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公开(公告)号:DE1956908A1
公开(公告)日:1970-06-18
申请号:DE1956908
申请日:1969-11-12
Applicant: STAMICARBON
Inventor: HERMANUS DE ROOIJ ABRAHAM , ELMENDORP JAN
Abstract: 1287302 Oximes STAMICARBON NV 11 Nov 1969 [12 Nov 1968] 55238/69 Heading C2C In a continuous process for the production of an oxime in which an aqueous reaction medium is recycled between a hydroxylamine saltforming zone in which nitrate ions are catalytically reduced with molecular hydrogen and an oxime formation zone in which hydroxylamine salt is reacted with a ketone or an aldehyde, the nitrate ions in the said aqueous reaction medium are replenished by absorption of nitrous gases, i.e. a mixture of NO 2 and NO therein to form nitric acid. The preparation is described of cyclohexanone oxime, referring to Figs. 1-3 (not shown).
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公开(公告)号:DE1620468A1
公开(公告)日:1970-04-30
申请号:DEST023466
申请日:1965-03-05
Applicant: STAMICARBON
Inventor: HERMANUS DE ROOIJ ABRAHAM
IPC: C07D201/16
Abstract: Lactams, particularly e - caprolactams, obtained in a concentrated sulphuric acid medium (which may contain free SO3) by e.g. a nitrosation or Beckman re-arrangement reaction, are separated from the sulphuric acid to which they are bound, by addition of an aqueous solution of ammonium sulphate, in such an amount that the molar ratio between ammonium sulphate and sulphuric acid in the medium is at least 0.75:1 and preferably not greater than 2:1. The lactam thus converted to the free base is then separated from the acid solution, for example by extraction with an organic solvent. Specified solvents are benzene, toluene, 1,2-dichloroethane, chloroform, ethyl ether, dibutyl carbitol.
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公开(公告)号:DE2059582A1
公开(公告)日:1971-06-16
申请号:DE2059582
申请日:1970-12-03
Applicant: STAMICARBON
IPC: C07C251/46 , C01B21/14 , C07C67/00 , C07C239/00
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公开(公告)号:DE1567832A1
公开(公告)日:1970-08-20
申请号:DE1567832
申请日:1965-05-06
Applicant: STAMICARBON
Inventor: HERMANUS DE ROOIJ ABRAHAM
Abstract: A solution containing a hydroxylammonium salt is prepared by catalytically reducing with the aid of molecular hydrogen a nitrate solution which has a pH of from 0-3 obtained by the addition to the solution of either phosphoric acid or a bisulphate. The solution preferably also contains a soluble sulphate or phosphate of such a type and amount that the solution is buffered at said pH. Suitable mixtures are phosphoric acid and ammonium monophosphate and ammonium bisulphate with ammonium sulphate. The catalyst may be palladium, or possibly a noble metal on a carrier, e.g. alumina or activated carbon, and the nitrate concentration is in the molar range 1 to 5.
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公开(公告)号:DE2059581A1
公开(公告)日:1971-06-24
申请号:DE2059581
申请日:1970-12-03
Applicant: STAMICARBON
IPC: C07C251/46 , C01B21/14 , C07C67/00 , C07C239/00
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公开(公告)号:DE1567834A1
公开(公告)日:1970-08-20
申请号:DE1567834
申请日:1965-10-08
Applicant: STAMICARBON
IPC: C01B21/14
Abstract: An acid solution of hydroxylamine is prepared by adding a nitrite ester to an acid and reducing the ester with molecular H2 in the presence of a hydrogenation catalyst. The catalyst may contain a noble metal of Group VIII of the Periodic Table. The catalyst, e.g. Pt or Pd, may be supported on a carrier, e.g. C or Al2O3, and may be present as 100-3000 mg./l. of reactant liquor. Specified acids are H2SO4, H3PO4, NH4HSO4, and CH3COOH, and the temperature range may be 0-60 DEG C., maintained by a cooling jacket. The nitrite ester may be methyl, ethyl or butyl nitrite, which may be added at rate of 120-400 millimols/hr./l., with vigorous stirring. In the examples, the reaction mixture may also contain methyl, ethyl or butyl alcohols. The alcohol formed may be removed by distillation.
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