Abstract:
PRODUCTION OF ORTHOFORMIC ACID ALKYLESTERS BY REACTING HYDROCYANIC ACID WITH A MONOHYDRIC ALCOHOL AND HYDROGEN CHLORIDE AT LOW TEMPERATURES TO OBTAIN THE CORRESPONDING FORMIMIDOALKYLESTER (FORMIMINOALKYLETHER)-HYDROCHLORIDE IN A ANHYDROUS, INERT ORGANIC SOLVENT AND BY REACTING THE FORMIMIDOALKYLESTER-HYDROCHLORIDE WITH A FURTHER QUANTITY OF THE ALKYL ALCOHOL TO OBTAIN THE ORTHOFORMIC ACID ALKYLESTER. THE FORMATION OF THE FORMIMIDOALKYLESTER-HYDROCHLORIDE IS EFFECTED IN TWO STEPS. THE FIRST STEP COMPRISES CONVEYING A SUBSTANTIALLY EQUIMOLAR MIXTURE OF HYDROCYANIC ACID AND AN ALKYL ALCOHOL HAVING FROM 1 TO 4 CARBON ATOMS THROUGH A COOLER HAVING A LARGE INNER SURFACE AND A HIGH HEAT TRANSMISSION COEFFICIENT, AND INTRODUCING GASEOUS HYDROGEN CHLORIDE IN A MOLAR RATIO OF HC1:HCN BETWEEN 1:1 AND 1.1:1 INTO THE MIXTURE TRAVELLING THROUGH THE COOLER AND COOLED DOWN TO A TEMPERATURE BETWEEN -8* C. AND -18* C. THE SECOND STEP COMPRISES POURING THE MIXTURE COMING FROM THE COOLER INTO COOLED, ORGANIC SOLVENT, THE SOLVENT BEING USED AT A RATE OF BETWEEN ABOUT 1000 BIS 1500 CUBIC CENTIMETERS PER 1000 GRAMS OF THEORETICALLY EXPECTED FORMIMIDOALKYLESTER-HYDROCHLORIDE AND AT A TEMPERATURE OF BETWEEN -20* C. AND +8* C. FOLLOWING CRYSTALLIZATION OF THE FORMIMIDOALKYLESTER-HYDROCHLORIDE, FURTHE ALKYL ALCOHOL IS ADDED, WITHOUT NEUTRALIZATION OF HYDROGEN CHLORIDE IN EXCESS, TO THE SAID FORMIMIDOALKYLESTER-HYDROCHLORIDE IN A QUANTITY CORRESPONDING TO 80 TO 90% OF THE ALCOHOL QUANTITY THEORETICALLY NEEDED, THE MIXTURE IS MAINTAINED AT TEMPERATURES BETWEEN 3 AND 50* C., CRYSTALLIZED AMMONIUM CHLORIDE IS ISOLATED, AND THE ORTHOFORMIC ACID ALKYLESTER IS PURIFIED BY SUBJECTING IT TO DISTILLATIVE TREATMENT.
Abstract:
Production of unsaturated esters of carboxylic acids by reaction of an olefinic compound and an aliphatic or aromatic carboxylic acid, which each contain from two to 20 carbon atoms, with molecular oxygen or air, in the gas phase, at elevated temperature and in contact with a carrier catalyst, the reaction being carried out in contact with a carrier catalyst containing palladium acetate, alkali metal acetate and one or more uranium compounds as its active constituents.
Abstract:
PRODUCTION OF UNSATURATED PHOSPHONIC ACID DICHLORIDES FROM HALOGENO-ALKANE PHOSPHONIC ACID DICHLORIDES CONTAINING A HALOGENO-ALKANE RADICAL WITH 2 TO 8 CARBON ATOMS BY THERMAL DEHYDROHALOGENATION AND CONTINOUS DISTILLATIVE REMOVAL OF RESULTING UNSATURATED PHOSPHONIC ACID DICHLORIDE FROM REACTION MIXTURE, WHEREIN THE THERMAL DEHYDROHALOGENATION IS CARRIED OUT IN THE PRESENCE OF TRIPHENYL-PHOSPHINE AS THE CATALYST.
Abstract:
PROCESS FOR ISOLATING ACRYLIC ACID FROM HOT REACTION GASES OBTAINED BY OXIDATION OF PROPYLENE TO ACROLEIN COMPRISING THE STEPS OF COOLING THE REACTION GAS DOWN TO A TEMPERATURE BETWEEN ABOUT 90 AND 200*C., EXTRACTING THEREAFTER THE GAS IN COUNTER-CURRENT FASHION WITH AN ESTER OF AN ALIPHATIC OR AROMATIC MONOCARBOXYLIC OR DICARBOXYLIC ACID OR WITH TRIBUTYL OR TRICRESYL PHOSPHATE, SUBJECTING RESULTING EXTRACT TO DISTILLATION TO REMOVE ACRYLIC ACID IN THE FORM OF A CONCENTRATED AQUEOUS SOLUTION, AND USING REMAINING DISTILLATION RESIDUE FOR THE EXTRACTION OF FURTHER ACRYLIC ACID-CONTAINING REACTION GAS.
Abstract:
ISOLATION OF PURE ACRYLIC ACID FROM AQUEOUS CRUDE ACID CONTAINING ACRYLIC ACID AND IN ADDITION SMALL PROPORTIONS OF ACETIC ACID AND POSSIBLY FORMALDEHYDE, BY ETHYL ACETATE EXTRACTION COMBINED WITH A SIMULTANEOUS WATER-WASH OF THE RESULTING ORGANIC EXTRACT AND DISTILLATIVE SEPARATION OF THE WASHED EXTRACT INTO (A) PURE ACRYLIC ACID AND (B) A READILY BOILING ETHYL ACETATE/WATER-AZEOTROPE COMPRISING EXTRACTING THE AQUEOUS ACRYLIC ACID-CONTAINING CRUDE ACID BY MEANS OF ABOUT 10 TO 15 PARTS BY WEIGHT ETHYL ACETATE, PER PART BY WEIGHT ACRYLIC ACID, AND SIMULTANEOUSLY WASHING THE RESULTING ORGANIC EXTRACT BY MEANS OF ABOUT 15 TO 25 PARTS OF WEIGHT WATER, PER PART BY WEIGHT ACRYLIC ACID.
Abstract:
Preparation of a carrier-supported catalyst consisting of oxides of iron, bismuth, molybdenum and optionally silver and phosphorus in the atomic ratio of Ag0 1.5Fe0.1 12 Bi0.1 12P0 5Mo12O30 110, and of silicon carbide, aluminum oxide or silicon dioxide as the carrier. The catalyst is prepared in two steps. In the first step a porous carrier is impregnated at least once with an aqueous solution of a molybdenum compound and the water is evaporated; in the second step, the said carrier is impregnated at least once, at temperatures of between 20* and 100*C, with an aqueous nitric acid solution of iron, bismuth and optionally silver nitrates and optionally phosphoric acid; after the last impregnation, the carrier so treated is allowed to remain in contact with the said aqueous nitric acid solution for a period of between 5 and 24 hours, water and nitric acid are evaporated with continuous agitation of the carrier, and the carrier with the said salts adhered thereto is dried at temperatures of between 100* and 300*C, and annealed at temperatures of between 450* and 550*C.