Ashland Oil, Inc.

Ralph F Pascoe

Lee R Zehner

Richard V Norton

Dace Grote

John E Corn, Jr

Carlo Scaccia

A process for separation of methacrylic acid from methacrylic acid-isobutyric acid mixtures involving the selective crystallization and removal of the methacrylic acid from said mixtures is decribed.

Purification of methacrylic acid from an oxydehydrogenation by

A process for the improvement in the utilization of carbon monoxide and for the utilization of propylene having varying grades of purity in the carbonylation of propylene with carbon monoxide and hydrogen fluoride to form isobutyryl fluoride in a carbonylation reactor whereby the effluent from the reactor is (a) passed into a first phase separator where the effluent is separated into an overhead gaseous stream and a bottom liquid stream which contains unreacted carbon monoxide, (b) the bottom liquid stream from (a) is passed into a second reactor where it is contacted with a gaseous stream which contains propylene and allowing essentially all of the propylene to react, (c) the effluent from the second reactor is passed to a second phase separator where overhead gases are separated from liquid bottoms, (d) the liquid bottoms from the second phase separator are passed to a degassing pot where overhead gases are removed and the liquid bottoms stream which is essentially isobutyryl fluoride is taken to recovery, (e) the overhead gases from (d) are optionally mixed with inert gases and the stream is recycled to the hydrogen fluoride fed to the carbonylation reactor and/or recycled back to the gaseous stream in (b), (f) the gases from overhead stream in (a) are passed to a compressor and then to the recycle gaseous stream from (e), (g) the overhead gases from (e) are divided into a first portion which is sent to recycle as in (e) and a second portion which is sent to a refrigeration unit where said second portion into a bottom stream of less volatile materials and an overhead stream of volatile materials, a portion of the bottoms stream is added to the isobutyryl fluoride stream for recovery in (d), and the overhead, less volatile stream from (g) is sent to waste disposal is described.

Process for the carbonylation of propylene

A process for the esterification of an olefinically unsaturated carboxylic acid, such as methacrylic acid, with a lower alkanol, such as methanol, to form the corresponding ester over a solid cationic catalyst in which the carboxylic acid is used in excess of the alkanol on a molar basis, the improvement which comprises: (A) employing a hydraulically fluidized solid catalyst reactor for the continuous esterification reaction, (B) including in the esterification reaction a solvent which is a hydrocarbon having from 6 to 15 carbon atoms, (C) passing the effluent from the esterification reactor into a first distillation column in which the ester product and water by-product are taken overhead, (D) taking the unesterified carboxylic acid, solvent, and heavies from the bottom of the first distillation column, (E) separating the water from the ester in the overhead from (C) and recoverying the ester product, (F) separating heavies from the carboxylic acid-solvent from (D) in a second distillation column, (G) recycling the carboxylic acid-solvent from (F) back to the esterification reactor (A), and (H) disposing of the heavies from (F) is described.

Continuous esterification of methacrylic acid and product recovery

An exothermic reaction's heat of a low-temperature reaction is used for further processing of the product mixture, for example, to separate the product from the reaction mixture.

Process and apparatus for further processing of pressurized exothermic

A process for the production of isobutyric acid anhydride in which propylene is initially carbonylated in the presence of a substantial molar excess of liquid anhydrous hydrogen fluoride to provide a reaction mixture of isobutyroyl fluoride and unreacted hydrogen fluoride. Following distillation of the reaction mixture to recover a recycle stream of hydrogen fluoride, the isobutyroyl fluoride residue is partially hydrolyzed in the presence of a hydrogen fluoride acceptor resulting in a hydrolysis product consisting essentially of isobutyroyl fluoride, isobutyric acid anhydride and a hydrogen fluoride complex of said acceptor. Following removal of the solid complex, the hydrolysis product is fractionally distilled to yield an overhead fraction of isobutyroyl fluoride for reuse in the hydrolysis reaction.

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Marysville, OH, United States of America

Ralph F Pascoe