Process for the preparation of catalysts useful for the manufacture of maleic anhydride

Claim 2

A process for manufacture of a phosphorus-vanadium oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having from about 2 to about 10 carbon atoms, with a phosphoryl halide in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

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

A process for the manufacture of a phosphorus-vanadium oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having from about 2 to about 10 carbon atoms, with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, wherein the phosphorus-vanadium oxide catalyst is dissolved and the dissolved phosphorus-vanadium oxide catalyst is solidified by evaporation or distillation of the organic solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and a phosphorous compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 6

A process for the manufacture of a phosphorus-vanadium oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having from about 2 to about 10 carbon atoms, with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, wherein the phosphorus-vanadium oxide catalyst is dissolved and the dissolved phosphorus-vanadium oxide catalyst is solidified by evaporation or distillation of the organic solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and a phosphorous compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 7

The process for the manufacture of a phosphorus-vanadium oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having from about 2 to about 10 carbon atoms, with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and an alkyl ester of orthophosphoric acid at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 8

The process for the manufacture of a phosphorus-vanadium oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having from about 2 to about 10 carbon atoms, with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and an alkyl ester of orthophosphoric acid at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 9

The process of claim 5 wherein the ether is tetrahydrofuran.

Claim 10

The process of claim 5 wherein the alkyl ester 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 11

The process of claim 7 wherein the alkyl ester is triethylphosphate.

Claim 12

The process of claim 7 wherein the alkyl ester is trimethylphosphate.

Claim 13

The process for the manufacture of a phosphorus-vanadium oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in fan organic ether solvent having from about 2 to about 10 carbon atoms, with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane, or another C 4 hydrocarbon feedstock and water wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream and a phosphorus compound selected from the group consisting of: ##STR3## wherein R is a phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R.

Claim 14

The process for the manufacture of a phosphorus-vanadium oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in fan organic ether solvent having from about 2 to about 10 carbon atoms, with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane, or another C 4 hydrocarbon feedstock and water wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream and a phosphorus compound selected from the group consisting of: ##STR3## wherein R is a phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R.

Claim 15

A process for the manufacture of a phosphorus-vanadium cometal oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein a cometal is used as a promoter and wherein the total atomic ratio of the cometal to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl halide in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 16

A process for the manufacture of a phosphorus-vanadium cometal oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein a cometal is used as a promoter and wherein the total atomic ratio of the cometal to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl halide in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 17

The process of claim 11 wherein the vanadium compound is vanadium pentoxide.

Claim 18

The process for the manufacture of a phosphorus-vanadium cometal oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein a cometal is used as a promoter and wherein the total atomic ratio of the cometal to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, wherein the phosphorus-vanadium cometal oxide catalyst is dissolved and the dissolved phosphorus-vanadium cometal oxide catalyst is solidified by evaporation or distillation of the organic solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 19

The process for the manufacture of a phosphorus-vanadium cometal oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein a cometal is used as a promoter and wherein the total atomic ratio of the cometal to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, wherein the phosphorus-vanadium cometal oxide catalyst is dissolved and the dissolved phosphorus-vanadium cometal oxide catalyst is solidified by evaporation or distillation of the organic solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 20

The process for the manufacture of a phosphorus-vanadium cometal oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein a cometal is used as a promoter and wherein the total atomic ratio of the cometal to vanadium is in the range of about 0.001:1 to about 0.4:1 and wherein the cometal is selected from the group consisting of zinc, molybdenum, niobium, tungsten, uranium, cobalt and tin suitable for use in the manufacture of maleic anhydride from butane or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and an alkyl ester of orthophosphoric acid at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 21

The process for the manufacture of a phosphorus-vanadium cometal oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein a cometal is used as a promoter and wherein the total atomic ratio of the cometal to vanadium is in the range of about 0.001:1 to about 0.4:1 and wherein the cometal is selected from the group consisting of zinc, molybdenum, niobium, tungsten, uranium, cobalt and tin suitable for use in the manufacture of maleic anhydride from butane or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and an alkyl ester of orthophosphoric acid at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 22

The process of claim 14 wherein the vanadium compound is vanadium pentoxide.

Claim 23

The process of claim 15 wherein the ether is tetrahydrofuran.

Claim 24

The process of claim 14 wherein the alkyl ester 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 25

The process of claim 17 wherein the alkyl ester is triethylphosphate.

Claim 26

The process of claim 17 wherein the alkyl ester is trimethylphosphate.

Claim 27

A process for the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane or another C.sub.4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C.sub.4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 28

A process for the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane or another C.sub.4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C.sub.4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 29

A process for the manufacture of a phosphorus-vanadium-moylbdenum oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ and wherein the cometal is molybdenum and the total atomic ratio of molybdenum to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, 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, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 30

A process for the manufacture of a phosphorus-vanadium-moylbdenum oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ and wherein the cometal is molybdenum and the total atomic ratio of molybdenum to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, 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, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 31

A process for the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ suitable for use in the manufacture of maleic anhydride from butane or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with an alkyl ester of orthophosphoric acid in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and an alkyl ester of orthophosphoric acid at a temperature of about 300° C. to about 500° C.

Claim 32

A process for the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ suitable for use in the manufacture of maleic anhydride from butane or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with an alkyl ester of orthophosphoric acid in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and an alkyl ester of orthophosphoric acid at a temperature of about 300° C. to about 500° C.

Claim 33

The process of claim 22 wherein the alkyl ester 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 34

The process of claim 23 wherein the alkyl ester is triethylphosphate.

Claim 35

The process of claim 23 wherein the alkyl ester is trimethylphosphate.

Claim 36

A process for the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ and wherein the cometal is molybdenum and the total atomic ratio of molybdenum to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane, another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane, or another C 4 hydrocarbon feedstock and water wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream and a phosphorus compound selected from the group consisting of: ##STR4## wherein R is a phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R.

Claim 37

A process for the manufacture of a phosphorus-vanadium-molybdenum oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ and wherein the cometal is molybdenum and the total atomic ratio of molybdenum to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane, another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane, or another C 4 hydrocarbon feedstock and water wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream and a phosphorus compound selected from the group consisting of: ##STR4## wherein R is a phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R.

Claim 38

A process for the manufacture of a phosphorus-vanadium-zinc oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein the total atomic ratio of zinc to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane, or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor gas stream.

Claim 39

A process for the manufacture of a phosphorus-vanadium-zinc oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein the total atomic ratio of zinc to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane, or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor gas stream.

Claim 40

The process of claim 27 wherein the vanadium compound is vanadium pentoxide.

Claim 41

A process for the manufacture of a phosphorus-vanadium-zinc oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein the total atomic ratio of zinc to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, 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, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 42

A process for the manufacture of a phosphorus-vanadium-zinc oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein the total atomic ratio of zinc to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane or another C 4 hydrocarbon feedstock which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, 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, or another C 4 hydrocarbon feedstock and water, and a phosphorus compound at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 43

The process of claim 29 wherein the ether is tetrahydrofuran.

Claim 44

A process for the manufacture of a phosphorus-vanadium-zinc catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein the total atomic ratio of zinc to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock, and an alkyl ester of orthophosphoric acid at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 45

A process for the manufacture of a phosphorus-vanadium-zinc catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein the total atomic ratio of zinc to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst by the addition of butane, or another C 4 hydrocarbon feedstock, and an alkyl ester of orthophosphoric acid at a temperature of about 300° C. to about 500° C. wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream.

Claim 46

The process of claim 31 wherein the alkyl ester or 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 47

The process of claim 31 wherein the alkyl ester is triethylphosphate.

Claim 48

The process of claim 31 wherein the alkyl ester is trimethylphosphate.

Claim 49

A process for the manufacture of a phosphorus-vanadium-zinc oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein the total atomic ratio of zinc to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane or another hydrocarbon feedstock and water wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream and a phosphorus compound selected from the group consisting of: ##STR5## wherein R is a phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R.

Claim 50

A process for the manufacture of a phosphorus-vanadium-zinc oxide catalyst which comprises a phosphorus-vanadium mixed oxide, the atomic ratio of vanadium to phosphorus being in the range of 0.5:1 to 1.25:1 wherein the catalyst has a characteristic powder X-ray diffraction pattern using copper K alpha radiation, as follows, ______________________________________ Line Position Relative d, angstrom 2θ degrees Intensity ______________________________________ 5.71 15.52 37 4.80 18.46 8 4.52 19.64 24 3.67 24.21 18 3.29 27.06 25 3.11 28.67 12 2.94 30.41 100 2.79 32.00 12 2.65 33.81 7 2.61 34.28 7 2.40 37.39 12 ______________________________________ wherein the total atomic ratio of zinc to vanadium is in the range of about 0.001:1 to about 0.4:1 and is suitable for use in the manufacture of maleic anhydride from butane which process comprises reacting at a temperature of about 0° C. to about 200° C. a vanadium compound in an organic ether solvent having about 2 to about 10 carbon atoms with a phosphoryl chloride in the presence of water or an aliphatic alcohol having from about 1 to about 8 carbon atoms, eliminating the solvent, and activating the catalyst at a temperature of about 300° C. to about 500° C. by the addition of butane or another hydrocarbon feedstock and water wherein the amount of water added is about 1,000 parts per million to about 40,000 parts per million by weight of the reactor feed gas stream and a phosphorus compound selected from the group consisting of: ##STR5## wherein R is a phenyl or an alkyl radical of 1 to 6 carbon atoms and X is H or R.