DE525924C - Process for the production of cobalt sulfide - Google Patents
Process for the production of cobalt sulfideInfo
- Publication number
- DE525924C DE525924C DEI36467D DEI0036467D DE525924C DE 525924 C DE525924 C DE 525924C DE I36467 D DEI36467 D DE I36467D DE I0036467 D DEI0036467 D DE I0036467D DE 525924 C DE525924 C DE 525924C
- Authority
- DE
- Germany
- Prior art keywords
- cobalt
- nitrite
- potassium
- parts
- production
- 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
Links
- 238000000034 method Methods 0.000 title claims description 7
- 238000004519 manufacturing process Methods 0.000 title claims 2
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 title description 6
- 229910017052 cobalt Inorganic materials 0.000 claims description 12
- 239000010941 cobalt Substances 0.000 claims description 12
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 12
- SJQCGMLIMSXKBO-UHFFFAOYSA-K potassium cobalt(2+) trinitrite Chemical compound [K+].[Co++].[O-]N=O.[O-]N=O.[O-]N=O SJQCGMLIMSXKBO-UHFFFAOYSA-K 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 150000004763 sulfides Chemical class 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- VRRFSFYSLSPWQY-UHFFFAOYSA-N sulfanylidenecobalt Chemical compound [Co]=S VRRFSFYSLSPWQY-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 6
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 6
- 150000001869 cobalt compounds Chemical class 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000004304 potassium nitrite Substances 0.000 description 4
- 235000010289 potassium nitrite Nutrition 0.000 description 4
- AZFNGPAYDKGCRB-XCPIVNJJSA-M [(1s,2s)-2-amino-1,2-diphenylethyl]-(4-methylphenyl)sulfonylazanide;chlororuthenium(1+);1-methyl-4-propan-2-ylbenzene Chemical compound [Ru+]Cl.CC(C)C1=CC=C(C)C=C1.C1=CC(C)=CC=C1S(=O)(=O)[N-][C@@H](C=1C=CC=CC=1)[C@@H](N)C1=CC=CC=C1 AZFNGPAYDKGCRB-XCPIVNJJSA-M 0.000 description 3
- 235000011054 acetic acid Nutrition 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 239000001103 potassium chloride Substances 0.000 description 3
- 235000011164 potassium chloride Nutrition 0.000 description 3
- 235000010288 sodium nitrite Nutrition 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 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 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- CAMXVZOXBADHNJ-UHFFFAOYSA-N ammonium nitrite Chemical compound [NH4+].[O-]N=O CAMXVZOXBADHNJ-UHFFFAOYSA-N 0.000 description 1
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- MIAJZAAHRXPODB-UHFFFAOYSA-N cobalt potassium Chemical compound [K].[Co] MIAJZAAHRXPODB-UHFFFAOYSA-N 0.000 description 1
- ZVLZZJUHYPMZAH-UHFFFAOYSA-L cobalt(2+) dinitrite Chemical compound [Co+2].[O-]N=O.[O-]N=O ZVLZZJUHYPMZAH-UHFFFAOYSA-L 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011572 manganese Substances 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
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002826 nitrites Chemical class 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/15—Sulfides; Oxysulfides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
Verfahren zur Gewinnung von Kobaltsulfid Die Gewinnung reiner Kobaltverbindungen aus Lösungen, die noch andere Schwermetalle, insbesondere Nickel, Zink, Mangan enthalten, ist mit großen Schwierigkeiten verbunden. Nach den üblichen Methoden wird ein unreines Kobalt erhalten, dessen endgültige Reinigung nur unter erheblichen Kobaltverlusten möglich ist.Method of Extraction of Cobalt Sulphide The extraction of pure cobalt compounds from solutions that also contain other heavy metals, in particular nickel, zinc, manganese, is fraught with great difficulties. According to the usual methods, an impure one becomes Obtained cobalt, its final cleaning only with considerable cobalt losses is possible.
Bekannt ist die in der analytischen Chemie angewandte Methode der Fällung des Kobalts mittels Kaliumnitrits und Essigsäure als Kaliumkobaltinitrit, die eine quantitative Trennung des Kobalts von den üblichen Begleitmetallen gestattet, wobei an Stelle des Kaliumnitrits auch Natriunmitrit in Verbindung mit einem Kaliumsalz treten kann. Es ist der Vorschlag gemacht worden, diese Abscheidungsmethode für Kobalt technisch nutzbar zu machen. Ihrer allgemeinen Anwendungsmöglichkeit steht jedoch der mit ihr verbundene hohe Verbrauch wertvoller Chemikalien entgegen, solange es nicht gelingt, die obenerwähnte Komplexverbindung unter Wiedergewinnung eines hohen Prozentsatzes des Nitrits und Kaliums auf einfache Kobaltverbindungen weiterzuverarbeiten.The method used in analytical chemistry is known Precipitation of cobalt using potassium nitrite and acetic acid as potassium cobalt nitrite, which allows a quantitative separation of the cobalt from the usual accompanying metals, where instead of potassium nitrite also sodium mitrite in connection with a potassium salt can kick. A proposal has been made to use this deposition method for To make cobalt technically usable. Your general application however, the associated high consumption of valuable chemicals opposes it, as long as it is it fails to recover the above-mentioned complex compound high percentage of nitrite and potassium on simple cobalt compounds.
Die aus der Literatur bekannten Methoden der Umwandlung des Kaliumkobaltinitrits erfüllen diese Forderung nicht, denn sie verlaufen entweder nur unvollständig, wie z. B. die Behandlung mittels Ätzalkalien, oder haben den Verlust des gesamten Nitrits zur Folge, wie z. B. die Zersetzung des Kaliumkobaltinitrits mittels Säuren oder durch Glühen. Eine Umsetzung mittels Schwefelverbindungen zu Kobaltsulfid wurde bereits versucht. Hierbei zeigte es sich aber, daß Schwefelwasserstoff nur von sehr geringer Wirksamkeit ist, während Ammoniumsulfid zwar rasch reagiert, dabei aber eine Wiedergewinnung des gesamten Nitrits infolge der leichten Zersetzlichkeit des entstehenden Ammoniumnitrits unmöglich-ist. Dieses ist außerdem in dem vorliegenden Falle für eine Rückführung in den Arbeitskreislauf ungeeignet.The methods known from the literature for converting potassium cobalt nitrite do not meet this requirement, because they are either incomplete, like z. B. the treatment with caustic alkalis, or have the loss of all nitrite result in such. B. the decomposition of potassium cobalt nitrite by means of acids or by glow. A conversion by means of sulfur compounds to cobalt sulfide was already tried. Here it was found, however, that hydrogen sulphide was only of very great effect is less effective, while ammonium sulfide reacts quickly, but at the same time recovery of all nitrite due to the easy decomposition of the resulting ammonium nitrite is impossible. This is also in this one Trap unsuitable for return to the working cycle.
Das nachstehend geschilderte Verfahren beruht demgegenüber auf der Verwendung der Sulfide der Alkalimetalle für die Umsetzung des Kaliumkobaltinitrits zu Kobaltsulfid. Es gestattet zum ersten Male die wirtschaftliche Trennung des Kobalts von anderen Schwermetallen über Kaliumkobaltinitrit als Zwischenprodukt bei quantitativer Ausbeute an Kobalt und unter vollständiger Wiedergewinnung des im Kaliumkobaltinitrit enthaltenen Nitrits.In contrast, the procedure outlined below is based on the Use of the sulfides of the alkali metals for the conversion of the potassium cobalt nitrite to cobalt sulfide. For the first time, it allows the cobalt to be separated economically of other heavy metals via potassium cobalt nitrite as an intermediate in quantitative Yield of cobalt and with complete recovery of that in the potassium cobalt nitrite contained nitrites.
Die möglichst konzentrierte, das Kobalt neben anderen Schwermetallen enthaltende Lösung wird in der üblichen Weise zwecks Fällung des Kaliumkobaltinitrits mit Natriumnitrit, Kaliumchlorid und Essigsäure versetzt, doch kann mit gleichem Erfolge statt Essigsäure auch Salz- oder Schwefelsäure Verwendung finden. Die Fällung verläuft quantitativ, der Niederschlag fällt in grobkristalliner, gut filtrier- und aaswaschbarer Form an. Das in Wasser aufgeschlämmte Kaliümkobaltinitrit wird nun reit Alkalisulfid zu Kobaltsuliid umgesetzt. Die Reaktion zwischen der komplexen Kobaltverbindung und Alkalisulfid verläuft ganz im Gegensatz zu der mit Ätzalkalien augenblicklich und quantitativ: -Dabei geht das gesamte im Kaliumkobaltmitrit enthaltene Kalium und Nitrit in Lösung. Bei Verwendung von Schwefelnatrium geht das Nitrit in ein Gemenge von Kalium und Natriumnitrit über, bei Verwendung von Kaliumsulfid erhält man eine reine Kaliumnitritlösung. In beiden Fällen wird das gesamte Kalium und Nitrit in Form einer wäßrigen Lösung wiedergewonnen, die nach einer etwaigen Konzentration bei einem neuen Ansatz wiederverwendet werden kann.The most concentrated one, the cobalt alongside other heavy metals containing solution is used in the usual way for the purpose of precipitation of the potassium cobalt nitrite mixed with sodium nitrite, potassium chloride and acetic acid, but the same can be used Successes instead of acetic acid, hydrochloric or sulfuric acid can also be used. The precipitation runs quantitatively, the precipitate falls in coarsely crystalline, well filterable and washable form. Potash cobalt nitrite suspended in water alkali sulfide is now converted to cobalt sulfide. The reaction between the complex cobalt compound and alkali sulfide runs quite the opposite of that with Caustic alkalis instantaneously and quantitatively: - All of this goes in the potassium cobalt mitrite contained potassium and nitrite in solution. If you use sodium sulphide it works the nitrite turns into a mixture of potassium and sodium nitrite when using Potassium sulphide gives a pure potassium nitrite solution. In both cases it will all potassium and nitrite recovered in the form of an aqueous solution, which after any concentration can be reused in a new approach.
Das ausgeschiedene Kobaltsulfid läßt sich nach den üblichen Methoden leicht auf andere reine Kobaltverbindungen aufarbeiten, indem man es z. B. abröstet oder mittels Chlors in Kobaltchlorid überführt. Beispiel Eine Lösung, welche in zooo Teilen 4o Teile Co, 28 Teile Zn, 2o Teile Mn als Sulfate enthält, wird in der Kälte mit Natriumnitrit, Kaliumchlorid und Schwefelsäure, und zwar auf r Gewichtsteil Co mit 9 Gewichtsteilen NaN 02, 5,7 Gewichtsteilen KCl, 1,8 Gewichtsteilen H@ S O , versetzt. Nach mehreren Stunden wird der entstandene Niederschlag abfiltriert und mit kaltem Wasser gewaschen.. Gefällt sind 98 °/o des Kobalts der Ausgangslösung. Das erhaltene Kaliumkobaltinitrit, enthaltend 39,2 Teile Kobalt und 177,5 Teile N 02, wird in 59o Teilen Wasser von 6o' C angerührt. Zu der Aufschlämmung wird unter Rühren so viel konzentrierte Schwefelnatriumlösung mit einem Gehalt von 151 g Na, S im Liter zugegeben, bis eben ein geringer Überschuß nachweisbar ist. Verbraucht werden 528 Volumteile Nag S-Lösung, entsprechend rot ()/o der nach der Gleichung 2 K3 Co (N02)" -f- 3 Nag S =2CoS+S+6KN02+6NaN02 theoretisch nötigen Menge. Das gesamte Kaliumkobaltinitrit ist in Kobaltsulfid umgewandelt, welches nach dem Abfiltrieren und Auswaschen auf beliebige andere reine Kobaltverbindungen weiterverarbeitet werden kann.The precipitated cobalt sulfide can easily be worked up to other pure cobalt compounds by the usual methods by z. B. roasted or converted into cobalt chloride by means of chlorine. EXAMPLE A solution which, in zooo parts, contains 40 parts Co, 28 parts Zn, 20 parts Mn as sulfates, is mixed in the cold with sodium nitrite, potassium chloride and sulfuric acid, to r part by weight of Co with 9 parts by weight of NaN 02, 5.7 parts by weight KCl, 1.8 parts by weight of H @ SO, added. After several hours, the precipitate formed is filtered off and washed with cold water. 98% of the cobalt in the starting solution is precipitated. The potassium cobalt nitrite obtained, containing 39.2 parts of cobalt and 177.5 parts of N 02, is stirred in 59o parts of water at 60.degree. Concentrated sodium sulphide solution with a content of 151 g Na, S per liter is added to the slurry with stirring until a slight excess can be detected. 528 parts by volume of Nag S solution are used, corresponding to red () / o the amount theoretically required according to the equation 2 K3 Co (N02) "-f- 3 Nag S = 2CoS + S + 6KN02 + 6NaN02. The entire potassium cobalt nitrite is in cobalt sulfide converted, which after filtering and washing can be processed further for any other pure cobalt compounds.
Im Filtrat (= 247o Völumteile) befinden sich 175,3 Gewichtsteile NO2 = 98,8 °/a der Nitritmenge des Kaliumkobaltinitrits. Zwecks Verwendung des Nitrits für eine neue Kobaltfällung wird das Filtrat auf ein Viertel des Volumens eingedampft. Ein Nitritverlust findet hierbei nicht statt, denn in dem Konzentrat werden 175,3 Gewichtsteile NO, wiedergefunden.The filtrate (= 247o parts by volume) contains 175.3 parts by weight of NO2 = 98.8 ° / a of the nitrite amount of the potassium cobalt nitrite. To use the nitrite for a new cobalt precipitation, the filtrate is evaporated to a quarter of the volume. There is no loss of nitrite here, because 175.3 parts by weight of NO are found in the concentrate.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEI36467D DE525924C (en) | 1928-12-15 | 1928-12-15 | Process for the production of cobalt sulfide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEI36467D DE525924C (en) | 1928-12-15 | 1928-12-15 | Process for the production of cobalt sulfide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE525924C true DE525924C (en) | 1931-05-30 |
Family
ID=7189261
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEI36467D Expired DE525924C (en) | 1928-12-15 | 1928-12-15 | Process for the production of cobalt sulfide |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE525924C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2456142A1 (en) * | 1979-05-10 | 1980-12-05 | Inco Ltd | PROCESS FOR SEPARATING NICKEL OR DISSOLVED COBALT OR BOTH OF AN AQUEOUS PELLET OF IRON OXIDE PARTICLES |
-
1928
- 1928-12-15 DE DEI36467D patent/DE525924C/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2456142A1 (en) * | 1979-05-10 | 1980-12-05 | Inco Ltd | PROCESS FOR SEPARATING NICKEL OR DISSOLVED COBALT OR BOTH OF AN AQUEOUS PELLET OF IRON OXIDE PARTICLES |
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