公开(公告)号：FR1434632A

公开(公告)日：1966-04-08

申请号：FR15881

申请日：1965-05-05

Applicant: BASF AG

Inventor： SUTER HUBERT ,  POEHLER GUENTER ,  MARTIN KARL ,  BRUNNMUELLER FRIEDRICH

IPC: C08F283/01 ,  C08G63/54

公开(公告)号：GB1007742A

公开(公告)日：1965-10-22

申请号：GB3107162

申请日：1962-08-14

Applicant: BASF AG

Inventor： SCHLIESSER WALTER ,  SUTER HUBERT

Abstract: Maleic anhydride is prepared by contacting maleic acid, or a mixture of maleic and phthalic acids, at a temperature of from 200 DEG to 450 DEG C., in a reaction zone, with moving particles of a dehydration catalyst of particle size of 0.05 to 0.5 mm., condensing from the gases leaving the reaction zone the anhydrides by cooling, and separating the maleic anhydride. The catalyst may be any solid dehydration catalyst for example, borates, phosphates, alumina, silica gel, titanium dioxide, zirconium dioxide, thorium oxide and mixtures thereof, which may be supported on a carrier which may be inert, e.g. pumice, aluminium silicate or silicon carbide, or may be active, e.g. silica gel. The catalyst is preferably used as a fluidized bed formed by a stream of inert gas or alternatively may be allowed to flow through the reaction chamber from top to bottom with continuous circulation without creating a fluidized bed. The reaction chamber may be heated by direct external heating or by using inert gases which have been preheated to, for example, 220-450 DEG C. The starting material, which may be pure or technical grade maleic acid or a mixture of maleic and phthalic acids obtained by, for example, oxidation of o-dialkyl benzenes, is fed to the reaction chamber in a molten or powdered state, preferably with the aid of a gas stream. When using a melt it is advantageous to atomize the liquid through a nozzle. A powder is preferably added at room temperature, or slightly above, e.g. 80-90 DEG C. The reaction is preferably carried out at 220-300 DEG C. at pressures of, for example, 200 mm. Hg to 5 atmospheres, preferably at ordinary pressure for a residence time of 0.5 to 20 secs. When the starting material consists essentially of maleic acid, for example 98% maleic acid, a residence time of 0.5 to 1 sec. may be used. With a large proportion of phthalic acid, residence times of up to 10 secs. may be required. All the reaction product may be condensed, but it is preferably to cool the products to 1 DEG to 5 DEG C. above the dew point of the water present to prevent the condensation of water. When a large amount of phthalic anhydride is present, e.g. above 90%, it is preferable to carry out a fractional condensation, initially at 130-135 DEG C. to give nearly pure phthalic anhydride followed by cooling to just above the dew point of water to give a mixture of maleic and phthalic anhydrides. The maleic anhydride, which is free of fumaric acid, may be purified by fractional distillation. The outgoing gases from the condensation may be washed with water to give a solution of maleic and phthalic acids which on removal of water may be recycled.

公开(公告)号：FR80631E

公开(公告)日：1963-05-24

申请号：FR878592

申请日：1961-11-10

Applicant: BASF AG

Inventor： SUTER HUBERT ,  POEHLER GUENTER

IPC: C07C51/265 ,  C07C51/573

公开(公告)号：GB897210A

公开(公告)日：1962-05-23

申请号：GB2793660

申请日：1960-08-12

Applicant: BASF AG

Inventor： SUTER HUBERT ,  POEHLER GUENTER

Abstract: Crude phthalic anhydride, containing at least 90% by weight of phthalic anhydride, obtained by the oxidation of naphthalene, is purified by distilling the crude material at a pressure of 20 to 200 mm. Hg and a still-temperature not exceeding 225 DEG C. until 5 to 25% of the material, including all the maleic acid or anhydride impurity, has distilled over; and then distilling the remaining material at such a pressure that the still-temperature does not exceed 200 DEG C. whereby pure phthalic anhydride is obtained as distillate, and a tarry residue containing naphthoquinone, sulphur-compounds and inorganic components remains in the still. In an example, the process is carried out in two distillation-columns, each packed with Raschig rings, the first column being operated at a pressure of 145 mm. Hg, and the second column at 85 mm. Hg.

公开(公告)号：CA609597A

公开(公告)日：1960-11-29

申请号：CA609597D

Applicant: BASF AG

Inventor： REICHENEDER FRANZ ,  SEEFELDER MATTHIAS ,  SUTER HUBERT ,  STOECKL ERICH ,  ORTH HELMUT

公开(公告)号：GB848395A

公开(公告)日：1960-09-14

申请号：GB1011059

申请日：1959-03-24

Applicant: BASF AG

Inventor： REICHENEDER FRANZ ,  SUTER HUBERT ,  DURY KARL ,  WILLERSINN CARL-HEINZ

IPC: B01J31/08 ,  B01J31/10 ,  C07C67/03

Abstract: Esters of propionylacrylic acid are prepared by reacting methylprotoanemonin with an alcohol at normal or elevated temperature under anhydrous conditions using an acid ion-exchanger as catalyst. The alcohol may be aliphatic, particularly C1-4 primary and secondary alcohols, cycloaliphatic or aromatic or may be a glycol monoether or a polyhydric alcohol such as a glycol. The ion-exchanger may contain carboxylic or sulphonic acid groups, specifically sulphurised polystyrene. The temperature is preferably about 10 DEG C. below the boiling point of the alcohol at the pressure used. Specified temperatures are 15 DEG -120 DEG C., preferably 50 DEG -90 DEG C. with pressures of 1 to 50 atmos. The mol ratio of methylprotoanemonin to alcohol may vary from 1 : 5 to about 1 : 50. The process may be operated batchwise or continuously.