IP Library Granted Patent US 10,252,251
Granted Patent B2
US 10,252,251 · App. 15/249,166 · Granted Apr 9, 2019

Production of organic materials using solid catalysts

Inventors: Hongfei Lin (Pullman, WA); Lisha Yang (Reno, NV)
Assignee: Board of Regents of the Nevada System of Higher Education, on Behalf of the University of Nevada, Reno
B01J29/7049B01J29/0308B01J35/002B01J35/1023B01J35/1042B01J35/1047B01J35/1061C07C67/00
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Quick Facts
Patent No.
US 10,252,251
App. No.
15/249,166
Granted
Apr 9, 2019
Kind
B2
Abstract

The present disclosure provides a method for producing organic compounds, such as esters, from an organic feedstock that includes at least one of a biopolymer or a lipid. The method includes heating the feedstock in the presence of a solid catalyst, such as a solid, inorganic Lewis acid catalyst, and reaction medium that includes an alcohol. At least certain ester products have an ester group corresponding to a substituent of the alcohol.

Claims (41)

1. A method for catalytically producing organic materials from a feedstock, the method comprising:

providing a feedstock comprising a substrate comprising cellulose;

contacting the feedstock with a reaction medium comprising an alcohol and having a critical temperature and with a solid inorganic Lewis acid catalyst comprising a mesoporous material isomorphically substituted with a transition metal, the mesoporous material having a silicon-to-transition metal ratio of between about 5:1 and about 100:1;

heating a mixture comprising the feedstock, reaction medium, and catalyst to a temperature that is at least substantially the critical temperature of the reaction medium; and

maintaining the mixture at the temperature for a period of time sufficient to form ester

products from the feedstock, wherein the catalyst converts at least a portion of the cellulose into an ester of lactic acid having an ester group corresponding to the alcohol.

2. The method of claim 1 , wherein the mixture is heated at a temperature of between about 220° C. and about 300° C.

3. The method of claim 1 , wherein the mixture is heated at a temperature of at least about 75% of the critical temperature of the reaction medium.

4. The method of claim 1 , wherein the mesoporous material isomorphically substituted with a transition metal comprises Zr-SBA-15.

5. The method of claim 1 , wherein the pores of the mesoporous material isomorphically substituted with a transition metal have an average pore size of between about 6 nm and about 50 nm.

6. The method of claim 1 , wherein the catalyst has an acid strength of between about 0.02 mmol/g NH 3 and about 10 mmol/g NH 3 , as measured by temperature-programmed desorption of ammonia.

7. The method of claim 1 , wherein the catalyst has a BET surface area of between about 600 m 2 /g and about 900 m 2 /g.

8. The method of claim 1 , wherein the pores of the mesoporous material isomorphically substituted with a transition metal have an average pore volume determined by the NLDFT model of between about 0.9 cm 3 /g and about 1.8 cm 3 /g.

9. The method of claim 1 , wherein the reaction medium comprising an alcohol and having a critical temperature is an alcohol-water mixture comprising between about 0.5% and about 10% by weight water.

10. The method of claim 1 , wherein the catalyst comprises Lewis acid sites and Brønsted acid sites.

11. The method of claim 1 , wherein the transition metal of the mesoporous material isomorphically substituted with a transition metal is Zr, Ti, Sn, Nb, Ga, Ge, V, or Fe.

12. The method of claim 1 , further comprising:

contacting the solid inorganic Lewis acid catalyst with between about 0.001 wt % and about 1 wt % of one or more alkali metal halides before contacting the feedstock with the solid inorganic Lewis acid catalyst; or

adding between about 0.001 wt % and about 1 wt % of one or more alkali metal halides to the mixture.

13. A method for catalytically producing organic materials from a feedstock, the method comprising:

providing a feedstock comprising a substrate comprising cellulose;

contacting the feedstock with a reaction medium comprising a mixture of water and an alkyl alcohol having between 1 and 15 carbon atoms, the reaction medium having a critical temperature, and with a solid inorganic catalyst comprising Zr-SBA-15;

heating a mixture comprising the feedstock, reaction medium, and catalyst to a temperature that is at least about 75% of the critical temperature of the reaction medium; and

maintaining the mixture at the temperature for a period of time sufficient to form ester

products from the feedstock, wherein the catalyst converts at least a portion of the cellulose into an ester of lactic acid having an ester group corresponding to the alcohol.

14. A method for catalytically producing organic materials from a feedstock, the method comprising:

providing a feedstock comprising a substrate comprising cellulose;

contacting the feedstock with a reaction medium comprising a mixture of water and an alkyl alcohol having between 1 and 15 carbon atoms, the reaction medium having a critical temperature, and with a solid inorganic catalyst comprising a mesoporous material isomorphically substituted with a transition metal, the mesoporous material having a silicon-to-transition metal ratio of between about 5:1 and about 100:1;

heating a mixture comprising the feedstock, reaction medium, and catalyst to a temperature that is at least about 90% of the critical temperature of the reaction medium; and

maintaining the mixture at the temperature for a period of time sufficient to form ester

products from the feedstock, wherein the catalyst converts at least a portion of the cellulose into an ester of lactic acid having an ester group corresponding to the alcohol.

15. The method of claim 13 , wherein the mixture is heated at a temperature of between about 220° C. and about 300° C.

16. The method of claim 13 , wherein the mixture is heated at a temperature of at least about 90% of the critical temperature of the reaction medium.

17. The method of claim 13 , wherein the solid inorganic catalyst has an acid strength of between about 0.02 mmol/g NH 3 and about 10 mmol/g NH 3 , as measured by temperature-programmed desorption of ammonia.

18. The method of claim 13 , further comprising:

contacting the solid inorganic catalyst with between about 0.001 wt % and about 1 wt % of one or more alkali metal halides before contacting the feedstock with the solid inorganic catalyst; or

adding between about 0.001 wt % and about 1 wt % of one or more alkali metal halides to the mixture.

19. The method of claim 14 , further comprising:

contacting the solid inorganic catalyst with between about 0.001 wt % and about 1 wt % of one or more alkali metal halides before contacting the feedstock with the solid inorganic catalyst; or

adding between about 0.001 wt % and about 1 wt % of one or more alkali metal halides to the mixture.

20. The method of claim 13 , wherein the Zr-SBA-15 has a silicon-to-zirconium ratio of between about 5:1 and about 100:1.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 29, 2021
From: BOARD OF REGENTS OF THE NEVADA SYSTEM OF HIGHER EDUCATION ON BEHALF OF THE UNIVERSITY OF NEVADA, RENO
To: NEVADA RESEARCH & INNOVATION CORPORATION
Reel/Frame 057026/0026 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 21, 2016
From: LIN, HONGFEI; YANG, LISHA
To: BOARD OF REGENTS OF THE NEVADA SYSTEM OF HIGHER EDUCATION, ON BEHALF OF THE UNIVERSITY OF NEVADA, RENO
Reel/Frame 039818/0219 →
CONFIRMATORY LICENSE Recorded Sep 19, 2016
From: UNIVERSITY OF NEVADA, RENO
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 040069/0527 →
Continuity (2)
Provisional Application 62211585 · Aug 28, 2015
Related Publication 20170057903A1 · Mar 2, 2017