Process for the manufacture of orthoformic acid alkylesters
    21.
    发明授权
    Process for the manufacture of orthoformic acid alkylesters 失效
    制备酸性酸酐的方法

    公开(公告)号:US3641164A

    公开(公告)日:1972-02-08

    申请号:US3641164D

    申请日:1969-12-02

    Applicant: KNAPSACK AG

    CPC classification number: C07C43/32 C07C69/06

    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.

    Preparation of a carrier-supported catalyst
    30.
    发明授权
    Preparation of a carrier-supported catalyst 失效
    载体负载催化剂的制备

    公开(公告)号:US3691096A

    公开(公告)日:1972-09-12

    申请号:US3691096D

    申请日:1970-08-21

    Applicant: KNAPSACK AG

    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.

    Abstract translation: 由AgO-1.5Fe0.1-12 Bi0.1-12P0-5Mo12O30-110的原子比由铁,铋,钼和任选的银和磷的氧化物组成的载体负载催化剂的制备和碳化硅,铝 氧化物或二氧化硅作为载体。 催化剂分两步制备。 在第一步中,多孔载体用钼化合物的水溶液浸渍至少一次,蒸发水; 在第二步中,所述载体在20-100℃的温度下,用铁,铋和任选的硝酸银和任选的磷酸的硝酸水溶液浸渍至少一次; 在最后浸渍之后,将如此处理的载体与硝酸水溶液保持接触5至24小时之间,继续搅拌载体,蒸发水和硝酸,并将载体与 所述盐附着在100℃至300℃的温度下干燥,并在450-550℃的温度下进行退火。

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