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    • 3. 发明专利
    • DE59607121D1
    • 2001-07-26
    • DE59607121
    • 1996-08-30
    • BASF AG
    • HERMELING DRHUGO RANDOLFSIEGEL DR
    • C07F9/02C07F9/53
    • A process for purifying tert. phosphine oxides of formula (R )(R )(R )P = O (I) in which R , R and R = 1-12 C alkyl, 5-8 FC cycloalkyl, aryl, 7-20 C aralkyl or 7-20 C alkylaryl, comprises reacting the (I) or a (I)-contg. mixt., opt. in an inert solvent, with an (in)organic acid at 0-150 degrees C and subsequently reacting the resulting salt with water or an (in)organic base. Pref. reaction with the acid is pref. carried out in an inert solvent such as aromatic hydrocarbons, aliphatic hydrocarbons, cycloaliphatic hydrocarbons or aromatic nitriles. Suitable acids are eg mineral acids such as HCl, HClO4, H2SO4 or H3PO4, Lewis acids such as BF3 or AlCl3, or organic acids such as acetic acid, formic acid or oxalic acid. The ratio acid to impure (I) is pref. 0.3 : 1 to 20 : 1, esp. 0.7 : 1 to 2 : 1. After crystallisation, the salt is recovered eg by filtration or centrifuging. The free (I) is liberated by treating the salt eg with an (in)organic base, esp. an aq. soln. of a base such as NaOH, KOH, Na2CO3, NH3, triethylamine, etc. The (I) is recovered e.g. by extraction with an inert solvent in the usual way.
    • 7. 发明专利
    • DE50000375D1
    • 2002-09-19
    • DE50000375
    • 2000-06-15
    • BASF AG
    • KRAMER DRMELDER DRRUETTER DRRIEWE GUENTERSIEGEL DRWEYER DR
    • C07D233/32C07D233/34C07D239/10
    • Formic acid-free N-alkyl-N'-methyl-alkylene ureas (I) are obtained from reaction mixtures obtained from the corresponding alkylene urea (II) and formaldehyde in presence of formic acid by supplying the mixture to the upper part of a distillation column, carrying out distillation under specific pressure and temperature conditions and recovering HCOOH-free (I) from the lower part of the column. Preparation of formic acid-free N-alkyl-N'-methyl-alkylene ureas of formula (I), by reacting the corresponding alkylene urea of formula (II) with monomeric or polymerized formaldehyde (HCHO) in presence of formic acid (HCOOH), involves supplying the reaction mixture containing (I) and HCOOH to the upper part of a distillation column, carrying out distillation without further additives and recovering HCOOH-free (I) from the lower part of the column. The pressure is in the upper part of the column is higher than that in the lower part by 10-100 (preferably 20-40) mbars and the temperature in the lower part of the column is higher than that in the upper part by 40-210 (preferably 80-150) degrees C. R1 = H or Me; R2 = H or 1-4C alkyl; x = 0 or 1.