IP Library Granted Patent US 10,081,612
Granted Patent B2
US 10,081,612 · App. 15/417,110 · Granted Sep 25, 2018

Process for production of hexanetriol from 5-hydroxymethylfurfural

Inventors: Valery Sokolovskii (Santa Clara, CA); Mayya Lavrenko (Campbell, CA); Alfred Hagemeyer (Sunnyvale, CA); Eric L. Dias (Belmont, CA); James A. W. Shoemaker (Gilroy, CA); Vincent J. Murphy (San Jose, CA)
Assignee: ARCHER-DANIELS-MIDLAND COMPANY
C07D307/28B01J8/04C07C29/09C07C29/103C07C29/132C07C29/172C07C29/60C07D307/12C07D307/42B01J2208/027
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Quick Facts
Patent No.
US 10,081,612
App. No.
15/417,110
Granted
Sep 25, 2018
Kind
B2
Abstract

Industrial scale conversions of 5-hydroxymethylfurfural to commodity chemicals such as 1,2,6-hexanetriol and 1,6-hexanediol by chemocatalytic conversions using hydrogen and a heterogeneous reduction catalyst are provided. The reactions are suitable for use in continuous flow reactors. Methods of carrying out the conversions are provided, as are product and catalyst compositions.

Claims (56)

1. A process for preparing 2,5-bis-hydroxymethylfuran (BHMF) from 5-hydroxymethylfurfural (HMF) comprising:

reacting the 5-hydroxymethylfurfural (HMF) with hydrogen in a continuous flow reactor in the presence of an organic solvent and a heterogeneous reduction catalyst comprising Cu to form the 2,5-bis-hydroxymethylfuran (BHMF) over an on-stream period of at least 150 hours.

2. A process for preparing 2,5-bis-hydroxymethylfuran (BHMF) from 5-hydroxymethylfurfural (HMF) comprising:

reacting the 5-hydroxymethylfurfural (HMF) with hydrogen in a continuous flow reactor in the presence of an organic solvent and a heterogeneous reduction catalyst comprising Pt to form the 2,5-bis-hydroxymethylfuran (BHMF) over an on-stream period of at least 150 hours.

3. The process of claim 1 , wherein the heterogeneous reduction catalyst further comprises a modifier.

4. The process of claim 3 , wherein the modifier is selected from the group consisting of Mn, Co, Au, W, Cu, Zn, Mo, Sb, Bi and Pb.

5. The process of claim 1 , wherein the heterogeneous reduction catalyst comprises a combination of metals selected from the group consisting of Co—Cu and Ni—Cu.

6. The process of claim 1 , wherein the heterogeneous reduction catalyst further comprises a catalyst support.

7. The process of claim 6 , wherein the catalyst support is selected from the group consisting of carbons, aluminas, zirconias, silicas, alumina-silicas, titanias, alumina-titanias, silicon carbides and mixed phases thereof.

8. The process of claim 1 , wherein the heterogeneous reduction catalyst further comprises an alumina catalyst support.

9. The process of claim 1 further comprising:

feeding the 5-hydroxymethylfurfural (HMF) through a guard bed comprising a transition metal to the continuous flow reactor.

10. The process of claim 9 , wherein the guard bed comprises at least one transition metal selected from the group consisting of Ag, Zn, Cu, Fe, Ni, Co and Pb or a salt or combination thereof.

11. The process of claim 9 , wherein the guard bed comprises at least one transition metal selected from the group consisting of Ag, Zn, Cu and Pb or a salt or combination thereof.

12. The process of claim 1 , wherein the process comprises feeding the 5-hydroxymethylfurfural (HMF) to the continuous flow reactor at a concentration of greater than about 6 weight percent in the organic solvent.

13. The process of claim 1 , wherein the 2,5-bis-hydroxymethylfuran (BHMF) is formed with at least about 90% selectivity and at least 85% conversion of the 5-hydroxymethylfurfural (HMF).

14. The process of claim 1 , wherein the process comprises forming the 2,5-bis-hydroxymethylfuran (BHMF) with at least about 90% selectivity and at least 90% 5-hydroxymethylfurfural (HMF) conversion.

15. The process of claim 1 , wherein the process comprises forming the 2,5-bis-hydroxymethylfuran (BHMF) with at least about 95% selectivity and at least 90% 5-hydroxymethylfurfural (HMF) conversion.

16. The process of claim 1 , wherein the organic solvent comprises less than about 25 weight % water.

17. The process of claim 1 , wherein the organic solvent comprises from about 5 weight % to about 20 weight % water.

18. The process of claim 1 , wherein the 5-hydroxymethylfurfural (HMF) is reacted with hydrogen at a temperature in a range of about 50° C. to about 150° C. and at a pressure in a range of about 50 psi to about 2000 psi.

19. The process of claim 1 , wherein:

the 5-hydroxymethylfurfural (HMF) is reacted with hydrogen in the continuous flow reactor at a pressure in a range of about 50 psi to about 2000 psi;

the organic solvent comprises less than about 25 weight % water; and

the 2,5-bis-hydroxymethylfuran (BHMF) is formed with at least about 90% selectivity and at least 85% 5-hydroxymethylfurfural (HMF) conversion.

20. The process of claim 1 , further comprising reacting the 2,5-bis-hydroxymethylfuran (BHMF) with hydrogen in a continuous flow reactor in the presence of a heterogeneous reduction catalyst comprising at least one metal selected from the group consisting of Ni, Co, Cu, Ag, Pd, Pt and Ru or a combination thereof to form 2,5-bis-hydroxymethyltetrahydrofuran (BHMTHF).

21. The process of claim 20 , further comprising reacting the 2,5-bis-hydroxymethyltetrahydrofuran (BHMTHF) with hydrogen in a continuous flow reactor in the presence of a heterogeneous reduction catalyst comprising at least one metal selected from the group consisting of Ni, Co, Cu, Ag, Pt and Ru or a combination thereof to form 1,2,6-hexanetriol (HTO).

22. The process of claim 21 , further comprising reacting the 1,2,6-hexanetriol (HTO) with hydrogen in a continuous flow reactor in the presence of a heterogeneous reduction catalyst comprising at least one metal selected from the group consisting of Ni, Co, Cu, Ag, Pt and Ru or a combination thereof to form 1,6-hexanediol (HDO).

23. The process of claim 1 , further comprising reacting the 2,5-bis-hydroxymethylfuran (BHMF) with hydrogen in a continuous flow reactor in the presence of a heterogeneous reduction catalyst comprising at least one metal selected from the group consisting of Ni, Co, Cu, Ag, Pt, Pd and Ru or a combination thereof to form 1,2,6-hexanetriol (HTO).

24. The process of claim 23 , further comprising reacting the 1,2,6-hexanetriol (HTO) with hydrogen in a continuous flow reactor in the presence of a heterogeneous reduction catalyst comprising at least one metal selected from the group consisting of Ni, Co, Cu, Ag, Pt and Ru or a combination thereof to form 1,6-hexanediol (HDO).

25. The process of claim 2 , wherein the heterogeneous reduction catalyst further comprises a modifier.

26. The process of claim 25 , wherein the modifier is selected from the group consisting of Mn, Co, Au, W, Cu, Zn, Mo, Sb, Bi and Pb.

27. The process of claim 2 , wherein the heterogeneous reduction catalyst comprises a combination of metals which is Pt—Au.

28. The process of claim 2 , wherein the heterogeneous reduction catalyst further comprises a catalyst support.

29. The process of claim 28 , wherein the catalyst support is selected from the group consisting of carbons, aluminas, zirconias, silicas, alumina-silicas, titanias, alumina-titanias, silicon carbides and mixed phases thereof.

30. The process of claim 2 , wherein the heterogeneous reduction catalyst further comprises an alumina catalyst support.

31. The process of claim 2 further comprising:

feeding the 5-hydroxymethylfurfural (HMF) through a guard bed comprising a transition metal to the continuous flow reactor.

32. The process of claim 31 , wherein the guard bed comprises at least one transition metal selected from the group consisting of Ag, Zn, Cu, Fe, Ni, Co and Pb or a salt or combination thereof.

33. The process of claim 31 , wherein the guard bed comprises at least one transition metal selected from the group consisting of Ag, Zn, Cu and Pb or a salt or combination thereof.

34. The process of claim 2 , wherein the process comprises feeding the 5-hydroxymethylfurfural (HMF) to the continuous flow reactor at a concentration of greater than about 6 weight percent in the organic solvent.

35. The process of claim 2 , wherein the 2,5-bis-hydroxymethylfuran (BHMF) is formed with at least about 90% selectivity and at least 85% conversion of the 5-hydroxymethylfurfural (HMF).

36. The process of claim 2 , wherein the process comprises forming the 2,5-bis-hydroxymethylfuran (BHMF) with at least about 90% selectivity and at least 90% 5-hydroxymethylfurfural (HMF) conversion.

37. The process of claim 2 , wherein the process comprises forming the 2,5-bis-hydroxymethylfuran (BHMF) with at least about 95% selectivity and at least 90% 5-hydroxymethylfurfural (HMF) conversion.

38. The process of claim 2 , wherein the organic solvent comprises less than about 25 weight % water.

39. The process of claim 2 , wherein the organic solvent comprises from about 5 weight % to about 20 weight % water.

40. The process of claim 2 , wherein the 5-hydroxymethylfurfural (HMF) is reacted with hydrogen at a temperature in a range of about 50° C. to about 150° C. and at a pressure in a range of about 50 psi to about 2000 psi.

41. The process of claim 2 , wherein:

the 5-hydroxymethylfurfural (HMF) is reacted with hydrogen in the continuous flow reactor at a pressure in a range of about 50 psi to about 2000 psi;

the organic solvent comprises less than about 25 weight % water; and

the 2,5-bis-hydroxymethylfuran (BHMF) is formed with at least about 90% selectivity and at least 85% 5-hydroxymethylfurfural (HMF) conversion.

42. The process of claim 2 , further comprising reacting the 2,5-bis-hydroxymethylfuran (BHMF) with hydrogen in a continuous flow reactor in the presence of a heterogeneous reduction catalyst comprising at least one metal selected from the group consisting of Ni, Co, Cu, Ag, Pd, Pt and Ru or a combination thereof to form 2,5-bis-hydroxymethyltetrahydrofuran (BHMTHF).

43. The process of claim 42 , further comprising reacting the 2,5-bis-hydroxymethyltetrahydrofuran (BHMTHF) with hydrogen in a continuous flow reactor in the presence of a heterogeneous reduction catalyst comprising at least one metal selected from the group consisting of Ni, Co, Cu, Ag, Pt and Ru or a combination thereof to form 1,2,6-hexanetriol (HTO).

44. The process of claim 43 , further comprising reacting the 1,2,6-hexanetriol (HTO) with hydrogen in a continuous flow reactor in the presence of a heterogeneous reduction catalyst comprising at least one metal selected from the group consisting of Ni, Co, Cu, Ag, Pt and Ru or a combination thereof to form 1,6-hexanediol (HDO).

45. The process of claim 2 , further comprising reacting the 2,5-bis-hydroxymethylfuran (BHMF) with hydrogen in a continuous flow reactor in the presence of a heterogeneous reduction catalyst comprising at least one metal selected from the group consisting of Ni, Co, Cu, Ag, Pt, Pd and Ru or a combination thereof to form 1,2,6-hexanetriol (HTO).

46. The process of claim 45 , further comprising reacting the 1,2,6-hexanetriol (HTO) with hydrogen in a continuous flow reactor in the presence of a heterogeneous reduction catalyst comprising at least one metal selected from the group consisting of Ni, Co, Cu, Ag, Pt and Ru or a combination thereof to form 1,6-hexanediol (HDO).

Assignments (5)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 7, 2018
From: RENNOVIA INC.
To: ARCHER-DANIELS-MIDLAND COMPANY
Reel/Frame 045137/0103 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 21, 2018
From: RENNOVIA INC.
To: ARCHER-DANIELS-MIDLAND COMPANY
Reel/Frame 045385/0614 →
RELEASE OF SECURITY INTEREST Recorded Feb 15, 2018
From: PACIFIC WESTERN BANK
To: RENNOVIA INC.
Reel/Frame 044946/0264 →
SECURITY INTEREST Recorded Jan 23, 2018
From: RENNOVIA INC.
To: PACIFIC WESTERN BANK
Reel/Frame 044703/0960 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 30, 2017
From: SOKOLOVSKII, VALERY; LAVRENKO, MAYYA; HAGEMEYER, ALFRED; DIAS, ERIC L.; SHOEMAKER, JAMES A.W.; MURPHY, VINCENT J.
To: RENNOVIA INC.
Reel/Frame 043984/0567 →
Continuity (3)
Continuation 14957551 · Dec 2, 2015
Provisional Application 62086651 · Dec 2, 2014
Related Publication 20170298036A1 · Oct 19, 2017