Crystalline bis-ammonia metal molybdate

Patent metadata

Field	Value
Publication number	US-10400181-B2
Application number	US-201615370574-A
Country	US
Kind code	B2
Filing date	Dec 6, 2016
Priority date	Dec 15, 2015
Publication date	Sep 3, 2019
Grant date	Sep 3, 2019

Abstract

A unique crystalline bis-ammonia metal molybdate material has been developed. The material may be used as a hydroprocessing catalyst. The hydroprocessing may include hydrodenitrification, hydrodesulfurization, hydrodemetallation, hydrodearomatization, hydrodesilication, hydroisomerization, hydrotreating, hydrofining, and hydrocracking.

First claim

The invention claimed is:

1. A crystalline bis-ammonia metal molybdate material having the formula:
(NH 3 ) 2−n M(OH 2 ) n Mo x O y
where ‘n’ varies from 0.1 to less than 2.0; ‘M’ is a metal selected from Mg, Mn, Fe, Co, Ni, Cu, Zn, and mixtures thereof; ‘x’ varies from 0.5 to 1.5; ‘y’ is a number which satisfies the sum of the valences of M and Mo, the material having a unique x-ray powder diffraction pattern showing the peaks at the d-spacings listed in Table A:

TABLE A

d (Å)
I/I 0 %

7.49-7.28
vs

 5.1-5.05
s

 4.4-4.257
w

3.966-3.915
m

 3.69-3.645
s

3.52-3.48
m

3.35-3.32
m

3.31-3.29
m

 3.12-3.097
w

  3-2.97
m

2.76-2.73
m.

2. The crystalline bis-ammonia metal molybdate material of claim 1 wherein the crystalline bis-ammonia metal molybdate material is present in a mixture with at least one binder and wherein the mixture comprises up to 25 wt % binder.

3. The crystalline bis-ammonia metal molybdate material of claim 2 wherein the binder is selected from the group consisting of silicas, aluminas, and silica-aluminas.

4. The crystalline bis-ammonia metal molybdate material of claim 1 wherein M is nickel or cobalt.

5. The crystalline bis-ammonia metal molybdate material of claim 1 wherein M is nickel.

6. The crystalline bis-ammonia metal molybdate material of claim 1 wherein the crystalline bis-ammonia metal molybdate material is sulfided.

7. A method of making a crystalline bis-ammonia metal molybdate material having the formula:
(NH 3 ) 2−n M(OH 2 ) n MO x O y
where ‘n’ varies from 0.1 to less than 2.0; ‘M’ is a metal selected from Mg, Mn, Fe, Co, Ni, Cu, Zn, and mixtures thereof; ‘x’ varies from 0.5 to 1.5; ‘y’ is a number which satisfies the sum of the valences of M and Mo, the material having a unique x-ray powder diffraction pattern showing the peaks at the d-spacings listed in Table A:

TABLE A

d (Å)
I/I 0 %

7.49-7.28
vs

 5.1-5.05
s

 4.4-4.257
w

3.966-3.915
m

 3.69-3.645
s

3.52-3.48
m

3.35-3.32
m

3.31-3.29
m

 3.12-3.097
w

  3-2.97
m

2.76-2.73
m

the method comprising:
(a) forming a reaction mixture containing NH 3 , H 2 O, and sources of M and Mo;
(b) adjusting the pH of the reaction mixture to a pH of from about 8.5 to about 10;
(c) heating the reaction mixture to between 85-100° C. until the resultant pH is between 8.5 and 9.5; and
(d) recovering the crystalline bis-ammonia metal molybdate material.

8. The method of claim 7 wherein the recovering is by filtration or centrifugation.

9. The method of claim 7 further comprising adding a binder to the recovered crystalline bis-ammonia metal molybdate material.

10. The method of claim 9 wherein the binder is selected from the group consisting of aluminas, silicas, and alumina-silicas.

11. The method of claim 7 further comprising sulfiding the recovered crystalline bis-ammonia metal molybdate material.

12. A hydroprocessing conversion process comprising contacting a feed with a catalyst at conversion conditions to give at least one product, the catalyst comprising: a crystalline bis-ammonia metal molybdate material having the formula:
(NH 3 ) 2−n M(OH 2 ) n MO x O y
where ‘n’ varies from 0.1 to less than 2.0; ‘M’ is a metal selected from Mg, Mn, Fe, Co, Ni, Cu, Zn, and mixtures thereof; ‘x’ varies from 0.5 to 1.5; ‘y’ is a number which satisfies the sum of the valences of M and Mo, the material having a unique x-ray powder diffraction pattern showing the peaks at the d-spacings listed in Table A:

TABLE A

d (Å)
I/I 0 %

7.49-7.28
vs

 5.1-5.05
s

 4.4-4.257
w

3.966-3.915
m

 3.69-3.645
s

3.52-3.48
m

3.35-3.32
m

3.31-3.29
m

Assignees

• Uop Llc

Inventors

• Miller Stuart
• Koster Susan C

Classifications

• B01J37/20

  Sulfiding · CPC title

• B01J23/8892

  Manganese · CPC title

• B01J23/883

  and nickel · CPC title

• B01J23/88

  Molybdenum · CPC title

• B01J37/088

  Decomposition of a metal salt · CPC title