# US 11,110,438 B2 · Methods for preparation and use of liquid synthesis catalysts

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- Number: US 11,110,438 B2
- Document ID: US11110438B2
- Status: Granted
- Kind: B2
- Application number: 16/528,124
- Filed: 2019-07-31
- Published: 2020-02-06
- Granted: 2021-09-07
- Earliest claimed: 2018-07-31
- Applicants: Board of Regents, The University of Texas System
- Inventors: Frederick M. MacDonnell; Brian H. Dennis
- Web page: https://patentgrep.com/patent/US11110438B2

## CPC

- B01J 23/8913: {Cobalt and noble metals}
- B01J 21/08: Silica
- B01J 23/75: Cobalt
- B01J 35/393: {Metal or metal oxide crystallite size}
- B01J 35/45: Nanoparticles
- B01J 37/0205: {in several steps}
- B01J 37/0207: {Pretreatment of the support}
- B01J 37/0236: {Drying, e.g. preparing a suspension, adding a soluble salt and drying}
- B01J 37/0242: {Coating followed by impregnation}
- B01J 37/08: Heat treatment {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/088: {Decomposition of a metal salt}
- B01J 37/18: with gases containing free hydrogen
- C07C 1/0435: {containing a metal of group 8 or a compound thereof}
- C07C 1/0445: {Preparation; Activation}
- C10G 2/332: {of the iron-group}
- B01J 35/37: Crush or impact strength
- B01J 35/40: characterised by dimensions, e.g. grain size (in a colloidal state B01J35/23; crystallite size B01J35/77)
- B01J 35/55: Cylinders or rings
- B01J 2235/30: Scanning electron microscopy; Transmission electron microscopy
- C07C 2521/08: Silica
- C07C 2523/46: Ruthenium, rhodium, osmium or iridium
- C07C 2523/75: Cobalt
- C07C 2523/89: combined with noble metals
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C10G: CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION (cracking to hydrogen or synthesis gas C01B; cracking or pyrolysis of hydrocarbon gases to individual hydrocarbons or mixtures thereof of definite or specified constitution C07C; cracking to cokes C10B); RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES

## Abstract

Described herein are catalysts relating to liquid synthesis, methods of their preparation, and methods of their use. In an embodiment according to the present disclosure, a method of producing a catalyst for liquid synthesis comprises: providing a silica oxide support; pretreating the silica oxide support to remove air and moisture; impregnating the pretreated silica oxide support with cobalt from a cobalt source using a cobalt impregnation method; and calcinating the impregnated silica oxide support in an oven with a temperature ramping profile, wherein the calcinating comprises feeding air into the oven.

## Claims

### Claim 1

A method of using a liquid synthesis catalyst, comprising:
impregnating a silica oxide support with cobalt;
drying the impregnated silica oxide support with an inert gas at a temperature of about 90° C. to about 130° C.;
after drying with the inert gas, calcinating the impregnated silica oxide support in the presence of oxygen to produce a liquid synthesis catalyst;
positioning the liquid synthesis catalyst in a reactor;
bedding and packing the liquid synthesis catalyst in the reactor;
reducing the liquid synthesis catalyst with H2 gas;
cooling the reactor to about 110° C. to about 160° C. while purging with H2 gas and increasing the reactor pressure to a set pressure point;
activating the liquid synthesis catalyst by introducing a gas stream into the reactor, wherein the gas stream comprises H2 gas and CO from a CO source at a molar ratio of 2:1 H2 to CO; and
collecting the reaction products in a reaction vessel.

### Claim 2 (depends on 1)

The method of claim 1, wherein the bedding and packing comprises diluting the liquid synthesis catalyst with quartz and holding the mixture in a position in the reactor.

### Claim 3 (depends on 1)

The method of claim 1, wherein the set pressure point is about 150 psig to about 300 psig.

### Claim 4 (depends on 1)

The method of claim 1, further comprising separating the collected reaction products.

### Claim 5 (depends on 1)

The method of claim 1, wherein the inert gas is nitrogen (N2) gas.