Abstract:
An improved process of distilling a cyclohexanone-rich overhead stream in a first still from a feed mixture comprising cyclohexanone, phenol and cyclohexanol of the type wherein a cyclohexanone-rich stream is withdrawn as a part of an overheads condensate from the first still and a phenol-rich stream is withdrawn as a part of a reboiled bottom stream from the first still. The improvement includes withdrawing a side stream substantially free of phenol from above the point where the feed mixture is fed to the first column and separating the side stream in a second still into a second cyclohexanone-rich overhead stream and a bottom stream containing cyclohexanone and cyclohexanol. The second cyclohexanone-rich stream may be returned to the first still.
Abstract:
A process for the preparation of a-phenoxy-benzaldehyde which comprises contacting the 3-phenoxy-benzyl alcohol of the formula ##STR1## wherein R.sup.1 and R.sup.2 are identical or different and represent hydrogen or halogen with an aqueous solution of a dichromate in the presence of aqueous sulphuric acid at a temperature in the range of 50.degree. to 125.degree. C. The 3-phenoxy-benzaldehyde can be in a mixture of other organic compounds such as obtained by hydrolyzing a 3-phenoxy toluene chlorinated in the side chain at a temperature of 140.degree.-210.degree. C. under pressure.
Abstract:
Acetone produced as a by-product in the reaction of methyl acetate with carbon monoxide and hydrogen in the presence of a Group VIII noble metal catalyst and methyl iodide is recovered from the reaction mixture by supplying acetone to provide an acetone to methyl iodide molar ratio of at least 1:10 and distilling the mixture comprising methyl iodide, acetone and methyl acetate to separate substantially all of the methyl iodide and the supplied acetone and some of the methyl acetate from the remaining acetone and methyl acetate and thereafter separating the acetone from the methyl acetate.
Abstract:
Symmetrical 1,3-dichloroacetone is prepared by contacting chlorine with an aqueous mixture of acetone, monochloroacetone, or mixtures thereof and an iodine-containing promoter.
Abstract:
Process for the manufacture of acetaldehyde by reaction of ethylene and oxygen in the presence of an aqueous solution of palladium and copper chloride, in which continuously part of the latter solution is regenerated by heating it outside of the reactor. The gaseous mixture leaving the reactor is treated (a) by cooling with recycling of the condensate formed to the reactor and completion of the water portion that has not condensed during cooling, by the addition of water to the reactor, (b) by washing of the cooled gas mixture with water whereby an aqueous acetaldehyde solution is obtained, (c) by extractive distillation of this solution using water as extraction agent. Next, pure acetaldehyde is obtained as an overhead product in a further distillation step. The water demand of step (b) and optionally additionally of steps (a) and/or (c) is satisfied with the waste water obtained in the bottoms of the last distillation step and the residual waste water in each case is discharged.
Abstract:
Cyclohexylbenzene is separated from a cyclohexylbenzene-cyclohexanone-phenol admixture by liquid-liquid extraction with a non-polar solvent such as hexadecane and a polar solvent, such as sulfolane, diethylene glycol, or mixtures with water. Cyclohexylbenzene is separated from the non-polar phase by fractional distillation. Phenol and cyclohexanone are separated from the polar solvent by fractional distillation.
Abstract:
Novel substituted propargyl alcohols of the formula: ##STR1## novel allylic alcohols of the formula: ##STR2## and; .delta.,.epsilon.-unsaturated ketones of the formula: ##STR3## are provided. In the above formulas, R represents a group of the formula: ##STR4## wherein X.sub.1 and X.sub.2 are both hydrogen atoms or wherein one of X.sub.1 and X.sub.2 is a hydrogen atom, the other jointly with Z represents a bond; Z jointly with X.sub.1 or X.sub.2 represents a bond or separately represent a hydrogen atom, a hydroxyl group or a lower alkoxy group; R.sub.1 and R.sub.2 are the same or different and represents hydrogen atoms or lower alkyl groups; n is 1 or 2; and when n is 2, X.sub.1, X.sub.2, X, R.sub.1 and R.sub.2 may be the same or different. These novel compounds are easily produced and are useful as perfumes and as interrelated intermediates for the production of terpenoid compounds.
Abstract:
Crude benzaldehyde, and especially benzaldehyde prepared by the oxidation of toluene with a gas containing molecular oxygen, will contain certain impurities which will cause unwarranted discoloration and olfactory problems. These impurities can be effectively removed by treating the benzaldehyde with an oxidizing agent and then distillation.
Abstract:
Novel substituted propargyl alcohols of the formula: ##STR1## novel allylic alcohols of the formula: ##STR2## .delta.,.epsilon.-unsaturated ketones of the formula: ##STR3## are provided. In the above formulas, R represents a group of the formula: ##STR4## wherein X.sub.1 and X.sub.2 are both hydrogen atoms or wherein one of X.sub.1 and X.sub.2 is a hydrogen atom, the other jointly with Z represents a bond; Z jointly with X.sub.1 or X.sub.2 represents a bond or separately represent a hydrogen atom, a hydroxyl group or a lower alkoxy group; R.sub.1 and R.sub.2 are the same or different and represents hydrogen atoms or lower alkyl groups; n is 1 or 2; and when n is 2, X.sub.1, X.sub.2, X, R.sub.1 and R.sub.2 may be the same or different. These novel compounds are easily produced and are useful as perfumes and as interrelated intermediates for the production of terpenoid compounds.
Abstract:
Disclosed is a process for separating 11-cyanoundecanoic acid, cyclohexanone and .epsilon.-caprolactam from a pyrolysis product obtained by pyrolyzing 1,1'-peroxydicyclohexylamine in the presence of steam at a temperature of 300.degree. to 1,000.degree. C. The pyrolysis product is first contacted with a mixture comprised of aqueous ammonia and at least one organic solvent selected from benzene, toluene and xylene, and the so prepared liquid is separated into the oily layer and the aqueous layer. On one hand, the oily layer is distilled to separate cyclohexanone therefrom. On the other hand, the aqueous layer is acidified to a pH of below 4.0 by adding thereto a mineral acid and maintained at a temperature of 40.degree. to 100.degree. C. to separate crude 11-cyanoundecanoic acid in molten form from the aqueous layer, and then, the separated crude molten 11-cyanoundecanoic acid is washed with hot water to extract .epsilon.-caprolactam therefrom.