Abstract: Concentrated acetic acid of 95 to 100 weight percent concentration containing both ionic and coordinate bromine can be successfully purified to a bromine content of less than 3 ppm by the sequential steps of catalytic hydrogenation, contacting the resulting acetic acid with alkali metal hydroxide, carbonate or bicarbonate, and then distilling acetic acid from the alkali metal.

Abstract: Acetic acid of 95 to 100 weight percent strength containing ionic and coordinate bromide impurities can be purified to a bromine content of less than 3 ppm by the sequence of steps comprising catalytic hydrogenating said acetic acid, treating the hydrogenated acetic acid with a solid absorbant and separating acetic acid therefrom.

Abstract: This invention relates to the removal of nickel, iron and copper co-dissolved with cobalt or manganese, or cobalt and manganese in water so that cobalt, manganese, or cobalt and manganese can be precipitated as carbonates and then converted to their acetates sufficiently low in nickel, iron and copper so that said acetates can be recycled to the liquid phase air oxidation of a di- or trimethyl benzene to its corresponding di- or tricarboxylic acid without material inhibition of such oxidation.

Abstract: Water is separated from a mixture of vapors containing 60 to 86 wt. % phthalic anhydride, 5 to 25 wt. % water, 0.8 to 10 wt. % benzoic acid, 0.1 to 4 wt. % o-toluic acid and up to 5 wt. % impurities boiling just above phthalic anhydride (PAN) by a fractionation zone whose reflux liquid is insert to PAN and the aromatic acids and immiscible with water but dissolves PAN at temperatures between its melting and freezing points and also dissolves benzoic acid and o-toluic acid at such temperatures. The reflux liquid or a component thereof when not a single compound leaves the top of the fractionation system as a vapor and does not leave the bottom thereof with PAN. Such water separation technique avoids having PAN vapors in a condenser whose cooled surfaces can and do become coated with solid PAN.

Abstract: This invention relates to the removal of substantially all of the disodium terephthalate (Na.sub.2 TA) dissolved in a dilute aqueous solution of sodium hydroxide. More particularly this invention pertains to the recovery for reuse of an aqueous solution containing 5 weight percent sodium hydroxide from an aqueous solution containing, on a weight basis, from 5 to 5.25 percent Na.sub.2 TA and 2.5 to 3.0 percent sodium hydroxide.

Abstract: Phthalic anhydride of commercially acceptable quality can be recovered from the neat catalytic oxidation of liquid o-xylene with air in the presence of the catalysis system provided by cobalt, manganese and bromine conducted in a single step and in the presence of a small amount of benzoic acid to make miscible liquid o-phthalic acid and liquid oxylene conducted in a single step to an 80 to 90 mole percent yield of o-phthalic acid provided the resulting liquid oxidation effluent is subjected to rapid dehydration of o-phthalic acid to its anhydride and rapid evaporation of the anhydride, water and compounds boiling between water and said anhydride which evaporation entrains phthalide in the vapor mixture followed by contact of the vapor mixture with Pd/C and introducing the vapor mixture into a fractionating system whose reflux liquid is inert, boils at a temperature below the boiling temperature of phthalic anhydride and is a solvent therefor at a temperature below the freezing temperature of said anhydride w

Abstract: Phthalic anhydride of commercially acceptable quality can be recovered from the neat oxidation of liquid o-xylene with air in the presence of the catalysis system provided by cobalt, manganese and bromine conducted in a single step and in the presence of a small amount of benzoic acid to make miscible liquid o-phthalic acid and liquid o-xylene conducted in a single step to an 85 to 90 mole percent yield of o-phthalic acid provided the resulting liquid oxidation effluent is subjected to rapid dehydration of o-phthalic acid to its anhydride and rapid evaporation of the anhydride, water and compounds boiling between water and said anhydride which evaporation entrains phthalide in the vapor mixture followed by contact of the vapor mixture in a fractionating system whose reflux liquid is inert, boils at a temperature below the boiling temperature of phthalic anhydride and is a solvent therefor at a temperature below the freezing temperature of said anhydride whereby impure liquid anhydride is withdrawn as a water

Abstract: Phthalic anhydride of commercially acceptable quality can be produced continuously in yields of from about 80 up to about 83 mole percent (% of theoretical) through a combination of steps starting with the neat oxidation of liquid o-xylene with air in the presence of catalysis provided by cobalt, manganese and bromine. Said oxidation is conducted in two steps wherein the first step is conducted under mild conditions and short residence time to provide a liquid effluent containing 8 to 40 weight percent o-phthalic acid and 6 to 30 weight percent o-xylene and the second step oxidizes such liquid effluent composition under more vigorous conditions including higher reaction temperature and longer residence time until substantially all the o-xylene and precursors of o-phthalic acid have been converted to o-phthalic acid.

Abstract: Phthalic anhydride of commercially acceptable quality is recovered in high (94-96%) yields from a mixture containing, on a weight basis, from 70 to 90% o-phthalic acid, 1.5 to 20% water, 0.3 up to 13% benzoic acid, 0.2 up to 2% o-toluic acid, 0.2 to 1% 2-carboxybenzaldehyde, 0.1 up to 2% phthalide and from 1.3 up to 10% higher boiling materials by rapid dehydration of o-phthalic acid to its anhydride and rapid evaporation thereof followed by contact of the resulting vapor mixture with an inert reflux liquid in a fractionation zone to remove water and to provide a partial purification of the anhydride, removal of phthalide therefrom by only heating said partially purified anhydride in the presence of a catalytic amount of an alkali metal hydroxide having a molecular weight of at least 56 followed by fractionation of the phthalide-free mixture.

Abstract: Phthalic anhydride of commercially acceptable quality can be produced continuously in yields of from about 80 up to about 83 mole percent (% of theoretical) through a combination of steps starting with the neat oxidation of liquid o-xylene with air in the presence of the catalysis provided by cobalt, manganese and bromine. Said oxidation is conducted in two steps wherein the first step is conducted under mild conditions and short residence time to provide a liquid effluent containing 8 to 40 weight percent o-phthalic acid and 6 to 30 weight percent o-xylene and the second step oxidizes such liquid effluent composition under more vigorous conditions including higher reaction temperature and longer residence time until substantially all of the o-xylene and precursors of o-phthalic acid have been converted to o-phthalic acid.

Abstract: Phthalic anhydride of commercially acceptable quality is recovered in high (94-96%) yields from a mixture containing on a weight basis from 70 to 90% o-phthalic acid, 1.5 to 21% water, 0.3 up to 13% benzoic acid, 0.2 up to 2% o-toluic acid, 0.2 to 1% 2-carboxybenzaldehyde, 0.1 up to 2% phthalide and from 1.3 up to 10% higher boiling materials by rapid dehydration of o-phthalic acid to its anhydride and rapid evaporation thereof followed by contact of the resulting vapor mixture with an inert reflux liquid in a fractionation zone to remove water and to provide a partial purification of the anhydride, removal of phthalide therefrom by only heating said partially purified anhydride in the presence of a catalytic amount of an alkali metal hydroxide having a molecular weight of at least 56 followed by fractionation of the phthalide-free mixture.

Abstract: This invention relates to the neat air oxidation of liquid o-xylene in a continuous manner in a single step to overcome the limited conversion of the process of British Patent Specification No. 856,245 or of the process of U.S. Pat. No. 3,920,735. More specifically this invention overcomes the limited conversion of o-xylene by its single step air oxidation in the presence of catalysis provided by ions of cobalt, manganese and bromine not only by maintaining the proper relationship of temperature, pressure and free water concentration in the reaction mixture to minimize the conversion of o-phthalic acid to its intramolecular anhydride but also by conducting the oxidation in the presence of small amounts of acetic or benzoic acid to make miscible the otherwise immiscible liquid phases of liquid o-xylene and liquid o-phthalic acid containing components of catalysis and free liquid water.

Abstract: Continuous production of iso- or terephthalic acid in a stirred reaction zone by catalytic air oxidation of m- or p-xylene in the presence of a benzoic acid-water liquid solvent system at constant gauge pressure within the range of 7 to 21 kg/cm.sup.2 wherein oxidation temperature within the range of 175.degree. to 235.degree. C. is maintained substantially constant by the novel control thereof by only varying the flow rate of water condensate reflux to the oxidation zone. The invention further pertains to novel means for achieving such temperature control.

Abstract: Phthalide, one intermediate in the oxidation of o-xylene to phthalic acid or its anhydride, is unique in that it is the only intermediate oxidation product which cannot be economically removed from said anhydride by fractional distillation or crystallization. According to the present invention, impure phthalic anhydride containing phthalide is heated to a temperature of at least 200.degree. C. in the presence of a catalytic amount of an alkali metal hydroxide having a molecular weight above 40. By such heat treatment of impure phthalic anhydride its phthalide content can be decreased to at least 0.1 weight percent and even to below the analytically detectable concentration of 0.001 weight percent (10 ppm by weight).

Abstract: Continuous oxidation of rubbery polymeric hyrocarbons by mixing an oxygen-containing gas and a hot solution of the polymer in an oleaginous solvent at the inlet to a spraying device and spraying the mixture into a hot chamber provides substantially instantaneous oxidation of the polymer and disengagement of gas and liquid and at least the same extent of oxidation as the time consuming oxidation accomplished by sparging such gas into a volume of stirred hot solution.

Abstract: This invention relates to the preparation of the subject aqueous solution from a non-bromine manganous salt. More specifically this invention pertains to a critical order of dissolving such salt and elemental bromine and to the use of an anti-oxidant for the manganous ion to prevent its conversion to hydrated manganous dioxide: MnO(OH).sub.2. According to "A Comprehensive Treatise On Inorganic And Theoretical Chemistry", J. W. Mellor, Vol. XII at pages 189 and 259 (published by Longmans, Green and Co., 1947) hydrated manganous dioxide results from the oxidation of a solution of manganous salt with chlorine, bromine, hypochlorous acid, hydrogen peroxide, etc. Such oxidation of a solution of manganous acetate was specifically mentioned. Such hydrated manganous dioxide is described as a white solid product which upon standing in contact with air becomes a dark brown to black product identified as MnO.sub.2.

Abstract: This invention relates to the continuous production of iso- or terephthalic acid in a stirred reaction zone by catalytic air oxidation of m- or p-xylene in the presence of a benzoic acid-water liquid solvent system at constant gauge pressure within the range of 7 to 21 kg/cm.sup.2 wherein oxidation temperature within the range of 175.degree. to 235.degree. C. is maintained substantially constant by the novel control thereof by only varying the flow rate of water condensate reflux to the oxidation zone. The invention further pertains to novel means for achieving such temperature control.

Abstract: Phenols alkylated with high molecular weight ethylene-propylene-diene terpolymers are obtained in essentially quantitative yields and with no measurable fragmentation of terpolymer by reacting terpolymer with a large excess of phenol, in the presence of BF.sub.3 as catalyst, at alkylation temperatures of about 170.degree.-300.degree. F. The preferred terpolymers consist essentially of about 35-45 mole percent propylene, 65-55 mole percent ethylene, and about 1.0-2.5 mole percent of a 5-alkenyl-2-norbornene such as 5-ethylidene-2-norbornene. The novel terpolymer alkylated phenol compositions are useful as intermediates for the preparation of multifunctional addition agents for lubricating oils, for example addition agents having combined dispersant-viscosity index improving properties.

Abstract: Terephthalic acid (TA) or isophthalic acid (IA) of fiber-grade quality is recovered under oxidation temperature and pressure conditions from fluid oxidation effluent from catalytic liquid phase oxidation of the respective xylene isomer in acetic acid with molecular oxygen by crystal size classification and acetic acid mother liquor displacement with hot, fresh acetic acid followed by quenching the new suspension of phthalic acid crystals in said hot solvent with colder fresh acetic acid solvent and separating the product crystals. Such technique eliminates the need for separately purifying crude TA or IA or converting TA or IA to the respective dimethyl ester and purifying the ester.

Abstract: This invention relates to a novel lubricant oil addition agent which is a phosphosulfurized C.sub.35 to C.sub.160 hydrocarbon modified N-(hydroxy and C.sub.50 - C.sub.160 alkyl-substituted benzyl) alkylene polyamine. Such novel addition agent imparts anti-oxidant and unexpected dispersancy functions to lubricant oils commonly used as crankcase lubricants for internal combustion engines. Such novel addition agent also imparts anti-oxidant and detergency functions to the less viscous oils used to lubricate automatic transmissions and at the same time prevent failure of the rubber seals used therein from deterioration (hardening) by oxidation and distortion softening by undue swelling. The present inventive addition agent unexpectedly provides both detergency and an anti-oxidant functions for lubricant oil which are superior to the related analog addition agent derived from the reaction of one molar proportion of a phosphosulfurized 500 to 2800 (Staudinger) molecular weight hydrocarbon with from 0.