摘要:
Process for separating water from a gas mixture, obtained in the manufacture of vinyl acetate by reacting ethylene with acetic acid and oxygen in contact with catalysts containing palladium or palladium compounds in the gaseous phase said gas mixture consisting essentially of acetic acid, vinyl acetate, water, carbon dioxide and ethylene, wherein(a) the gas mixture leaving the reaction zone is condensed to give a condensate containing the major portion of acetic acid, vinyl acetate and water and(b) an acetic acid solution containing the residual amount of vinyl acetate and water being prepared by absorption of the non-condensed gas in acetic acid, is characterized in that(c) the condensate obtained in step (a) and the solution obtained in step (b) are introduced separately from each other into the same distillation column, the feeding point of the condensate being above the feeding point of the solution, the water is distilled off at the head of said column as azeotrope together with the vinyl acetate and(d) the water phase is removed from the distillate separating into a water phase and a vinyl acetate phase.
摘要:
The invention relates to a process for the manufacture of unsaturated carboxylic acid esters by the reaction of olefins or cyclo-olefins with oxygen and carboxylic acids in the gaseous phase, in the presence of a catalyst which contains elements of the subsidiary group VIII of the periodic system and/or compounds thereof, and an alkali metal acetate, at temperatures of from 100.degree. to 250.degree. C. and pressures of from 0.5 to 21 bar absolute, wherein from 1 to 8000 parts per million (by weight), calculated on the carboxylic acid used, of organic chlorine compounds are added to the reaction mixture.
摘要:
The invention relates to a process for the isolation of vinyl acetate which involves not combining the bottom product of the recylced gas washings with the water-saturated vinyl acetate but rather introducing it to further multiple distillation columns from the gas mixture formed in the reaction of ethylene with acetic acid and oxygen over catalysts containing palladium or palladium compounds in the gas phase.
摘要:
The invention relates to a process for the isolation of vinyl acetate from a gas mixture containing vinyl acetate, ethyl acetate, water and carbon dioxide formed in the reaction of ethylene with acetic acid and oxygen in the gas phase over catalysts containing palladium or palladium compounds. The gas mixture leaving the reaction zone is passed into a distillation column and the gas mixture leaving the top thereof is cooled. The gas which is not condensed during the cooling is washed with acetic acid in a washing column, an acetic acid solution containing vinyl acetate being obtained. The bottom product from the distillation column is passed to a second distillation column and a side stream containing ethyl acetate is removed from an enrichment zone above the bottom thereof, all or some of the bottom product from the second distillation column, which product chiefly consists of acetic acid, being used for the wash in the washing column. The top vapor of the second distillation column is cooled. A portion of the organic phase of the condensate thereby formed is passed, together with the acetic acid solution obtained as the bottom product in the washing column, into a third distillation column, which may have an intermediate tray. The bottom product of the third distillation column is passed into a fourth distillation column. Pure vinyl acetate is removed at the top of the fourth distillation column.
摘要:
The invention relates to a process for the preparation of vinyl acetate in the gas phase from ethylene, acetic acid and oxygen or oxygen-containing gases on a catalyst which contains palladium and/or compounds thereof and if appropriate additionally gold and/or gold compounds and, as activators, alkali metal compounds and if appropriate additionally cadmium compounds, on a support. The support consists of cylindrical particles with curved front faces. The support material is aerogenic SiO.sub.2 or an aerogenic SiO.sub.2 -Al.sub.2 O.sub.3 mixture having a surface area of 50-250 m.sup.2 /g and a pore volume of 0.4-1.2 ml/g, which is formed to the extent of at least 50% by pores having a diameter of 50-200 .ANG..
摘要:
Method of separating vinylphosphonic acid from crude mixtures.The invention relates to a method for separating vinylphosphonic acid from crude mixtures, the separation being carried out by extraction with alcohols and/or ketones, which in each case comprise at least 5 carbon atoms.According to the invention, vinylphosphonic acid can be obtained in high purity and good yield from highly contaminated crude mixtures.
摘要:
Process for the preparation of pure propanephosphonic anhydride, which comprises distilling crude, impure propanephosphonic anhydride having an average degree of polymerization of 20 to 200 and containing less than 0.5% by weight of water by heating to 230 to 300.degree. C. under a pressure of 0.1 to 100 mbar, pure propanephosphonic anhydride having an average degree of polymerization of 20 to 60 being obtained.
摘要:
A process for the preparation of diesters of carboxymethylphosphonic acid of the formula: (RO).sub.2 P(O)CH.sub.2 CO.sub.2 H, in which R is a straight-chain or branched alkyl radical having 1 to 20 carbon atoms, a cycloaliphatic radical having 5 to 8 carbon atoms, a phenyl or naphthyl radical which can be substituted, an aralkyl radical having 7 to 10 carbon atoms, or in which the (RO).sub.2 P group forms a ring having 2 to 5 carbon atoms which can be substituted, characterized in that dialkyl ester of 2-hydroxyethylphosphonic acid of the formula (RO).sub.2 P(O)CH.sub.2 CH.sub.2 OH, in which R has the abovementioned meaning, is reacted with oxygen in the presence of water and a catalyst which contains at least one metal selected from the platinum metals group.
摘要:
N,N'-Diacetylethylene diamine (DAED) is produced by first adding the stoichiometric amount of acetic acid (2 mols per mol of ethylene diamine) at least partially in the form of aqueous acetic acid to ethylene diamine, distilling off in a second step the water contained in the reaction mixture, adding acetic acid in excess to the remaining product, distilling off the aqueous acetic acid formed and recycling it into the first process step. The DAED remains as sump product after distillation of the acetic acid.
摘要:
The present invention relates to a process for preparing vinylphosphonic acids of the formula ##STR1## in which m is an integer from 1 to 20 by heating 2-chloroethylphosphonic acids of the formula ##STR2## in which n is an integer equal to or smaller than m, if desired in the form of a solution, in the absence or presence of a catalyst to a temperature of 180 to 350.degree. C. and eliminating hydrogen chloride and, where appropriate, water under atmospheric pressure or reduced pressure and, if desired, hydrolysing the vinylphosphonic acids of the formula (I).