Production of Maleic Anhydride and Maleic Acid.

    公开(公告)号:GB1154148A

    公开(公告)日:1969-06-04

    申请号:GB4487466

    申请日:1966-10-07

    Applicant: BASF AG

    Abstract: 1,154,148. Oxidation catalysts. BADISCHE ANILIN-& SODA-FABRIK A.G. 7 Oct., 1966 [9 Oct., 1965], No. 44874/66. Heading B1E. [Also in Division C2] A catalyst composition comprises 1-30% V 2 O 5 , 0-25% WO 3 , 5-70% P 2 O 5 , 4-90%. of a Cu, Ag, Cr, Mn, Fe, Co or Ni oxide and 0-90% of an inert carrier material, by weight. Preferably the ratio of P 2 O 5 to V 2 O 5 in the catalyst is more than 2:1 and the catalyst has an internal surface area of 1-100 sq. m/g. The catalysts may be prepared by conventional methods and may be used in the oxidation of olefinically unsaturated aliphatic hydrocarbons to anhydrides and acids.

    Production of catalysts or catalyst carriers in the form of hollow beads

    公开(公告)号:GB1069284A

    公开(公告)日:1967-05-17

    申请号:GB2380864

    申请日:1964-06-09

    Applicant: BASF AG

    Abstract: In Examples 5 and 8, nitrobenzene is hydrogenated to aniline in presence of hollow silica beads impregnated with copper, at temperatures of 280 DEG -290 DEG C.ALSO:Catalysts or catalyst carriers in the form of hollow beads are prepared by spraying a hydrogel containing at least 30% by weight of water and/or a suspension and/or a solution of metal compounds at a pressure of 10 to 100 atmospheres into a tower-shaped vessel, and cocurrently introducing a gas at 300 DEG to 700 DEG C. in amounts of 4 to 18 cubic meters per kgm. of initial material. Hydrogels of silicic acid, alumina, silicates and titania are mentioned, Al, Mg, Zr or Zn salts may be added in preparing a silicic acid hydrogel. The metal compounds may be compounds of Cu, Ag, Zn, Mg, Al, Sn, Pb, V, Cr, Mo, W, Mn, Fe, Ni, Co, Pt or Pd. The hollow beads may be treated with halogen or a phosphoric acid. Examples relate to (1), (5) silica gel; (2), (3) alumina gel; (4) aluminium phosphate; (6) alumina + Co + Mo; (7) Mo + P + V; (8) silica gel + Cu.ALSO:Catalysts or catalyst carriers in the form of hollow beads are prepared by spraying a hydrogel containing at least 30% by weight of water and/or a suspension and/or a solution of metal compounds at a pressure of 10 to 100 atmospheres into a tower-shaped vessel, and cocurrently introducing a gas at 300 DEG to 700 DEG C. in amounts of 4 to 18 cubic meters per kgm of initial material. Hydrogels of silicic acid, alumina, silicates and titania are mentioned. Al, Mg, Zr or Zn salts may be added in preparing a silicic acid hydrogel. The metal compounds may be compounds of Cu, Ag, Zn, Mg, Al, Sn, Pb, V, Cr, Mo, W, Mn, Fe, Ni, Co, Pt or Pd. The hollow beads may be treated with halogen or a phosphoric acid. Examples relate to (1), (5) silica gel (2), (3) alumina gel; (4) aluminium phosphate; (6) alumina +Co+Mo; (7) Mo+P+V; (8) silica gel +Cu. A reactor for hydrogenation of nitrobenzene has diameter to height ratio 1:4 and has twenty two-component nozzles arranged at three levels above the grate at the bottom of the reactor. The upper portion of the vessel is widened to 1 1/2 times and includes a cyclone; reaction gases leaving by the cyclone are recycled via a heat exchanger, condenser, gas-liquid separator, preheater and pump. Cooling tubes are arranged in the catalyst layer at a distance from the wall of the reactor.

    Improvements in the separation of liquid mixtures into their components

    公开(公告)号:GB900457A

    公开(公告)日:1962-07-04

    申请号:GB4199358

    申请日:1958-12-30

    Applicant: BASF AG

    Abstract: A liquid mixture, which contains material of low volatility, is separated into fractions by introducing it through pipe 1 into distillation column 3 the base of which is connected, by pipes 7 and 9, to a tubular evaporator 8; the base of the column and/or the tubular evaporator being also connected to a film-evaporator 12. Non-volatile material is withdrawn from the film-evaporator via pipe 13; and the volatile fraction is removed from the head of the column via dephlegmator 6 and pipe 10. In the embodiment shown, the vapour withdrawn from the film-evaporator via pipe 14 is condensed; and the condensate is introduced via pipe 22 into the column with fresh feed. The film-evaporator may be maintained at low pressure by a vacuum pump connected to pipe 19. The level of the liquid in the base of the column is maintained constant by valve 15. The operation is preferably conducted so that the bottoms product contains 40 to 60% of the low-volatile material. The process is suitable for fractionating the crude products of organic syntheses; and the heat of reaction may be used to preheat in heat-exchanger 2 the feed to the column. There are five examples, which relate to the production of cyclohexanol, dicyclohexylamine, dichlorbutane, adiponitrile, and beta-naphthol.

    Improvements in the production of cycloaliphatic alcohols and ketones by oxidation of cyclo-aliphatic hydrocarbons

    公开(公告)号:GB849134A

    公开(公告)日:1960-09-21

    申请号:GB2599858

    申请日:1958-08-13

    Applicant: BASF AG

    Abstract: In a process for the production of cycloaliphatic alcohols and ketones, by the oxidation of cycloaliphatic hydrocarbons in the liquid phase with oxygen or oxygen-containing gases in a plurality of successive oxidation-vessels, the oxidation-mixture from the last vessel is washed with fresh water to remove monobasic acids formed during the oxidation, the washing-water is separated from the oxidation-mixture, the washing-water is then used, wholly or partly, for washing the intermediate oxidation-mixture from each of the preceding oxidation-stages, and the final oxidation-mixture is submitted to distillation, for the separation of the unreacted cycloaliphatic hydro-carbon and the individual oxidation products. The oxidation-mixture is preferably washed with aqueous alkali hydroxide or carbonate solution before the distillation. Organic acids can be recovered from the washing-water and from the aqueous alkaline solution. The process may be used for the oxidation of cyclohexane in order to produce cyclohexanone and cyclohexanol; it may also be used for the oxidation of methyl-cyclohexane and cyclooctane. The oxidation is advantageously carried out at a temperature of 130 DEG -150 DEG C., a pressure of 3 to 30 atm., and in the presence of an oxidation-catalyst, such as cobalt naphthenate. The gaseous and vaporous constituents of the intermediate oxidation-mixtures are preferably subjected to water-washing together with the liquid constituents; the gaseous streams are then combined and cooled to recover unreacted cycloaliphatic hydrocarbon. The gaseous stream is finally washed with the liquid oxidationproduct, i.e., the final oxidation-mixture from which the unchanged hydrocarbon has been removed by distillation. Specification 776,803 is referred to.

    Dehydrogenation of cycloalkanols
    30.
    发明专利

    公开(公告)号:GB1061447A

    公开(公告)日:1967-03-15

    申请号:GB4969663

    申请日:1963-12-17

    Applicant: BASF AG

    Abstract: The gas phase dehydrogenation of cycloalkanols to cycloalkanones is conducted at elevated temperature in presence of a catalyst consisting of at least 80% of ZnO which has been obtained by precipitation from a Zn salt with a basic precipitant, and drying and annealing the ZnO, which has a surface of 5-20 m.2/g. The production of cyclohexanone from cyclohexanol is exemplified; other specified starting materials are 4-methylcyclohexanol, cyclooctanol and cyclododecanol.ALSO:ZnO, intended for use as a dehydrogenation catalyst, is prepared by precipitation from a Zn salt with a basic precipitant, dried and annealed to obtain a surface of 5-20 m2/g. The precipitate may be slowly heated to 400 DEG C. and annealed at between 400 DEG and 600 DEG C. until the desired surface is obtained. An after-treatment with H2 at 300-500 DEG is optional.ALSO:A dehydrogenation catalyst comprises ZnO which has been prepared by precipitation from a Zn salt with a basic precipitant, dried and annealed to obtain a surface of 5-20 m2/g. Ingredients which may be present in an amount of up to 20% are: pumice or other silicates, Cu compounds, alkali or alkaline earth metal salts of mineral acids and rare earth compounds; the Cu compounds may be e.g. oxide, hydroxide, carbonate or nitrate. The ZnO is preferably annealed at 400-600 DEG C. and may be treated with H2 at 300-500 DEG before use. A binding agent such as starch, graphite or stearic acid may be used in making the catalyst.

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