US3775270A - Process for the electrolytic refining of potassium - Google Patents
Process for the electrolytic refining of potassium Download PDFInfo
- Publication number
- US3775270A US3775270A US00106593A US3775270DA US3775270A US 3775270 A US3775270 A US 3775270A US 00106593 A US00106593 A US 00106593A US 3775270D A US3775270D A US 3775270DA US 3775270 A US3775270 A US 3775270A
- Authority
- US
- United States
- Prior art keywords
- potassium
- electrolyte
- aluminium
- sodium
- electrolysis
- 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
- 238000000034 method Methods 0.000 title claims abstract description 12
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title abstract description 42
- 229910052700 potassium Inorganic materials 0.000 title abstract description 38
- 239000011591 potassium Substances 0.000 title abstract description 38
- 238000007670 refining Methods 0.000 title abstract description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052793 cadmium Inorganic materials 0.000 claims description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 abstract description 27
- 238000005868 electrolysis reaction Methods 0.000 abstract description 16
- 150000001875 compounds Chemical class 0.000 abstract description 11
- ZXRRHFSTAFVGOC-UHFFFAOYSA-N [AlH3].[K] Chemical compound [AlH3].[K] ZXRRHFSTAFVGOC-UHFFFAOYSA-N 0.000 abstract description 8
- 230000008018 melting Effects 0.000 abstract description 8
- 238000002844 melting Methods 0.000 abstract description 8
- 239000003701 inert diluent Substances 0.000 abstract description 3
- 239000012442 inert solvent Substances 0.000 abstract description 3
- 125000002370 organoaluminium group Chemical group 0.000 abstract description 2
- 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 description 12
- 229910052708 sodium Inorganic materials 0.000 description 12
- 239000011734 sodium Substances 0.000 description 12
- 230000008021 deposition Effects 0.000 description 11
- 229910000567 Amalgam (chemistry) Inorganic materials 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- MJGFBOZCAJSGQW-UHFFFAOYSA-N mercury sodium Chemical compound [Na].[Hg] MJGFBOZCAJSGQW-UHFFFAOYSA-N 0.000 description 3
- 150000003112 potassium compounds Chemical class 0.000 description 3
- 229910001023 sodium amalgam Inorganic materials 0.000 description 3
- 229910000497 Amalgam Inorganic materials 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- YCNZFPXXIWEFCF-UHFFFAOYSA-N alumane;sodium Chemical compound [Na].[AlH3] YCNZFPXXIWEFCF-UHFFFAOYSA-N 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 230000001427 coherent effect Effects 0.000 description 2
- -1 for example Inorganic materials 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002902 organometallic compounds Chemical class 0.000 description 2
- 150000003388 sodium compounds Chemical class 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- MRMOZBOQVYRSEM-UHFFFAOYSA-N tetraethyllead Chemical group CC[Pb](CC)(CC)CC MRMOZBOQVYRSEM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/02—Electrolytic production, recovery or refining of metals by electrolysis of melts of alkali or alkaline earth metals
Definitions
- ABSTRACT A process for refining potassium electrolytically using an organo-aluminium potassium complex compound as electrolyte in which the electrolyte used contains potassium-aluminium tetra-alkyl compounds and the electrolysis is effected at a temperature of not above 70C.
- the electrolysis is carried out at a temperature within the range of 64 70C and the melting point of the electrolyte is lowered to this range or below it by the addition of a potassiumaluminum-monoalkoxyalkyl compound or an inert solvent or diluent.
- This invention relates to a process for the electrolytic refining of potassium.
- the electrolytes mostsuitable for the separation of sodium consist either totally or to a high percentage of sodium-aluminium tetraethyl.
- the capacity for smoothly separating out the sodium metal, and in fact in molten form, from such electrolytes is possible be.- cause the electrolyte is completely stable at the elec trolysis temperatures (100 140C) with respect to molten sodium-aluminium tetraethyl.
- molten potassium is active with respect to potassium-aluminium tetraethyl and the electrolyte slowly becomesdecomposed, finely divided aluminium separating out. Consequently the separation of the potassium in a coherent, liquid form in appreciable amounts is made impossible.
- An electrolytic arrangement which has constantly to supply potassium at the cathode without any disturbance and over a relatively long time period, it is a requirement that the metal is separate out in a layer which coheres satisfactorily, from which layer it is possible at a suitable position either to skim off the liquid potassium or to remove it by way of an overflow.
- Suitable additives of this nature are, for example, potassium-monoalkoxy-triethyl-aluminium compounds of the general formula l([ROAl(C l-l in which 1 the radical R preferably represents a hydrocarbon radical with at least three carbon atoms, for example, threeto 10 carbon atoms. It is true that they lower the conductivity of the potassium-aluminium tetraethyl, but not so strongly that the electrolysis would be impossible.
- adjusting the melting point of the electrolyte to a suitable degree is the concurrent use of limited quantities of inert solvents or diluents for the organic potassium complex compound used as electrolyte.
- Particularly suitable for this purpose can be ethers of sufficiently high-boiling point as well as inert hydrocarbons, for example, of the toluene type.
- the main compound of the electrolyte is potassiumaluminum tetraalkyl, and alkyl radicals with up to 2 carbon atoms are preferred. Potassium-aluminium tetraethyl is especially suitable.
- the electrolytic deposition of potassium offers a distinct advantage as compared with the electrolytic deposition of sodium.
- the electrolytic deposition of sodium from the analogous sodiumcontaining complex compounds (or even their mixtures with complex potassium compounds, from which, up to a relatively high potassium content, only sodium is deposited)
- the densities of the molten sodium and of the molten electrolyte are normally so very close to one another that the problem of a clean, spontaneous layer formation arises, for the solution of which problem certain measures have proved to be advantageous (German Pat. No. 1,168,651).
- the molten potassium in the molten state at 6370C is of substantially lower specific gravity than the molten electrolyte and consequently is certain to rise to the top in the electrolysis cell.
- the deposition of the potassium from potassium amalgam can consequently be operated in a particularly simple manner in accordance with the known principle of the so-called three-layer electrolysis.
- the starting material containing potassium, for example, potassium amalgam, as the lowermost layer is covered with the molten electrolyte.
- the potassium product purified by the procedure of electrolysis separates out at the top as a third layer on the electrolyte.
- the crude potassium can be alloyed with a small quantity of mercury, in which case an amalgam is obtained which is of decidedly greater specific gravity than the electrolyte, and then the electrolysis is once again operated in the usual way by the principle of the three-layer process.
- EXAMPLE Disposed on the bottom of a cylindrical electrolysis vessel are 3240 g of 0.516 percent potassium amalgam as anode, while arranged above the anode at a spacing of about 0.7 cm is an upwardly open, cylindrical basket made of a copper lattice with 25 meshes per square centimetre, which is provided with a cadmium coating in a thickness of about 100 p. for the better adhesion of the alkali metal.
- the basket is immersed to about two-thirds to three-fourths into the electrolyte melt.
- the potassium which separates is of lower specific gravity than the electrolyte and ascends in the basket to the surface of the liquid and can be withdrawn from this surface at intervals.
- Electrolyte 27.3 g( 150 m.mol)-potassium tetraethyl-aluminium 17.0 g( m.mol)potassium triethyl-aluminium butoxide Temp: 67-69C Voltage: 4 volts Current strength: 0.2 ampere Anode surface: 12.6 cm Cathode surface, calculated only for underside of basket: 6.25 cm 2.68 amp-hours supply 3.9 g of potassium of melting point 630C; the melting point is about 05C higher than that of a comparison sample of commercial potassium.
- a process for cathodic deposition of pure potassium which comprises electrolyzing between an anode which is a potassium amalgam and a cathode for deposit of pure potassium at a temperature of about 6470C. an electrolyte consisting essentially of potassium aluminium tetraethyl and enough K [ROAl (C H wherein wherein R is an alkyl radical of three to 10 carbon atoms to lower the melting point of said tetraethyl compound to said temperature range, for deposition of the pure potassium at the cathode.
Landscapes
- 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)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19702001409 DE2001409A1 (de) | 1970-01-14 | 1970-01-14 | Verfahren zur elektrolytischen Raffination von Kalium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3775270A true US3775270A (en) | 1973-11-27 |
Family
ID=5759566
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US00106593A Expired - Lifetime US3775270A (en) | 1970-01-14 | 1971-01-14 | Process for the electrolytic refining of potassium |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US3775270A (enExample) |
| AT (1) | AT302675B (enExample) |
| BE (1) | BE761391A (enExample) |
| CA (1) | CA926339A (enExample) |
| CH (1) | CH537981A (enExample) |
| DE (1) | DE2001409A1 (enExample) |
| FR (1) | FR2080906B1 (enExample) |
| GB (1) | GB1294251A (enExample) |
| NL (1) | NL7100318A (enExample) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3028323A (en) * | 1959-12-24 | 1962-04-03 | Ethyl Corp | Manufacture of organolead products |
| US3028322A (en) * | 1962-04-03 | Malmei | ||
| GB955252A (en) * | 1959-05-06 | 1964-04-15 | Kabl Ziegler | Process for the electrolytic precipitation of sodium |
| US3234114A (en) * | 1961-06-30 | 1966-02-08 | Ziegler Karl | Process for the recovery of purified sodium |
-
1970
- 1970-01-14 DE DE19702001409 patent/DE2001409A1/de active Pending
- 1970-12-22 CH CH1895470A patent/CH537981A/de not_active IP Right Cessation
-
1971
- 1971-01-04 GB GB281/71A patent/GB1294251A/en not_active Expired
- 1971-01-07 CA CA102180A patent/CA926339A/en not_active Expired
- 1971-01-08 BE BE761391A patent/BE761391A/xx unknown
- 1971-01-11 NL NL7100318A patent/NL7100318A/xx unknown
- 1971-01-13 FR FR717101005A patent/FR2080906B1/fr not_active Expired
- 1971-01-14 US US00106593A patent/US3775270A/en not_active Expired - Lifetime
- 1971-01-14 AT AT29671A patent/AT302675B/de active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3028322A (en) * | 1962-04-03 | Malmei | ||
| GB955252A (en) * | 1959-05-06 | 1964-04-15 | Kabl Ziegler | Process for the electrolytic precipitation of sodium |
| US3028323A (en) * | 1959-12-24 | 1962-04-03 | Ethyl Corp | Manufacture of organolead products |
| US3234114A (en) * | 1961-06-30 | 1966-02-08 | Ziegler Karl | Process for the recovery of purified sodium |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2080906A1 (enExample) | 1971-11-26 |
| FR2080906B1 (enExample) | 1973-05-25 |
| BE761391A (fr) | 1971-07-08 |
| CA926339A (en) | 1973-05-15 |
| AT302675B (de) | 1972-10-25 |
| DE2001409A1 (de) | 1971-07-22 |
| GB1294251A (en) | 1972-10-25 |
| NL7100318A (enExample) | 1971-07-16 |
| CH537981A (de) | 1973-06-15 |
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