AT72604B - Process for the preparation of pure zinc oxide. - Google Patents
Process for the preparation of pure zinc oxide.Info
- Publication number
- AT72604B AT72604B AT72604DA AT72604B AT 72604 B AT72604 B AT 72604B AT 72604D A AT72604D A AT 72604DA AT 72604 B AT72604 B AT 72604B
- Authority
- AT
- Austria
- Prior art keywords
- zinc
- ammonia
- ammonium
- sulfite
- sulfur dioxide
- Prior art date
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims description 10
- 238000000034 method Methods 0.000 title claims description 10
- 239000011787 zinc oxide Substances 0.000 title claims description 5
- 238000002360 preparation method Methods 0.000 title claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 36
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 22
- 229910021529 ammonia Inorganic materials 0.000 claims description 17
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 claims description 13
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 12
- 229910052725 zinc Inorganic materials 0.000 claims description 12
- 239000011701 zinc Substances 0.000 claims description 12
- HSYFJDYGOJKZCL-UHFFFAOYSA-L zinc;sulfite Chemical compound [Zn+2].[O-]S([O-])=O HSYFJDYGOJKZCL-UHFFFAOYSA-L 0.000 claims description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- 239000003518 caustics Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 4
- 150000003751 zinc Chemical class 0.000 claims description 4
- AOSFMYBATFLTAQ-UHFFFAOYSA-N 1-amino-3-(benzimidazol-1-yl)propan-2-ol Chemical compound C1=CC=C2N(CC(O)CN)C=NC2=C1 AOSFMYBATFLTAQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000000137 annealing Methods 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 239000002253 acid Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 3
- 235000011130 ammonium sulphate Nutrition 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
- 229910001656 zinc mineral Inorganic materials 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Description
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Verfahren zur Darstellung von reinem Zinkoxyd.
Vorliegendes Verfahren beabsichtigt die Erzeugung von reinem Zinkoxyd unter Verwendung von Zinkmineralien und speziell jener Mineralien, deren Zinkgehalt zu niedrig ist, um hüttenmännisch verarbeitet zu werden oder unter Verwendung irgend eines Zinksalzes als Ausgangsmaterial.
Bisher wurde das Zink auf bekannte Weise mittels einer geeigneten Säure, wie Schwefelsäure, Salzsäure oder Salpetersäure, aus den Mineralien gelaugt ; die verwendete Säure wurde zweckmässig mit einer genügenden Menge Wasser versetzt, um ein Auskristallisieren des Zinksalzes während des Laugens zu vermeiden. Die erhaltenen Laugen wurden, wie üblich, von den fremden Metallen, die zum Teil auch von der Säure aufgelöst wurden, befreit und darauf aus denselben das Zink vermittelst Ammoniumsulfit als Zinksulfit gefällt, aus welchem letzteren nach dem Abfiltrieren und Waschen durch Glühen reines Zinkoxyd gewonnen wird, welches zu allen bekannten Verwendungen geeignet ist, namentlich als weisses Pigment für die Malerei als auch als Ausgangsmaterial zur Herstellung von reinem metallischem Zink.
Das Schwefeldioxid, welches während des Glühens entweicht, wird zur Regeneration des Ammouiumsnints verwendet.
Bei der Ausführung dieses bekannten Verfahrens pflegte man bisher so zu verfahren, dass man das Ammoniumsulfat der Zinklösung in dem gelösten Zinksalz äquivalenter Menge zugab.
Unter diesen Bedingungen wird jedoch ein Teil des verwendeten Zinkes nicht gefällt und bleibt in der Mutterlauge gelöst. Dieser Umstand ist kein Hindernis bei der Dar- stellung des Zinksulfites im Laboratorium, wird es aber bei der fabriksmässigen Erzeugung dieses Produktes, denn die Menge Zink, welche der Ausfällung entgeht, vermindert die ausbeute um 10 bis 200f0.
Bei dem vorhegendnn Verfahren werden diese Verluste vermieden und es wird fast das gesamte Zink ausgefällt, indem während oder vor der Reaktion kaustisches Ammoniak oder kohlensaures Ammoniak dem Reaktionsgemisch oder dem dazu verwendeten Ammonium- sulfit zugesetzt wird. Diese Wirkung des Ammoniaks war nicht vorauszusehen, denn be- kanntlich werden die meisten Zinkniederschläge durch einen Überschuss an Ammoniak oder kohlensaurem Ammoniak im Gegenteil wieder aufgelöst. Man kann auch das kaustische
Ammoniak oder das kohlensaure Ammoniak während oder vor der Reaktion dadurch er- zeugen, dass man dem Reaktionsgemisch oder dem dazu verwendeten Ammoniumsulfit ein
Alkali oder Erdalkali hinzufügt, welches durch doppelte Umsetzung mit dem Ammonium- sulfit Ammoniak oder kohlensaures Ammoniak erzeugt, namentlich Kalkhydrat oder kohlen- saures Natrium.
Das Schwefeldioxyd, welches während des Glühens des Zinksulfites entsteht, wird zur
Erzeugung von Ammoniumsuiit verwendet, so dass dieses immer wieder regeneriert wird, wie bereits erwähnt wurde.
Nach einem bekannten Verfahren wird Ammoniumsulfat erzeugt, indem Schwefeldioxyd in Ammoniakwaseer absorbiert wird. Dieses Verfahren würde sich-für vorliegende Erfn'dung nicht eignen, denn das Schwefeldioxyd, welches während des Glühens des Zinksulfites oder der Zinkblende entweicht, enthält eine gewisse Menge Luft, und es wurde gefunden :
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EMI2.1
oxydiert wird, wodurch ein bedeutender Verlust an Schwefeldioxyd entsteht ;
2. dass die beigemengte Luft beim Hindurchstreichon durch das wässerige Ammoniak eine bedeutende Menge Ammoniak mit sich reisst, wodurch ein Ammoniakverlust entsteht.
Es wurde weiter gefunden, dass Ammoniumsulfit bedeutend weniger oxydierbar ist bei Gegenwart von freier Säure, als bei Gegenwart von freiem Alkali, und dass man die
EMI2.2
Ammoniak absorbiert, wohl aber in einer Lösung von neutralem oder schwach saurem Ammoniumsulfat. Man könnte zu diesem Zwecke auch schwach alkalisches Ammoniumsulfit verwenden, weil eine geringe Alkalinität rasch durch das saure Schwefeldioxyd unschädlich gemacht würde.
Da bei gewöhnlicher Temperatur das Ammoniumsulfit sowie das Ammoniumbisulfit in wässeriger Lösung nicht fruchtig ist, kann auch kein Ammoniak durch den Luftstrom mitgerissen werden ; zudem wird das Ammoniumsulfit durch das absorbierte Schwefeldioxyd sofort sauer, so dass die Oxydation zu Sulfat unter diesen Bedingungen nur gering ist, wie bereits erwähnt wurde. Das im Ammoniumsulfit als Bisulfit gelöste Schwefeldioxyd wird nachträglich ausserhalb des Absorptionsapparates mit kaustischem Ammoniak neutralisiert, und. zwar in einem geschlossenen Behälter, um die Oxydation durch Luft zu vermeiden.
Das zu diesem Zwecke nötige Ammoniak wird aus dem Ammoniaksalze gewonnen, welches bei der Fällung des Zinksulfites durch doppelte Umsetzung nach folgender Gleichung
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Process for the preparation of pure zinc oxide.
The present process intends to produce pure zinc oxide using zinc minerals and especially those minerals whose zinc content is too low to be processed by metallurgy or using any zinc salt as a starting material.
So far, the zinc has been leached from the minerals in a known manner using a suitable acid such as sulfuric acid, hydrochloric acid or nitric acid; The acid used was expediently mixed with a sufficient amount of water in order to prevent the zinc salt from crystallizing out during the leaching process. As usual, the alkaline solutions obtained were freed from the foreign metals, some of which were also dissolved by the acid, and the zinc was then precipitated as zinc sulfite by means of ammonium sulfite, from which pure zinc oxide was obtained after filtering and washing by annealing , which is suitable for all known uses, namely as a white pigment for painting and as a starting material for the production of pure metallic zinc.
The sulfur dioxide that escapes during the glow is used to regenerate the ammouium snint.
In carrying out this known process, the procedure used to date was to add the ammonium sulfate to the zinc solution in an equivalent amount to the dissolved zinc salt.
Under these conditions, however, some of the zinc used is not precipitated and remains dissolved in the mother liquor. This circumstance is not an obstacle to the preparation of zinc sulphite in the laboratory, but it becomes so in the case of the factory production of this product, for the amount of zinc which escapes the precipitation reduces the yield by 10 to 200%.
In the above process, these losses are avoided and almost all of the zinc is precipitated by adding caustic ammonia or carbonate of ammonia to the reaction mixture or to the ammonium sulfite used for this purpose during or before the reaction. This effect of ammonia could not be foreseen, because it is well known that most zinc precipitates are dissolved again by an excess of ammonia or carbonate of ammonia. You can also do the caustic
Generate ammonia or the carbonic acid ammonia during or before the reaction by adding to the reaction mixture or the ammonium sulfite used for this purpose
Adds alkali or alkaline earth which, through double reaction with ammonium sulphite, produces ammonia or carbonate of ammonia, namely hydrated lime or carbonate of sodium.
The sulfur dioxide that is produced during the glowing of the zinc sulphite becomes
Generation of Ammoniumsuiit used, so that this is regenerated again and again, as already mentioned.
According to a known method, ammonium sulfate is produced by absorbing sulfur dioxide in ammonia water. This process would not be suitable for the present invention, because the sulfur dioxide which escapes during the glowing of the zinc sulphite or the zinc blende contains a certain amount of air, and it was found:
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EMI2.1
is oxidized, resulting in a significant loss of sulfur dioxide;
2. that the added air, when passing through the aqueous ammonia, carries with it a significant amount of ammonia, causing a loss of ammonia.
It was also found that ammonium sulfite is significantly less oxidizable in the presence of free acid than in the presence of free alkali, and that the
EMI2.2
Ammonia absorbed, but probably in a solution of neutral or weakly acidic ammonium sulfate. One could also use weakly alkaline ammonium sulphite for this purpose, because a low alkalinity would quickly be rendered harmless by the acidic sulfur dioxide.
Since ammonium sulfite and ammonium bisulfite in aqueous solution are not fruity at normal temperature, ammonia cannot be carried away by the air flow; In addition, the ammonium sulfite becomes immediately acidic due to the absorbed sulfur dioxide, so that the oxidation to sulfate is only slight under these conditions, as already mentioned. The sulfur dioxide dissolved in the ammonium sulfite as bisulfite is subsequently neutralized outside the absorption apparatus with caustic ammonia, and. in a closed container to avoid oxidation by air.
The ammonia required for this purpose is obtained from the ammonia salt, which is produced in the precipitation of the zinc sulfite by double conversion according to the following equation
EMI2.3
Claims (1)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE1474X | 1912-12-07 |
Publications (1)
Publication Number | Publication Date |
---|---|
AT72604B true AT72604B (en) | 1916-10-25 |
Family
ID=89537694
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
AT72604D AT72604B (en) | 1912-12-07 | 1913-12-06 | Process for the preparation of pure zinc oxide. |
Country Status (4)
Country | Link |
---|---|
AT (1) | AT72604B (en) |
FR (1) | FR465816A (en) |
GB (1) | GB191328188A (en) |
NL (1) | NL1474C (en) |
-
1913
- 1913-12-06 FR FR465816A patent/FR465816A/en not_active Expired
- 1913-12-06 GB GB191328188D patent/GB191328188A/en not_active Expired
- 1913-12-06 AT AT72604D patent/AT72604B/en active
- 1913-12-06 NL NL3751A patent/NL1474C/en active
Also Published As
Publication number | Publication date |
---|---|
FR465816A (en) | 1914-04-28 |
NL1474C (en) | 1916-08-01 |
GB191328188A (en) | 1915-07-15 |
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