DE235765C - - Google Patents
Info
- Publication number
- DE235765C DE235765C DENDAT235765D DE235765DA DE235765C DE 235765 C DE235765 C DE 235765C DE NDAT235765 D DENDAT235765 D DE NDAT235765D DE 235765D A DE235765D A DE 235765DA DE 235765 C DE235765 C DE 235765C
- Authority
- DE
- Germany
- Prior art keywords
- aluminum
- nitrogen compounds
- alkali
- nitrogen
- admixtures
- 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.)
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- PIGFYZPCRLYGLF-UHFFFAOYSA-N aluminum nitride Chemical class [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 4
- 150000002830 nitrogen compounds Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims 1
- 238000006011 modification reaction Methods 0.000 claims 1
- 239000003513 alkali Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000004927 clay Substances 0.000 description 4
- 229910052570 clay Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N AI2O3 Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- YVKMMZAFUFUAAX-UHFFFAOYSA-N aluminum;tetrahydrate Chemical compound O.O.O.O.[Al] YVKMMZAFUFUAAX-UHFFFAOYSA-N 0.000 description 2
- 229910001570 bauxite Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910017083 AlN Inorganic materials 0.000 description 1
- 241001648288 Kineosporiaceae Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive Effects 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- SMYKVLBUSSNXMV-UHFFFAOYSA-J aluminum;tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-J 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- TWXTWZIUMCFMSG-UHFFFAOYSA-N nitride(3-) Chemical compound [N-3] TWXTWZIUMCFMSG-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
KAISERLICHESIMPERIAL
PATENTAMT.PATENT OFFICE.
PATENTSCHRIFTPATENT LETTERING
- M 235765 KLASSE 12k. GRUPPE- M 235765 CLASS 12 k. GROUP
Verfahren zur Darstellung von Ammoniak-Zusatz zum Patente 235300 vom 16. September 1909. Process for the preparation of ammonia additive to patent 235300 dated September 16, 1909.
Patentiert im Deutschen Reiche vom 29. Dezember 1909 ab. Längste Dauer: 15. September 1924.Patented in the German Empire on December 29, 1909. Longest duration: September 15, 1924.
In dem Patent 235300 ist gezeigt worden, daß man Gemische von Aluminiumstickstoffverbindungen mit Stickstoffverbindungen anderer Elemente und eventuell anderen Beimengungen derart zersetzen kann, daß zunächst nur die Stickstoffverbindungen des Aluminiums zersetzt werden, wodurch man zu reinen, wertvollen Aluminiumverbindungen gelangt. Es wurde nun gefunden, daß dieses Verfahren auch in den Fällen ausführbar und von großer technischer Bedeutung ist, in denen es sich um die Verarbeitung von Aluminiumstickstoffverbindungen handelt, die keine anderen Stickstoffverbindungen, sondern nur Beimengungen sonstiger Art enthalten. Es ist hierdurch möglich, aus unreinen Aluminiumstickstoffverbindungen, wie sie technisch aus wohlfeiler, unreiner Tonerde, z. B. rohem Bauxit, leicht erhältlich sind, auf bequemem Wege neben Ammoniak eine sehr reine, z. B. für die Aluminiumfabrikation geeignete, Tonerde zu gewinnen. Man kann hierbei auch so verfahren, daß man das Rohnitrid zunächst mit Wasser erhitzt oder mit Wasserdampf behandelt und hierauf die Säure oder das Alkali zufügt.It has been shown in the 235300 patent that one can produce mixtures of aluminum nitrogen compounds can decompose with nitrogen compounds of other elements and possibly other admixtures in such a way that initially only the Nitrogen compounds of aluminum are decomposed, resulting in pure, valuable ones Aluminum compounds. It has now been found that this method is feasible and of great importance even in cases technical importance is, in which it concerns the processing of aluminum nitrogen compounds acts that contain no other nitrogen compounds, but only admixtures of other kinds. This makes it possible from impure aluminum-nitrogen compounds, as they are technically from cheaper, impure ones Clay, e.g. B. raw bauxite, are readily available, conveniently in addition to ammonia a very pure, z. B. suitable for aluminum production to win alumina. The procedure here can also be such that the raw nitride is first heated with water or treated with steam and then adding the acid or alkali.
Besonders vorteilhaft hat sich die Behandlung mit Ätzalkalilauge in solchen Mengen erwiesen, daß auf je 1 Molekül in dem Rohprodukt enthaltenen Aluminiumnitrids (als AlN betrachtet) etwa ι bis 2 (im Mittel also etwa 1,5) Moleküle Alkalihydroxyd kommen.Treatment with caustic alkali has proven to be particularly advantageous in such quantities that for every 1 molecule of aluminum nitride contained in the crude product (considered as AlN ) there are about ι to 2 (on average about 1.5) molecules of alkali hydroxide.
100 kg rohes Stickstoffaluminium mit 28 Prozent gebundenem Stickstoff und einem reichliehen Gehalt an Eisen, unveränderter Tonerde, Siliciumverbindungen, Kohle u. dgl. werden im Rührautoklaven mit 120 kg Ätznatron und 600 kg Wasser langsam erwärmt und 3 Stunden auf 120 bis 130 ° gehalten, wobei das entwickelte Ammoniak zeitweise oder stetig abgelassen wird. Zum Schluß läßt - man behufs völliger Austreibung der letzten Ammoniakanteile einige Zeit unter Anlegung eines Minderdrucks kochen, wobei gleichzeitig eine Konzentration der Lösung erfolgt, filtriert und behandelt das Filtrat zwecks Ausfällung der Tonerde in bekannter Weise mit einer kleinen Menge kristallisierten Tonerdehydrats unter Schütteln oder Rühren. Man erhält eine sehr reine, z. B; für die Aluminiumfabrikation unmittelbar brauchbare Tonerde. 100 kg of raw nitrogen aluminum with 28 percent bound nitrogen and a rich one Contents of iron, unchanged alumina, silicon compounds, coal and the like are in the Stirring autoclave with 120 kg of caustic soda and 600 kg of water slowly heated for 3 hours kept at 120 to 130 °, with the evolved ammonia drained temporarily or continuously will. At the end - a few are left in order to completely expel the last of the ammonia Boil time while applying a reduced pressure, while simultaneously increasing the concentration of the solution takes place, filtered and treated the filtrate for the purpose of precipitation of the clay in a known manner Way with a small amount of crystallized alumina hydrate while shaking or stirring. A very pure, e.g. B; for aluminum production immediately usable clay.
Die Konzentration der Alkalilauge kann auch höher oder niedriger (100Be. und darunter) gewählt werden; auch kann man natürlich statt reiner Alkalilauge z. B. die nach Ausfällung des Tonerdehydrats aus Aluminatlaugen nach dem Bayersclaen Verfahren zurückbleibendenThe concentration of the alkali lye can also be chosen to be higher or lower (10 0 Be. And below); you can of course instead of pure alkali z. B. those remaining after precipitation of the alumina hydrate from aluminate liquors by the Bayersclaen process
Laugen unter Berücksichtigung ihres Tonerdegehalts verwenden. Die Zersetzung kann ferner auch schon bei einer Temperatur von ioo° und darunter vorgenommen werden, und man kann das Stickstoffaluminium und die Alkalilauge allmählich zusammenbringen. Weiterhin kann die Entfernung der in den Laugen gelösten Ammoniakreste statt durch Minderdruck auch durch Hindurchleiten indifferenter Gase er-Die verbleibenden Rückstände können in der Regel, falls sie noch genügend Tonerde enthalten, eventuell mit Bauxit gemischt, von neuem für die Herstellung von Aluminiumstickstoffverbindungen verwertet werden.Use alkalis taking into account their alumina content. The decomposition can also can also be carried out at a temperature of 100 ° and below, and one can gradually bring the nitrogen aluminum and the alkali together. Furthermore, the Removal of the ammonia residues dissolved in the alkaline solutions instead of using reduced pressure by passing indifferent gases through, the remaining residues can usually, if they still contain enough clay, possibly mixed with bauxite, again for the production of aluminum-nitrogen compounds be recycled.
ίο folgen.ίο follow.
Claims (2)
Publications (1)
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