Calcination process to produce enhanced ODH catalyst

Patent metadata

Field	Value
Publication number	US-11654419-B2
Application number	US-202117236669-A
Country	US
Kind code	B2
Filing date	Apr 21, 2021
Priority date	Mar 26, 2018
Publication date	May 23, 2023
Grant date	May 23, 2023

Abstract

Mixed metal oxide catalysts having an amorphous content of not less than 40 wt. % are prepared by calcining the catalyst precursor fully or partially enclosed by a porous material having a melting temperature greater than 600° C. in an inert container including heating the catalyst precursor at a rate from 0.5 to 10° C. per minute from room temperature to a temperature from 370° C. to 540° C. under a stream of pre heated gas chosen from steam and inert gas and mixtures thereof at a pressure of greater than or equal to 1 psig having a temperature from 300° C. to 540° C. and holding the catalyst precursor at that temperature for at least 2 hours and cooling the catalyst precursor to room temperature.

First claim

What is claimed is:

1. A method to calcine a catalyst precursor of the formula
Mo 1 V 0.1-1 Nb 0.1-1 Te 0.01-0.2 X 0-2 O d
where X is chosen from Pd, Sb Ba, Al, W, Ga, Bi, Sn, Cu, Ti, Fe, Co, Ni, Cr, Zr, Ca, oxides thereof and mixtures thereof, and d is a number to satisfy the valence of the catalyst while maintaining an amorphous content of not less than 40 wt. % the method comprising
calcining the catalyst precursor in an inert container with flow passage there through, at a rate from 0.5 to 10° C. per minute from room temperature to a holding temperature from 370° C. to 540° C. under a stream of pre heated gas chosen from steam and inert gas and mixtures thereof at a rate of flow comparable to a flow rate of not less than 150 sccm through a 2.54 cm diameter tube with a length of 152 cm, at a pressure of greater than or equal to 1 psig, said stream of pre heated gas having a temperature from 300° C. to 540° C.;
holding the catalyst precursor at the holding temperature for at least 2 hours; and
cooling the catalyst precursor to room temperature, said catalyst precursor being fully or partially enclosed by a porous material having a melting temperature greater than 600° C.

2. The method according to claim 1 , wherein the inert container is made from high temperature glass, quartz, ceramics, or steel.

3. The method according to claim 2 , wherein the inert container has a heat conductivity greater than 0.34 W m −1 ·K.

4. The method according to claim 1 , wherein the pressure of inert gas is greater than 1 psig.

5. The method according to claim 4 , wherein rate for heating the catalyst precursor is 0.9 to 2.0° C. per min.

6. The method according to claim 4 , wherein the catalyst precursor is held at the holding temperature from 2-24 hours.

7. The method according to claim 6 , wherein the holding temperature is from 400° C. to 525° C.

8. The method according to claim 7 , wherein the inert gas comprises nitrogen.

9. The method according to claim 8 , wherein the porous material is chosen from glass and mineral fiber.

10. The method according to claim 9 , wherein charcoal or activated carbon is present on an outer surface of the porous material in an amount up to 0.5 g per 1 g of catalyst precursor.

11. The method according to claim 10 , wherein X is one or more metals and oxides thereof are chosen from Pd, Sb, Ba, Al, Cu, Ti, Fe, Ca, Zr and mixtures thereof.

12. The method according to claim 11 , wherein the molar ratio of said one or more metals and oxides chosen from Pd, Sb, Ba, Al, Cu, Ti, Fe, Ca, Zr and mixtures thereof to Mo is from 1:0.001-0.3.

13. The method according to claim 12 , wherein the X is chosen from of one or more metals and oxides thereof are chosen from Pd, Sb, Ba, Al, Cu and mixtures thereof.

14. The method according to claim 1 , wherein in the catalyst precursor X is absent.

15. The method according to claim 14 , wherein the catalyst precursor has the formula:
Mo 1.0 V 0.10-0.49 Te 0.06-0.17 Nb 0.13-0.19 O d .

Assignees

• Nova Chem Int Sa

Inventors

• Simanzhenkov Vasily
• Gao Xiaoliang
• Sullivan David
• Styles Yipei
• Kim Yoonhee
• Drag Hanna
• Barnes Marie

Classifications

• B01J2235/00

  Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties · CPC title

• B01J35/80

  characterised by their amorphous structures · CPC title

• B01J2235/30

  Scanning electron microscopy; Transmission electron microscopy · CPC title

• B01J35/70

  characterised by their crystalline properties, e.g. semi-crystalline (catalysts comprising carbon B01J21/18; molecular sieves B01J29/00) · CPC title

• B01J2235/15

  X-ray diffraction · CPC title