Crystalline bis-ammonia transition metal molybdotungstate

Patent metadata

Field	Value
Publication number	US-2018169633-A1
Application number	US-201615373803-A
Country	US
Kind code	A1
Filing date	Dec 9, 2016
Priority date	Dec 15, 2015
Publication date	Jun 21, 2018
Grant date	—

Abstract

A unique crystalline bis-ammonia transition metal molybdotungstate 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

1 . A crystalline bis-ammonia transition metal molybdotungstate material having the formula:
(NH 3 ) 2-n M(OH 2 ) n Mo x W y O z
where ‘n’ varies from 0.1 to 2.0; ‘M’ represents a metal selected from Mg, Mn, Fe, Co Ni, Cu, Zn and mixtures thereof; ‘x’ varies from 0.5 to 1.5; ‘y’ varies from 0.01 to 0.25; the sum of (x+y) must be ≤1.501; ‘z’ is a number which satisfies the sum of the valences of M, Mo and W; the material having a unique x-ray powder diffraction pattern showing 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 transition metal molybdotungstate material of claim 1 wherein the crystalline bis-ammonia metal molybdotungstate 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 transition metal molybdotungstate material of claim 2 wherein the binder is selected from the group consisting of silicas, aluminas, and silica-aluminas.

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

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

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

7 . A method of making a crystalline bis-ammonia transition metal molybdotungstate material having the formula:
(NH 3 ) 2-n M(OH 2 ) n Mo x W y O z
where ‘n’ varies from 0.1 to 2.0; ‘M’ represents a metal selected from Mg, Mn, Fe, Co Ni, Cu, Zn and mixtures thereof; ‘x’ varies from 0.5 to 1.5; ‘y’ varies from 0.01 to 0.25; the sum of (x+y) must be ≤1.501; ‘z’ is a number which satisfies the sum of the valences of M, Mo and W; the material having a unique x-ray powder diffraction pattern showing 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 sources of M, W, 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 about 85 and about 100° C. until the resultant pH is between 8.5 and 9.5; and
(d) recovering the crystalline bis-ammonia transition metal molybdotungstate 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 bis-ammonia transition metal molybdotungstate material.

10 . The method of claim 7 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 bis-ammonia transition metal molybdotungstate material.

12 . A 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 transition metal molybdotungstate material having the formula:
(NH 3 ) 2-n M(OH 2 ) n Mo x W y O z
where ‘n’ varies from 0.1 to 2.0; ‘M’ represents a metal selected from Mg, Mn, Fe, Co Ni, Cu, Zn and mixtures thereof; ‘x’ varies from 0.5 to 1.5; ‘y’ varies from 0.01 to 0.25; the sum of (x+y) must be ≤1.501; ‘z’ is a number which satisfies the sum of the valences of M, Mo and W; the material having a unique x-ray powder diffraction pattern showing 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

Assignees

• Uop Llc

Inventors

• Miller Stuart
• Collins Laura
• Koster Susan C

Classifications

• B01J23/883 Primary

  and nickel · CPC title

• C10G49/04

  containing nickel, cobalt, chromium, molybdenum, or tungsten metals, or compounds thereof · CPC title

• B01J37/08

  Heat treatment {(B01J37/0009, B01J37/0018 take precedence)} · CPC title

• B01J21/04

  Alumina · CPC title

• B01J37/031

  Precipitation · CPC title