http://rdf.ncbi.nlm.nih.gov/pubchem/patent/GB-1358389-A

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classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C01B21-16
http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C251-88
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C01B21-16
filingDate 1971-09-06-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationDate 1974-07-03-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-1358389-A
titleOfInvention Process for the manufacture of hydrazine
abstract 1358389 Hydrazine and its salts UGINE KUHLMANN 6 Sept 1971 [7 Jan 1971] 41517/71 Heading C1A [Also in Division C2] Hydrazine is prepared by reacting ammonia and hydrogen peroxide with a ketone R 1 COR 2 , and a nitrile R 3 .CN, where R 1 and R 2 are straight or branched chain alkyl or cyclo-alkyl radicals having a maximum of 10 C atoms, or phenyl radicals possibly substituted by radicals which are stable in the reaction medium or R 1 and R 2 jointly signify a divalent straight or branched chain containing 3 to 11 carbon atoms, and R 3 is an acyclic or a cyclic radical containing less than 8 carbons or a phenyl radical possibly substituted by radicals stable in the reaction medium, the resulting ketazine and carboxyl amide formed being separated by fractional distillation, when the ketazine is hydrolysed with water or a strong acid to give hydrazine or a hydrazine salt, the ketone so liberated being recycled, the carboxylamide being dehydrated to the nitrile which is also recycled to the earlier stage. Preferably R 1 and R 2 are alkyl radicals having one to three carbon atoms and the ketone used is acetone or M.E.K. The preferred nitrile is acetonitrile. The ketazine forming reaction may be carried out in the presence of 0À01 to 2% by wt. of the reaction mix of a catalyst which is the ammonium or alkali metal salt of a mineral acid, an aliphatic or aromatic carboxylic acid, or an alkyl sulphonic or arylsulphonic acid having less than 20 carbon atoms the anions of which acids are stable under the conditions used. Preferably the ammonium salt is a salt of the acid corresponding to the nitrile used. The ketazine may be separated at a temp. below 80‹ C. The hydrolysis may be carried out with sulphuric acid or with water, when pressures in the range 1-25 bars and temps. in the range 100-200‹ C. are used. The ketazine may be partially hydrolysed with water under pressure, the hydrazine formed, separated and the residual ketazine hydrolysed with sulphuric acid. The carbonyl amide may be dehydrated in the vapour phase using a catalyst consisting of alumina impregnated with 5 to 30% by weight of phosphoric acid.
priorityDate 1971-01-07-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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