Process for manufacture of maleic anhydride catalysts

Claim 2

A process for the manufacture of a phosphorus-vanadium oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent, with a phosphoryl halide in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl halide is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 3

The process of claim 1 wherein the vanadium compound is vanadium pentoxide.

Claim 4

The process of claim 1 wherein the ether is tetrahydrofuran.

Claim 5

The process of claim 1 wherein the phosphoryl halide is phosphoryl chloride.

Claim 6

A process for the manufacture of a phosphorus-vanadium oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent, with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and an alkylester of orthophosphoric acid at a temperature of about 300° C. to about 500° C. and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 7

A process for the manufacture of a phosphorus-vanadium oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent, with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and an alkylester of orthophosphoric acid at a temperature of about 300° C. to about 500° C. and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 8

The process of claim 5 wherein the alkylester of orthophosphoric acid has the following structure: (RO).sub.3 P═O wherein R is hydrogen or a C 1 to C 4 alkyl, at least one R being a C 1 to C 4 alkyl.

Claim 9

The process of claim 6 wherein the alkylester is triethylphosphate.

Claim 10

The process of claim 6 wherein the alkylester is trimethylphosphate.

Claim 11

A process for the manufacture of a phosphorus-vanadium-co-metal oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with a phosphoryl halide in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl halide is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and a phosphorus compound at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 12

A process for the manufacture of a phosphorus-vanadium-co-metal oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with a phosphoryl halide in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl halide is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and a phosphorus compound at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 13

The process of claim 9 wherein the vanadium compound is vanadium pentoxide.

Claim 14

The process of claim 9 wherein the ether is tetrahydrofuran.

Claim 15

The process of claim 9 wherein the phosphoryl halide is phosphoryl chloride.

Claim 16

The process of claim 9 wherein the phosphorus compound is an alkyl ester of orthophosphoric acid.

Claim 17

The process of claim 13 wherein the alkylester of orthophosphoric acid has the following structure: (RO).sub.3 P═O wherein R is hydrogen or a C 1 or C 4 alkyl, at least one R being a C 1 to C 4 alkyl.

Claim 18

The process of claim 14 wherein the alkylester is triethylphosphate.

Claim 19

The process of claim 14 wherein the alkylester is trimethylphosphate.

Claim 20

A process for the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with a phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and a phosphorus compound at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 21

A process for the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with a phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and a phosphorus compound at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 22

The process of claim 17 wherein the vanadium compound is vanadium pentoxide.

Claim 23

The process of claim 17 wherein the ether is tetrahydrofuran.

Claim 24

A process for the manufacture of a phosphorus-vanadium-zinc catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and an alkylester of orthophosphoric acid at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 25

A process for the manufacture of a phosphorus-vanadium-zinc catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and an alkylester of orthophosphoric acid at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 26

The process of claim 20 wherein the alkylester of orthophosphoric acid has the following structure: (RO).sub.3 P═O where R is hydrogen or a C 1 to C 4 alkyl, at least one R being a C 1 to C 4 alkyl.

Claim 27

The process of claim 20 wherein the alkylester is triethylphosphate.

Claim 28

The process of claim 20 wherein the alkylester is trimethylphosphate.

Claim 29

A process for the manufacture of a phosphorus-vanadium oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane, benzene, butene or butadiene and a phosphorus compound selected from the group consisting of: ##STR3## wherein R is phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 30

A process for the manufacture of a phosphorus-vanadium oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane, benzene, butene or butadiene and a phosphorus compound selected from the group consisting of: ##STR3## wherein R is phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 31

A process for the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, wherein the phosphorus-vanadium-molybdenum oxide catalyst is dissolved and the dissolved phosphorus-vanadium-molybdenum oxide catalyst is solidified by evaporation or distillation of the organic solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and a phosphorus compound at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas comprising at least about 0.1 wt. % oxygen is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 32

A process for the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, wherein the phosphorus-vanadium-molybdenum oxide catalyst is dissolved and the dissolved phosphorus-vanadium-molybdenum oxide catalyst is solidified by evaporation or distillation of the organic solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and a phosphorus compound at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas comprising at least about 0.1 wt. % oxygen is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 33

A process of the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane, benzene, butene or butadiene and a phosphorus compound selected from the group consisting of: ##STR4## wherein R is phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 34

A process of the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane, benzene, butene or butadiene and a phosphorus compound selected from the group consisting of: ##STR4## wherein R is phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 35

A process for the manufacture of a phosphorus-vanadium-zinc oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, wherein the phosphorus-vanadium-zinc oxide catalyst is dissolved and the dissolved phosphorus-vanadium-zinc oxide catalyst is solidified by evaporation or distillation of the organic solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and a phosphorus compound at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 36

A process for the manufacture of a phosphorus-vanadium-zinc oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, wherein the phosphorus-vanadium-zinc oxide catalyst is dissolved and the dissolved phosphorus-vanadium-zinc oxide catalyst is solidified by evaporation or distillation of the organic solvent and activating the catalyst by the addition of butane, benzene, butene or butadiene and a phosphorus compound at a temperature of about 300° C. to about 500° C., and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 37

A process for the manufacture of a phosphorus-vanadium-zinc oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane, benzene, butene or butadiene and a phosphorus compound selected from the group consisting of: ##STR5## wherein R is phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.

Claim 38

A process for the manufacture of a phosphorus-vanadium-zinc oxide catalyst suitable for use in the manufacture of maleic anhydride from butane, benzene, butene or butadiene which process comprises reacting in a reaction mixture at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent with phosphoryl chloride in the presence of water wherein the molar ratio of water to phosphorus from the phosphoryl chloride is in the range of about 2.25:1 to about 3.75:1, eliminating the solvent and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane, benzene, butene or butadiene and a phosphorus compound selected from the group consisting of: ##STR5## wherein R is phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R and wherein an oxygen containing gas is introduced into said reaction mixture at a rate sufficient to provide an atmosphere comprising at least about 0.1 wt. % oxygen during said reacting.