DE2343052C3 - Process for the preparation of the aluminum salt of N-nitroso-N-cyclohexylhydroxylamine - Google Patents
Process for the preparation of the aluminum salt of N-nitroso-N-cyclohexylhydroxylamineInfo
- Publication number
- DE2343052C3 DE2343052C3 DE19732343052 DE2343052A DE2343052C3 DE 2343052 C3 DE2343052 C3 DE 2343052C3 DE 19732343052 DE19732343052 DE 19732343052 DE 2343052 A DE2343052 A DE 2343052A DE 2343052 C3 DE2343052 C3 DE 2343052C3
- Authority
- DE
- Germany
- Prior art keywords
- salt
- nitroso
- solution
- aluminum
- cyclohexylhydroxylamine
- 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
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical class [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 10
- 238000000034 method Methods 0.000 title claims description 6
- 238000002360 preparation method Methods 0.000 title claims description 3
- LXCJGJYAOVCKLO-UHFFFAOYSA-N N-cyclohexyl-N-hydroxynitrous amide Chemical compound O=NN(O)C1CCCCC1 LXCJGJYAOVCKLO-UHFFFAOYSA-N 0.000 title description 3
- 239000000243 solution Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 159000000001 potassium salts Chemical class 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- OXSRSCRBMKYOKX-UHFFFAOYSA-N aluminum;N-cyclohexylhydroxylamine Chemical compound [Al].ONC1CCCCC1 OXSRSCRBMKYOKX-UHFFFAOYSA-N 0.000 claims description 2
- 150000001447 alkali salts Chemical class 0.000 claims 4
- 239000003929 acidic solution Substances 0.000 claims 3
- 241001676573 Minium Species 0.000 claims 1
- ADXYMYHMDXYUNI-UHFFFAOYSA-N N-hexylhydroxylamine Chemical compound CCCCCCNO ADXYMYHMDXYUNI-UHFFFAOYSA-N 0.000 claims 1
- 230000002378 acidificating Effects 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000001264 neutralization Effects 0.000 claims 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 159000000000 sodium salts Chemical class 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K Aluminium chloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 230000000875 corresponding Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H Aluminium sulfate Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- VXVTWBRLTJLQBZ-UHFFFAOYSA-N N-cyclohexyl-N-hydroxynitrous amide;potassium Chemical compound [K].O=NN(O)C1CCCCC1 VXVTWBRLTJLQBZ-UHFFFAOYSA-N 0.000 description 1
- NRRQGHTXRQKQCJ-UHFFFAOYSA-N [Al].NO Chemical compound [Al].NO NRRQGHTXRQKQCJ-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- KRVHVYOPJDYDPS-UHFFFAOYSA-N aluminum;N-cyclohexyl-N-hydroxynitrous amide Chemical compound [Al].O=NN(O)C1CCCCC1 KRVHVYOPJDYDPS-UHFFFAOYSA-N 0.000 description 1
- -1 hexylhydroxylamine potassium salt Chemical compound 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
Description
"~~"~~"~ Beispiel"~~" ~~ "~ example
30 Teile (Gewichtsteile) einer 30%igen (Gewichts-30 parts (parts by weight) of a 30% (weight
Die vorliegende Erfindung betrifft ein wertvolles prozent) wäßrigen Lösung des N-Nitroso-N-cycloneues Verfahren zur Herstellung des Aluminiumsalzes »ο hexylhydroxylamin-Kaliumsalzes werden mit 30 Teilen von N-Nitroso-N-cyclohexylhydroxylamin unter Kon- Wasser verdünnt und durch Zusatz von verdünnter trolle des pH-Wertes. Schwefelsäure (50%ig) auf einen pH-Wert von 7 bis 8The present invention relates to a valuable percent) aqueous solution of N-nitroso-N-cycloneues Process for the preparation of the aluminum salt »ο hexylhydroxylamine potassium salt are with 30 parts of N-nitroso-N-cyclohexylhydroxylamine under water and diluted by adding dilute troll the pH. Sulfuric acid (50%) to a pH value of 7 to 8
Es ist bekannt, daß man aus der wäßrigen Lösung eingestellt. Man kühlt die Lösung auf 00C ab und läßt des N-Nitroso-N-cyclohexylhydroxylamin-Kaliumsal- eine Lösung aus 11,1 Teilen A12(SO4)3 · 18 H2O und zes durch doppelte Umsetzung mit Aluminiumsalzen 25 25 Teilen Wasser, die mit verdünnter Schwefelsäure von Mineralsäuren, beispielsweise Aluminiumchlorid (50%ig) auf einen pH-Wert von 1,5 bis 2 eingestellt oder Aluminiumsulfat, das N-Nitroso-N-cyclohexyl- wurde, rasch zulaufen. Die entstandene Fällung wird hydroxylamin-Aluminiumsalz erhält. nach einstündigem Nachrühren abfiltriert, mit WasserIt is known that one adjusts from the aqueous solution. The solution is cooled to 0 ° C. and the N-nitroso-N-cyclohexylhydroxylamine potassium salt is allowed to form a solution of 11.1 parts of A1 2 (SO 4 ) 3 · 18 H 2 O and zes by double reaction with aluminum salts 25 25 Parts of water which have been adjusted to a pH of 1.5 to 2 with dilute sulfuric acid of mineral acids, for example aluminum chloride (50%), or aluminum sulfate, which is N-nitroso-N-cyclohexyl, run in rapidly. The resulting precipitate is obtained as hydroxylamine aluminum salt. filtered off after stirring for one hour, with water
Man geht so vor, daß man eine verdünnte wäßrige sulfatfrei gewaschen und bei 60 bis 65 0C getrocknet.
Lösung des Kaliumsalzes auf 00C abkühlt, die in der 30 Man erhält 7,5 Teile N-Nitroso-N-cyclohexylhy-Lösung
vorhandene Kalilauge neutralisiert und eine droxylamin-Aluminiumsalz, das frei ist von dem obenwäßrige
Lösung eines Aluminiumsalzes einer Mineral- erwähnten Nebenprodukt,
säure zugibt. Verwendet man dagegen eine in üblicher WeiseThe process is performed so that one washed free of sulphate a dilute aqueous solution, and dried at 60 to 65 0 C. Solution of potassium salt cooled to 0 0 C, neutralized in the 30 Man 7.5 parts obtained N-nitroso-N-cyclohexylhy solution existing potassium hydroxide solution and a droxylamin aluminum salt which is free of the obenwäßrige solution mentioned an aluminum salt of a mineral By-product,
adding acid. On the other hand, if you use one in the usual way
Die entstandene Fällung wird abgetrennt, mit durch Auflösen von 11,1 Teilen A12(SO4)3 · 18 H2O in Wasser gewaschen und bei niedriger Temperatur ge- 35 25 Teilen Wasser erhaltene Lösung für die Umsetzung trocknet. (entsprechend GB-PS 815 537), dann enthält die inThe precipitate formed is separated off, washed with the solution obtained by dissolving 11.1 parts of A1 2 (SO 4 ) 3 · 18 H 2 O in water and dried for the reaction at a low temperature. (corresponding to GB-PS 815 537), then the in
Es zeigte sich, daß bei dieser Fällung des N-Nitroso- entsprechender Weise aufgearbeitete Fällung mben N-cyclohexylhydroxylamin-Aluminiumsalzes ein Ne- 7,2 Teilen N-Nitroso-N-cydohexylhydroxylamin-Alubenprodukt mit einem Schmelzpunkt von über 36O°C miniumsalz noch 0,2 bis 0,4 Teile des obenerwähnten entsteht. 40 Nebenprodukts, das im Gegensatz zu dem Alum nium-It was found that in this precipitation of the N-nitroso the precipitate was worked up in a manner corresponding to that N-cyclohexylhydroxylamine aluminum salt, a Ne 7.2 parts N-nitroso-N-cyclohexylhydroxylamine aluminum product with a melting point of more than 360 ° C miniumsalz still 0.2 to 0.4 parts of the above-mentioned arises. 40 by-product, which in contrast to the aluminum
Es wird vermutet, daß das Alumination Al(OH)4, salz in organischen Lösungsmitteln unlöslich ist. Nach (ähnlich wie das Silikation) unter Wasseraustritt zu dem erfindungsgemäßen Verfahren wird also eine Poly-Aluminationen kondensiert unter Einschluß eines größere Menge eines reinen Produktes erhalten als Mols N-Nitroso-N-cyclohexylhydroxylamin. nach üblichen Verfahren.It is assumed that the Alumination Al (OH) 4 , salt is insoluble in organic solvents. After (similar to the silication) with the escape of water to the process according to the invention, a polyaluminum condensed with inclusion of a larger amount of a pure product is obtained than moles of N-nitroso-N-cyclohexylhydroxylamine. according to usual procedures.
Claims (1)
gekennzeichnet, daß man für die Um- Für die Lösung des Alkalisalzes von N-Nitroso-Process for the preparation of the aluminum salt pH 6.5 to 8 and a strongly acidic solution of N-nitroso-Nrcyclohexylhydroxylamin by 5 of the aluminum salt with a pH value of 1 to 2.5 double conversion of an approximately neutral aqueous used. The alkali salt is to be understood as the potassium salt or solution of an alkali salt of N-nitroso-N-cyclo- the sodium salt or its mixture, hexylhydroxylamine with a pH of 6.5. The potassium salt is preferred. Under the Mineralbis 8 to be adjusted with the acidic aqueous solution of an aluminum acid, sulfuric acid or nitric acid. minium salt of a mineral acid, which means that sulfuric acid is preferred,
characterized that for the solution of the alkali salt of N-nitroso-
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19732343052 DE2343052C3 (en) | 1973-08-25 | Process for the preparation of the aluminum salt of N-nitroso-N-cyclohexylhydroxylamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19732343052 DE2343052C3 (en) | 1973-08-25 | Process for the preparation of the aluminum salt of N-nitroso-N-cyclohexylhydroxylamine |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| DE2343052A1 DE2343052A1 (en) | 1975-03-27 |
| DE2343052B2 DE2343052B2 (en) | 1975-12-11 |
| DE2343052C3 true DE2343052C3 (en) | 1976-07-15 |
Family
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