US3915892A — Vanadium-phosphorus mixed oxide oxidation catalys…

Claim 1

Independent Claim 7 words

INTRODUCING SAID OXIDE INTO A TREATING ZONE,

Claim 2

Dependent Claim 7 words

INTRODUCING SAID OXIDE INTO A TREATING ZONE,

Claim 3

Independent Claim 56 words

THE METHOD FOR THE PREPARATION OF AN IMPROVED OXIDATION CATALYST FROM A PARTICLATE COMPLEX MIXED OXIDE DIHYDRATE OF VANADIUM AND PENTAVALENT PHOSPHORUS, SAID OXIDE HAVING A PHOSPHORUS TO VANADIUM ATOMIC RATIO IN THE RAGE FROM ABOUT 1-2 TO 1, AND SAID VANADIUM HAVING AN AVERAGE VALENCE IN THE RANGE FROM ABOUT 3.9 TO 4,5 WHICH COMPRISES,

Claim 4

Independent Claim 56 words

THE METHOD FOR THE PREPARATION OF AN IMPROVED OXIDATION CATALYST FROM A PARTICLATE COMPLEX MIXED OXIDE DIHYDRATE OF VANADIUM AND PENTAVALENT PHOSPHORUS, SAID OXIDE HAVING A PHOSPHORUS TO VANADIUM ATOMIC RATIO IN THE RAGE FROM ABOUT 1-2 TO 1, AND SAID VANADIUM HAVING AN AVERAGE VALENCE IN THE RANGE FROM ABOUT 3.9 TO 4,5 WHICH COMPRISES,

Claim 5

Dependent Claim 42 words

MAINTAINING SAID OXIDE AND ZONE AT A TEMPERATURE IN THE DIHYDRATE-MONOHYDRATE TRANSITION TEMPERATURE RANGE OF THE OXIDE OF ABOUT 370* TO 394*C FOR A PERIOD SUFFICIENT FOR THE LIBERATION OF ABOUT ONE MOL OF WATER OF HYDRATION PER MOL OF THE OXIDE,

Claim 6

Dependent Claim 42 words

MAINTAINING SAID OXIDE AND ZONE AT A TEMPERATURE IN THE DIHYDRATE-MONOHYDRATE TRANSITION TEMPERATURE RANGE OF THE OXIDE OF ABOUT 370* TO 394*C FOR A PERIOD SUFFICIENT FOR THE LIBERATION OF ABOUT ONE MOL OF WATER OF HYDRATION PER MOL OF THE OXIDE,

Claim 7

Dependent Claim 33 words

passing a molecular oxygen-containing gas over or through said oxide during said first treatment, said gas being selected from the group consisting of air and molecular oxygen in admixture with an inert gas;

Claim 8

Dependent Claim 33 words

passing a molecular oxygen-containing gas over or through said oxide during said first treatment, said gas being selected from the group consisting of air and molecular oxygen in admixture with an inert gas;

Claim 9

Dependent Claim 27 words

The method as in claim 1 wherein the removal of said water balance is carried out by maintaining said temperature in the monohydrate-anhydrous oxide transition temperature range.

Claim 10

Dependent Claim 42 words

maintaining said oxide and zone at a temperature in the dihydrate-monohydrate transition temperature range of the oxide of about 370* to 394*C for a period sufficient for the liberation of about one mol of water of hydration per mol of the oxide;

Claim 11

Dependent Claim 42 words

maintaining said oxide and zone at a temperature in the dihydrate-monohydrate transition temperature range of the oxide of about 370* to 394*C for a period sufficient for the liberation of about one mol of water of hydration per mol of the oxide;

Claim 12

Dependent Claim 33 words

passing a molecular oxygen-containing gas over or through said oxide during said first treatment, said gas being selected from the group consisting of air and molecular oxygen in admixture with an inert gas;

Claim 13

Dependent Claim 33 words

passing a molecular oxygen-containing gas over or through said oxide during said first treatment, said gas being selected from the group consisting of air and molecular oxygen in admixture with an inert gas;

Claim 14

Dependent Claim 46 words

raising the temperature of the oxide resulting from the first treatment to a temperature in the range from about 395*C. to 425*C. and maintaining said temperature in the second treatment for a period sufficient for an additional weight loss of about 5 percent by said oxide;

Claim 15

Dependent Claim 46 words

raising the temperature of the oxide resulting from the first treatment to a temperature in the range from about 395*C. to 425*C. and maintaining said temperature in the second treatment for a period sufficient for an additional weight loss of about 5 percent by said oxide;

Claim 16

Dependent Claim 46 words

raising the temperature of the oxide resulting from the first treatment to a temperature in the range from about 395*C. to 425*C. and maintaining said temperature in the second treatment for a period sufficient for an additional weight loss of about 5 percent by said oxide;

Claim 17

Dependent Claim 46 words

raising the temperature of the oxide resulting from the first treatment to a temperature in the range from about 395*C. to 425*C. and maintaining said temperature in the second treatment for a period sufficient for an additional weight loss of about 5 percent by said oxide;

Claim 18

Dependent Claim 102 words

MAINTAINING THE AVERAGE VALENCE OF THE VANADIUM IN THE VANADIUM COMPONENT OF SAID OXIDE IN THE RANGE FROM ABOUT 4.1-4.5 AND WITHDRAWING SAID LIBERATED WATER FROM SAID ZONE DURING LIBERATION BY PASSING A CARRIER GAS THROUGH SAID ZONE, SAID CARRIER GAS BEING SELECTED FROM THE GROUP CONSISTING OF AIR, OXYGEN, AN INLET GAS CONTAINING OXYGEN AND OF SAID OXYGEN-CONTAINING GASES PLUS A HYDROCARBON COMPONENT, SAID GASES CONTANING SUFFICIENT OF MOLECULAR OXYGEN OR OF MOLECULAR OXYGEN AND HYDROCARBON TO PROVIDE AN EFFLUENT STREAM CONTAINING AT LEAST ABOUT ONE VOLUME PERCENT OF OXYGEN OR OF ONE VOLUME PERCENT EACH OF OXYGEN AND HYDROCARBON, AND

Claim 19

Dependent Claim 102 words

MAINTAINING THE AVERAGE VALENCE OF THE VANADIUM IN THE VANADIUM COMPONENT OF SAID OXIDE IN THE RANGE FROM ABOUT 4.1-4.5 AND WITHDRAWING SAID LIBERATED WATER FROM SAID ZONE DURING LIBERATION BY PASSING A CARRIER GAS THROUGH SAID ZONE, SAID CARRIER GAS BEING SELECTED FROM THE GROUP CONSISTING OF AIR, OXYGEN, AN INLET GAS CONTAINING OXYGEN AND OF SAID OXYGEN-CONTAINING GASES PLUS A HYDROCARBON COMPONENT, SAID GASES CONTANING SUFFICIENT OF MOLECULAR OXYGEN OR OF MOLECULAR OXYGEN AND HYDROCARBON TO PROVIDE AN EFFLUENT STREAM CONTAINING AT LEAST ABOUT ONE VOLUME PERCENT OF OXYGEN OR OF ONE VOLUME PERCENT EACH OF OXYGEN AND HYDROCARBON, AND

Claim 20

Dependent Claim 103 words

maintaining the average valence of the vanadium in the vanadium component of said oxide in the range from about 4.1-4.5 and withdrawing said liberated water from said zone during said liberation by passing a carrier gas through said zone, said carrier gas being selected from the group consisting of air, oxygen, an inert gas containing oxygen, and of said oxygen-containing gases plus a hydrocarbon component, said gases containing sufficient of molecular oxygen or of molecular oxygen and hydrocarbon to provide an effluent stream containing at least about one volume percent of oxygen or of one volume percent each of oxygen and hydrocarbon; and

Claim 21

Dependent Claim 103 words

maintaining the average valence of the vanadium in the vanadium component of said oxide in the range from about 4.1-4.5 and withdrawing said liberated water from said zone during said liberation by passing a carrier gas through said zone, said carrier gas being selected from the group consisting of air, oxygen, an inert gas containing oxygen, and of said oxygen-containing gases plus a hydrocarbon component, said gases containing sufficient of molecular oxygen or of molecular oxygen and hydrocarbon to provide an effluent stream containing at least about one volume percent of oxygen or of one volume percent each of oxygen and hydrocarbon; and

Claim 22

Dependent Claim 35 words

The method as in claim 2 wherein said resulting anhydrous oxide is maintained at a temperature in the bulk phase crystal transition range for a period in the range from about 4 to 26 hours.

Claim 23

Dependent Claim 17 words

The method as in claim 2 wherein said transition temperature range is from about 395*C. to 425*C.

Claim 24

Dependent Claim 39 words

raising the temperature of the oxide resulting from the second treatment to a temperature in the range from about 450*C. to 500*C. and maintaining said temperature for a period in the range from about 4 to 26 hours; and

Claim 25

Dependent Claim 39 words

raising the temperature of the oxide resulting from the second treatment to a temperature in the range from about 450*C. to 500*C. and maintaining said temperature for a period in the range from about 4 to 26 hours; and

Claim 26

Dependent Claim 42 words

removing the balance of the water of hydration from the resulting monohydrate by maintaining said zone and resulting monohydrate at a temperature in the range from about 395*C. to 600*C. and by passing a carrier gas through said zone as in (3).

Claim 27

Dependent Claim 42 words

removing the balance of the water of hydration from the resulting monohydrate by maintaining said zone and resulting monohydrate at a temperature in the range from about 395*C. to 600*C. and by passing a carrier gas through said zone as in (3).

Claim 28

Dependent Claim 39 words

raising the temperature of the oxide resulting from the second treatment to a temperature in the range from about 450*C. to 500*C. and maintaining said temperature fOr a period in the range from about 4 to 26 hours; and

Claim 29

Dependent Claim 39 words

raising the temperature of the oxide resulting from the second treatment to a temperature in the range from about 450*C. to 500*C. and maintaining said temperature fOr a period in the range from about 4 to 26 hours; and

Claim 30

Dependent Claim 42 words

REMOVING THE BALANCE OF THE WATER OF HYDRATION FROM THE RESULTING MONOHYDRATE BY MAINTAINING SAID ZONE AND RESULTING MONOHYDRATE AT A TEMPERATURE IN THE RANGE FROM ABOUT 395*C, TO 600*C, AND BY PASSING A CARRIER GAS THROUGH SAID ZONE AS IN (3),

Claim 31

Dependent Claim 42 words

REMOVING THE BALANCE OF THE WATER OF HYDRATION FROM THE RESULTING MONOHYDRATE BY MAINTAINING SAID ZONE AND RESULTING MONOHYDRATE AT A TEMPERATURE IN THE RANGE FROM ABOUT 395*C, TO 600*C, AND BY PASSING A CARRIER GAS THROUGH SAID ZONE AS IN (3),

Claim 32

Dependent Claim 60 words

maintaining the average valence of the vanadium component of said oxide at a value in the range from about 4.1 to 4.5 during said second and third treatments by passing a gas containing a hydrocarbon component through or over said oxide, said gas being selected from the group consisting of air and molecular oxygen in admixture with an inert gas.

Claim 33

Dependent Claim 60 words

maintaining the average valence of the vanadium component of said oxide at a value in the range from about 4.1 to 4.5 during said second and third treatments by passing a gas containing a hydrocarbon component through or over said oxide, said gas being selected from the group consisting of air and molecular oxygen in admixture with an inert gas.

Claim 34

Dependent Claim 60 words

maintaining the average valence of the vanadium component of said oxide at a value in the range from about 4.1 to 4.5 during said second and third treatments by passing a gas containing a hydrocarbon component through or over said oxide, said gas being selected from the group consisting of air and molecular oxygen in admixture with an inert gas.

Claim 35

Dependent Claim 60 words

maintaining the average valence of the vanadium component of said oxide at a value in the range from about 4.1 to 4.5 during said second and third treatments by passing a gas containing a hydrocarbon component through or over said oxide, said gas being selected from the group consisting of air and molecular oxygen in admixture with an inert gas.

Claim 36

Dependent Claim 17 words

The method as in claim 3 wherein said transition temperature range is from about 450*C. to 500*C.

Claim 37

Independent Claim 127 words

The method for the preparation of a homogeneous mixed oxide of vanadium and phosphorus by reacting a pentavalent phosphorus oxide compound with a vanadium oxide compound In an aqueous medium, which comprises admixing said reactants with concentrated aqueous hydrochloric acid, the atomic ratio of phosphorus to vanadium in the mixture being in the range from about 1-2 to 1; adjusting the average valence of the vanadium component to a value in the range from about 3.9 to 4.5; concentrating the resulting solution by heating until a thick aqueous slurry is produced; drying said slurry to a solid of constant weight by maintaining it at a temperature at or below about 150*C; pulverizing the dried solid; and subjecting the dried solid to a series of three treatments by:

Claim 38

Independent Claim 127 words

The method for the preparation of a homogeneous mixed oxide of vanadium and phosphorus by reacting a pentavalent phosphorus oxide compound with a vanadium oxide compound In an aqueous medium, which comprises admixing said reactants with concentrated aqueous hydrochloric acid, the atomic ratio of phosphorus to vanadium in the mixture being in the range from about 1-2 to 1; adjusting the average valence of the vanadium component to a value in the range from about 3.9 to 4.5; concentrating the resulting solution by heating until a thick aqueous slurry is produced; drying said slurry to a solid of constant weight by maintaining it at a temperature at or below about 150*C; pulverizing the dried solid; and subjecting the dried solid to a series of three treatments by:

Claim 39

Dependent Claim 13 words

The method as in claim 6 wherein said atomic ratio is about 1.2.

Claim 40

Dependent Claim 28 words

The method as in claim 6 wherein said first treatment is at a temperature of about 385*C., and said second treatment is at a temperature of about 410*C.

Claim 41

Dependent Claim 15 words

The improved anhydrous mixed oxide composition prepared in accordance with the method of claim 6.

Claim 42

Dependent Claim 15 words

The composition of claim 9 wherein the phosphorus to vanadium atomic ration is about 1.2.

Claim 43

Independent Claim 66 words

The method for the preparation of an improved oxidation catalyst from a particulate complex mixed oxide dihydrate of vanadium and pentavalent phosphorus, said oxide having a phosphorus to vanadium atomic ratio in the range from about 1-2 to 1, and said vanadium having an average valence in the range from about 3.9 to 4.5, which comprises subjecting said oxide to a series of three treatments by:

Claim 44

Independent Claim 66 words

The method for the preparation of an improved oxidation catalyst from a particulate complex mixed oxide dihydrate of vanadium and pentavalent phosphorus, said oxide having a phosphorus to vanadium atomic ratio in the range from about 1-2 to 1, and said vanadium having an average valence in the range from about 3.9 to 4.5, which comprises subjecting said oxide to a series of three treatments by:

Claim 45

Dependent Claim 35 words

The method as in claim 11 wherein the temperature during said first treatment is about 385*C.; the temperature during said second treatment is about 410*C.; and the temperature during said third treatment is about 480*C.

Claim 46

Independent Claim 118 words

A METHOD FOR PREPARING A CATALYST COMPRISING A MIXED VANADIUM PHOSPHORUS OXIDE WHICH CMPRISES: A. MIXING AND HEATING A VANADIUM OXIDE COMPOUND WITH A PENETAVALENT PHOSPHORUS OXIDE COMPOUND IN THE PRESENCE OF A LIQUID MEDIUM TO OBTAIN A SLURRY CONTAINING VANADIUM-PHOSPHORUS OXIDE HYDRATE, B. REMOVING LIQUID MEDUIM FROM THE SLURRY TO OBTAIN THE OXIDE HYDRATES, C. HEATING THE OXIDE HYDRATE IN THE PRESENCE OF AN OXYGENCONTAINING GAS FOR ABOUT 0.5 TO 2,0 HOURS AND AT A TEMPERATURE BETWEEN ABOUT 370* AND 394*C. TO REMOVE WATER OF HYDRATION FROM THE OXIDE HYDRATE AND OBTAIN A RESULTING OXIDE, AND D. HEATING THE RESULTING OXIDE AT A TEMPERATURE BETWEEN ABOUT 395* AND 600*C, AND IN THE PRESENCE OF FLOWING OXYGEN-CONTAINING GAS.

Claim 47

Independent Claim 118 words

A METHOD FOR PREPARING A CATALYST COMPRISING A MIXED VANADIUM PHOSPHORUS OXIDE WHICH CMPRISES: A. MIXING AND HEATING A VANADIUM OXIDE COMPOUND WITH A PENETAVALENT PHOSPHORUS OXIDE COMPOUND IN THE PRESENCE OF A LIQUID MEDIUM TO OBTAIN A SLURRY CONTAINING VANADIUM-PHOSPHORUS OXIDE HYDRATE, B. REMOVING LIQUID MEDUIM FROM THE SLURRY TO OBTAIN THE OXIDE HYDRATES, C. HEATING THE OXIDE HYDRATE IN THE PRESENCE OF AN OXYGENCONTAINING GAS FOR ABOUT 0.5 TO 2,0 HOURS AND AT A TEMPERATURE BETWEEN ABOUT 370* AND 394*C. TO REMOVE WATER OF HYDRATION FROM THE OXIDE HYDRATE AND OBTAIN A RESULTING OXIDE, AND D. HEATING THE RESULTING OXIDE AT A TEMPERATURE BETWEEN ABOUT 395* AND 600*C, AND IN THE PRESENCE OF FLOWING OXYGEN-CONTAINING GAS.

Claim 48

Dependent Claim 22 words

A method in accordance with claim 13 wherein the step (d) heating is carried out at a temperature between 450* - 520*C.

Claim 49

Dependent Claim 22 words

A method in accordance with claim 14 wherein the valence of the vanadium is maintained between 4.1 and 4.5 during step (d).

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1978-10-27	1979-04-28	1979-10-28	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1982-10-27	1983-04-28	1983-10-28	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1986-10-27	1987-04-28	1987-10-28	$7700.00	Window Closed / Lapsed

Vanadium-phosphorus mixed oxide oxidation catalysts

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