摘要:
A process for purifying esters of tetrahydropyran-4-carboxylic acid of the formula I ##STR1## where R.sup.1 to R.sup.3 are each C.sub.1 -C.sub.4 -alkyl, and R.sup.2 and R.sup.3 are each additionally hydrogen, from mixtures produced in the reaction of butyrolactones of the formula II ##STR2## where R.sup.2 and R.sup.3 have the abovementioned meanings, and R.sup.4 is hydrogen, alkyl of 1-6 carbons or acyl of the formula --CO--R.sup.2, with alcohols of the formula R.sup.1 OH in the presence of oxide catalysts, by distillation, which entailsa) removing overhead, in a first column with 5-25 theoretical plates with a distillate pressure of 700-1100 mbar and a distillate temperature of 50.degree.-80.degree. C., an alcohol and up to 10% of the water,b) transferring the bottom product from the first column into a second column with 18-40 theoretical plates, into which a water entrainer is metered between plates 15 and 30, and is circulated, and which operates with a distillate pressure of 35-350 mbar and a distillate temperature of 18.degree.-70.degree. C., with the esters of tetrahydropyran-4-carboxylic acid being removed between plates 8 and 18 at 90.degree.-150.degree. C., and, where appropriate,c) feeding the bottom product from the second column into a third column with 5-25 theoretical plates, and returning the overhead products at a distillate pressure of 1-100 mbar and a distillate temperature of 90.degree.-140.degree. C. to the synthesis of the esters of tetrahydropyran-4-carboxylic acid.
摘要:
Catalysts or carriers which consist essentially of monoclinic zirconium dioxide are prepared by pecipitation of zirconium salts with ammonia, by adding a zirconyl nitrate or zirconyl chloride solution to an aqueous ammonia solution at a decreasing pH from 14 to 6 and drying, calcining and pelletizing the product.
摘要:
Catalysts or carriers which consist essentially of monoclinic zirconium dioxide are prepared by pecipitation of zirconium salts with ammonia, by adding a zirconyl nitrate or zirconyl chloride solution to an aqueous ammonia solution at a decreasing pH from 14 to 6 and drying, calcining and pelletizing the product.
摘要:
The invention concerns a process for the preparation of 6-aminocapronitrile or 6-aminocapronitrile-hexamethylene diamine mixtures by: a) reacting 5-formylvaleronitrile with ammonia and hydrogen in the presence of hydrogenation catalysts selected from the group consisting of metals or metal compounds rhenium, copper and elements of group VIII of the periodic table of elements, a hydrogenation discharge product being obtained; and b) extracting from the hydrogenation discharge product 6-aminocapronitrile and optionally hexamethylene diamine, provided that the hydrogenation catalyst does not contain copper, nickel or copper and nickel as it's only components.
摘要:
A process for the preparation of 1,2-butylene oxide by the catalytic hydrogenation of vinyl oxirane, in which use is made of a palladium catalyst on a support of barium sulfate, zirconium oxide or titanium dioxide or a rhenium-containing supported palladium catalyst.
摘要:
Crude capronitrile is purified by hydrogenation, subsequent treatment in an acidic medium and subsequent distillation in an alkaline medium, by a process in which(a) 6-aminocapronitrile is converted into crude caprolactam by reaction with water,(b) high boilers and low boilers are separated off from the crude caprolactam from step (a),(c) the crude caprolactam from step (b) is treated with hydrogen at from 50.degree. to 150.degree. C. and from 1.5 to 250 bar in the presence of a hydrogenation catalyst and, if desired, of a solvent to give a mixture A,(d1) mixture A in a solvent is passed, at from 30.degree. to 80.degree. C. and from 1 to 5 bar, over an ion exchanger containing terminal acid groups to give a mixture B1, or(d2) mixture A is distilled in the presence of sulfuric acid, any solvent present being removed before the addition of the sulfuric acid, to give a mixture B2, and(e) mixture B1 or mixture B2 is distilled in the presence of a base to give pure caprolactam.
摘要:
A process for preparing 4-hydroxymethyltetrahydropyran comprises reacting tetrahydrofurans of the general formula I ##STR1## where R.sup.1 is hydrogen, C.sub.1 - to C.sub.6 -alkyl or --CO--R.sup.2, andR.sup.2 is hydrogen or C.sub.1 - to C.sub.6 -alkyl,at from 0.degree. to 400.degree. C. and from 0.001 to 400 bar in the presence of acidic catalysts.
摘要:
Abstract of the Disclosure: Products of the reduction of 4-hydroxybutyric acid derivatives of the formula IIa ##STR1## where one of A and B is methylene and the other is cyclopropylidene, or of C.sub.1 --C.sub.4 --alkyl esters (IIb) or lactones (IIc) of these acids IIa, are prepared by hydrogenating the compounds IIa or IIb or IIc catalytically using hydrogen in the presence of a heterogeneous hydrogenation catalyst, giving novel compounds which can be used to prepare polymers.