IP Library Granted Patent US 8,889,938
Granted Patent B2
US 8,889,938 · App. 13/838,761 · Granted Nov 18, 2014

Methods of producing para-xylene

Inventors: Makoto N. Masuno (Elk Grove, CA); Patrick B. Smith (Midland, MI); Dennis A. Hucul (Midland, MI); Katherine Brune (Midland, MI); Ryan L. Smith (Sacramento, CA); John Bissell (Sacramento, CA); Dimitri A. Hirsch-Weil (Sacramento, CA); Edmund J. Stark (Midland, MI)
Assignee: Micromidas, Inc.
C07C51/16C07C2527/122C07C2527/188C07C2527/135C07C2/867C07C2527/128C07C2527/18C07C2527/138C07C2527/133
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 8,889,938
App. No.
13/838,761
Granted
Nov 18, 2014
Kind
B2
Abstract

The present disclosure provides methods to produce para-xylene, toluene, and other compounds from renewable sources (e.g., cellulose, hemicellulose, starch, sugar) and ethylene in the presence of a catalyst. For example, cellulose and/or hemicellulose may be converted into 2,5-dimethylfuran (DMF), which may be converted into para-xylene by cycloaddition of ethylene to DMF. Para-xylene can then be oxidized to form terephthalic acid.

Claims (24)

1. A method for producing para-xylene, comprising:

combining 2,5-hexanedione, ethylene, and catalyst to form a reaction mixture, wherein the catalyst is copper chloride, copper triflate, yttrium triflate, a heteropolyacid, or η 2 -ethylene-copper(II)triflate; and

producing para-xylene from at least a portion of the 2,5-hexanedione and ethylene in the reaction mixture.

2. The method of claim 1 , further comprising isolating para-xylene from the reaction mixture.

3. The method of claim 1 , wherein the 2,5-hexanedione, the ethylene, and the catalyst are further combined with a solvent system to form the reaction mixture.

4. The method of claim 3 , wherein the solvent system comprises an aprotic solvent.

5. The method of claim 3 , wherein the solvent system comprises an ether solvent.

6. The method of claim 3 , wherein the solvent system comprises a C1-C20 aliphatic solvent, a C6-C20 aromatic solvent, an alkyl phenyl solvent, a C2-C20 ether, a C2-C20 ester, a C1-C20 alcohol, a C2-C20 ketone, or any combinations or mixtures thereof.

7. The method of claim 3 , wherein the solvent system comprises dimethylacetamide, acetonitrile, sulfolane, dioxane, dioxane, dimethyl ether, diethyl ether, glycol dimethyl ether (monoglyme), ethylene glycol diethyl ether (ethyl glyme), diethylene glycol dimethyl ether (diglyme), diethylene glycol diethyl ether (ethyl digylme), triethylene glycol dimethyl ether (triglyme), diethylene glycol dibutyl ether (butyl diglyme), tetraethylene glycol dimethyl ether (tetraglyme), polyglyme, proglyme, highlyme, tetrahydrofuran, ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, cyclobutanone, cyclopentanone, cyclohexanone, cycloheptanone, cyclooctanone, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methyl lactate, ethyl lactate, propyl lactate, butyl lactate, triacetin, dibutylphthalate, butane, pentane, cyclopentane, hexane, cyclohexane, heptane, cycloheptane, octane, cyclooctane, nonane, decane, undecane, dodecane, hexadecane, tetrachloride, chloroform, dichloromethane, nitromethane, toluene, anisole, nitrobenzene, bromobenzene, N-methylpyrrole, para-xylene, mesitylene, dodecylbenzene, pentylbenzene, hexylbenzene, diphenyl ether, methyldiphenyl ether, ethyldiphenyl ether, water, or any combinations or mixtures thereof.

8. The method of claim 3 , wherein the solvent system comprises dioxane, glyme, diglyme, triglyme, decane, dodecane, para-xylene, or any combinations or mixtures thereof.

9. The method of claim 8 , wherein the solvent system comprises para-xylene.

10. The method of claim 1 , wherein the catalyst is copper chloride, copper triflate, or yttrium triflate.

11. The method of claim 1 , wherein the catalyst is a heteropolyacid.

12. The method of claim 1 , wherein the catalyst is η 2 -ethylene-copper(II)triflate.

13. The method of claim 3 , wherein the solvent system comprises an ether, a C 8+ alkyl solvent, or para-xylene.

14. The method of claim 1 , wherein the catalyst is copper chloride, copper triflate, or yttrium triflate; and the solvent system comprises dioxane, dodecane, para-xylene, or any mixtures or combinations thereof.

15. The method of claim 1 , wherein at least a portion of the 2,5-hexanedione and ethylene are converted to para-xylene at a temperature of at least 150° C.

16. The method of claim 15 , wherein at least a portion of the 2,5-hexanedione and ethylene are converted to para-xylene at a temperature of between 150° C. and 300° C.

17. The method of claim 1 , wherein the catalyst is copper chloride.

18. The method of claim 1 , wherein the catalyst is copper triflate.

19. The method of claim 1 , wherein the catalyst is yttrium triflate.

20. The method of claim 3 , wherein the solvent system comprises aliphatic solvent.

21. The method of claim 3 , wherein the solvent system comprises alkyl phenyl solvent.

22. The method of claim 15 , wherein at least a portion of the 2,5-hexanedione and ethylene are converted to para-xylene at a temperature of between 200° C. and 400° C.

Assignments (7)
CHANGE OF NAME Recorded Feb 14, 2022
From: MICROMIDAS, INC.
To: ORIGIN MATERIALS OPERATING, INC.
Reel/Frame 059109/0403 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 25, 2014
From: HIRSCH-WEIL, DIMITRI A.
To: MICROMIDAS, INC.
Reel/Frame 033179/0472 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 25, 2014
From: STARK, EDMUND J.
To: MICHIGAN MOLECULAR INSTITUTE
Reel/Frame 033179/0511 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 25, 2014
From: MICHIGAN MOLECULAR INSTITUTE
To: MICROMIDAS, INC.
Reel/Frame 033180/0659 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 16, 2013
From: MICHIGAN MOLECULAR INSTITUTE
To: MICROMIDAS, INC.
Reel/Frame 031414/0710 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 2, 2013
From: MASUNO, MAKOTO N.; SMITH, RYAN L.; BISSELL, JOHN; FOSTER, MARC
To: MICROMIDAS, INC.
Reel/Frame 031327/0220 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 2, 2013
From: SMITH, PATRICK B.; HUCUL, DENNIS A.; DUMITRASCU, ADINA; BRUNE, KATHERINE
To: MICHIGAN MOLECULAR INSTITUTE
Reel/Frame 031327/0163 →
Continuity (4)
Provisional Application 61611114 · Mar 15, 2012
Provisional Application 61651594 · May 25, 2012
Provisional Application 61701276 · Sep 14, 2012
Related Publication 20130245316A1 · Sep 19, 2013