated off and the resultant solution used as cell feed. After electrowinning under the conditions herein disclosed chromium metal of composition 270.3 grams chromium, 0.8 gram iron, was obtained. 1605 cc. of anolyte was produced containing 48 grams of hexavalent chromium ion, 69 grams of ammonium sulfate, 40 grams of sodium sulfate, and 714 grams of sulfuric acid. This anolyte was reduced'with 40 grams of molasses to'form455 cc. of reduced anolyte, 328 cc. of which was considered above as being used to leach the ferrochromium, and 127 cc. of which was described above as the dissolving agent for the granular basic chromium sulfate P p What is claimed is: In a cyclic process for the electrowinning of metallic chromium utilizing a compartment cell and an electrolyte prepared from iron-chromium alloys, the steps of digesting an iron-chromium alloy with dilute sulfuric acid at a temperature of between approximately 60 C. and 105 C. separating the leach; liquor from the residue, adding said leach liquor under substantially non-oxidizing atmospheric conditions to an aqueous solution containing a base selected from the group consisting of the alkalies and alkaline earth metal bases at a temperature above 60 C. until a final pH below approximately 3.8 is obtained to yield a-granular basic chromium sulfate precipitate, separating said granular basic chromium sulfate precipitate from said solution, dissolving said granular basic chromium sulfate precipitate in a solution of sulfuric acid, addin at least one neutral salt to such solution to increase its conductivity, evaporating excess water from such solution to form a cell feed, introducing said cell feed into the cathode compartment of a diaphragm electrolytic cell and electrolyzing to form metallic chromium at the oathode and to form in the anode compartment of such cell an anolyte containing sulfuric and chromic acids, treating said anolyte with a redueing agent to convert the chromium ions therein to the trivalent state, dissolving an additional portion of s'aidgranular basic chromium reduced anolytel I sulfate precipitate with a portion of said reduced anolyte, and leaching an additional portion of iron-chromium alloy with the excess of said MICHAEL (J. CAROSELLA.
JOHN D. METTLER.
References Cited in the file of this patent UNITED STATES PATENTS OTHER EFERENCES Lloyd et al., Journal of the Electrochemical Society, vol. 97 (July 1950) pp. 227-34.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US230413A US2651611A (en) | 1951-06-07 | 1951-06-07 | Electrowinning of chromium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US230413A US2651611A (en) | 1951-06-07 | 1951-06-07 | Electrowinning of chromium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2651611A true US2651611A (en) | 1953-09-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US230413A Expired - Lifetime US2651611A (en) | 1951-06-07 | 1951-06-07 | Electrowinning of chromium |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2651611A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3332862A (en) * | 1963-02-13 | 1967-07-25 | Yawata Iron & Steel Co | Process for treating liquid extracted from soda-roasted laterite |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2507475A (en) * | 1946-02-04 | 1950-05-09 | Crimora Res & Dev Corp | Electrodeposition of chromium |
| US2507476A (en) * | 1946-02-04 | 1950-05-09 | Crimora Res & Dev Corp | Electrodeposition of chromium |
-
1951
- 1951-06-07 US US230413A patent/US2651611A/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2507475A (en) * | 1946-02-04 | 1950-05-09 | Crimora Res & Dev Corp | Electrodeposition of chromium |
| US2507476A (en) * | 1946-02-04 | 1950-05-09 | Crimora Res & Dev Corp | Electrodeposition of chromium |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3332862A (en) * | 1963-02-13 | 1967-07-25 | Yawata Iron & Steel Co | Process for treating liquid extracted from soda-roasted laterite |
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