Hydrothermal synthesis of alkali promoted MOS2-based catalyst

Patent metadata

Field	Value
Publication number	US-10316254-B2
Application number	US-201515522644-A
Country	US
Kind code	B2
Filing date	Oct 31, 2015
Priority date	Oct 31, 2014
Publication date	Jun 11, 2019
Grant date	Jun 11, 2019

Abstract

Certain embodiments are directed to method for making and using an alkali promoted transition metal sulfide Fischer Tropsch catalyst. Certain embodiments are directed to alkali promoted transition metal sulfide Fischer Tropsch catalyst synthesized using steps comprising (i) mixing an ammonium tetrathiomolybdate (ATM) precursor compound with an alkali metal compound and molybdenum disulfide in deionized water to form a reaction mixture, (ii) heating the reaction mixture at a temperature of at least 200, 250, 300, 350, 400C at a pressure of at lease 900, 1000, 1100, 1500, 2000 psi for more than 0.5 1, 1.5, 2.0, 3 or more hours to form a reaction product, (iii) filtering, washing, and drying the reaction product.

First claim

The invention claimed is:

1. A method of synthesizing alkali promoted transition metal sulfide Fischer-Tropsch catalyst using steps comprising of:
(i) mixing an ammonium tetrathiomolybdate (ATM) precursor compound with an alkali metal compound and molybdenium disulfide in deionized water forming a reaction mixture;
(ii) heating the reaction mixture at a temperature above 250° C. and at a pressure above 1000 psi for more than 1 hour to form a transition metal sulfide Fischer-Tropsch catalyst; and
(iii) filtering, washing, and drying the transition metal sulfide Fischer-Tropsch catalyst.

2. Method of claim 1 , wherein the ATM precursor, alkali metal, and molybdenium is present at a starting molar ratio of about 5:0.3:1.

3. Method of claim 1 , wherein the alkali metal is potassium.

4. Method of claim 1 , wherein the ammonium tetrathiomolybdate (ATM) precursor compound is synthesized by steps comprising:
(i) dissolving heptamolybdate in deionized water,
(ii) adding ammonium sulfide solution, and
(iii) heating the solution above 55° C. for 30 minutes with stirring to produce the ammonium tetrathiomolybdate (ATM) precursor compound.

5. A transition metal sulfide Fischer-Tropsch catalyst produced using steps comprising of:
(i) mixing an ammonium tetrathiomolybdate (ATM) precursor compound with an alkali metal compound and molybdenium disulfide in deionized water forming a reaction mixture;
(ii) heating the reaction mixture at a temperature above 250° C. and at a pressure above 1000 psi for more than 1 hour to form the transition metal sulfide Fischer-Tropsch catalyst and
(iii) filtering, washing, and drying the transition metal sulfide Fischer-Tropsch catalyst.

6. The transition metal sulfide Fischer-Tropsch catalyst of claim 5 , whererin the alkali metal is cesium, the reaction mixture further comprises cobalt nitrate hexahydrate, and the transition metal sulfide Fischer-Tropsch catalyst is a Cs 3 Co 5 MoS 2 catalyst.

7. A method of synthesizing alkali promoted transition metal sulfide Fischer-Tropsch catalyst using steps comprising of:
(i) mixing an ammonium tetrathiomolybdate (ATM) precursor compound with an alkali metal compound, cobalt nitrate hexahydrate, and molybdenium disulfide in deionized water to form a reaction mixture;
(ii) heating the reaction mixture at a temperature above 250° C. at a pressure above 1000 psi for more than 1 hour to form a transition metal sulfide Fischer-Tropsch catalyst; and
(iii) filtering, washing, and drying the transition metal sulfide Fischer-Tropsch catalyst.

8. The method of claim 7 , wherein the ATM precursor, alkali metal, cobalt, and molybdenium is present at a starting molar ratio of 5:0.3:0.3:1.

9. The method of claim 7 , wherein the alkali metal is potassium.

10. The method of claim 7 , wherein the ammonium tetrathiomolybdate (ATM) precursor compound is synthesized by steps comprising of:
(i) dissolving heptamolybdate in deionized water,
(ii) adding ammonium sulfide solution, and
(iii) heating the solution above 55° C. for 30 minutes with stirring to produce the ammonium tetrathiomolybdate (ATM) precursor compound.

11. A process for converting synthesis gas to hydrocarbons comprising contacting a transition metal sulfide Fischer-Tropsch catalyst with synthesis gas at a pressure 250 to 500 psi and a temperature 250 to 400° C. in order to convert the synthesis gas into hydrocarbons,
wherein the transition metal sulfide Fischer-Tropsch catalyst is made with a method comprising:
mixing an ammonium tetrathiomolybdate (ATM) precursor compound with an alkali metal compound and molybdenium disulfide in deionized water forming a reaction mixture;
heating the reaction mixture at a temperature above 250° C. and at a pressure above 1000 psi for more than 1 hour to form the transition metal sulfide Fischer-Tropsch catalyst and
filtering, washing, and drying the transition metal sulfide Fischer-Tropsch catalyst.

12. The process of claim 11 , wherein the alkali metal is cesium, the reaction mixture further comprises cobalt nitrate hexahydrate, and the transition metal sulfide Fischer-Tropsch catalyst is a Cs 3 Co 5 MoS 2 , Cs 3 MoS 2 , CsCo 0.5 MoS 2 , or Co 0.5 MoS 2 catalyst.

13. The process of claim 11 , wherein the synthesis gas has a H 2 :CO ratio of about 0.8.

Assignees

• Molina Belinda D
• Torres Brenda
• Zarei Chaleshtori Maryam
• Chianelli Russell R
• Benson Tracy
• Hosseini Mahsa
• Univ Texas

Inventors

• Molina Belinda D
• Torres Brenda
• Zarei-Chaleshtori Maryam
• Chianelli Russell R
• Benson Tracy
• Hosseini Mahsa

Classifications

• C10G2/33

  characterised by the catalyst used · CPC title

• B01J27/051

  Molybdenum · CPC title

• B01J37/06

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

• C10G2/332 Primary

  of the iron-group · CPC title

• C01G51/30

  Chemistry & Metallurgy · mapped topic