IP Library Granted Patent US 11,498,062
Granted Patent B2
US 11,498,062 · App. 16/337,603 · Granted Nov 15, 2022

Phosphorus-containing solid catalysts and reactions catalyzed thereby, including synthesis of p-xylene

Inventors: Hong Je Cho (Amherst, MA); Wei Fan (Amherst, MA); Michael Tsapatsis (Edina, MN); Paul J. Dauenhauer (Shoreview, MN); Limin Ren (Minneapolis, MN); Raul Lobo (Newark, DE)
Assignees: Regents of the University of Minnesota; University of Massachusetts Amherst; University of Delaware
B01J29/85B01J29/40B01J29/7007B01J35/109B01J35/1085B01J37/0201B01J37/28C07C1/24C07C2/865C07C6/06C07C51/42B01J2229/18B01J2229/183B01J2229/186B01J2229/37C07C2521/04C07C2521/06C07C2521/08C07C2521/10C07C2521/12C07C2521/18C07C2523/10C07C2523/20C07C2527/167C07C2527/18C07C2527/188C07C2529/08C07C2529/40C07C2529/70C07C2529/82C07C2529/85
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Quick Facts
Patent No.
US 11,498,062
App. No.
16/337,603
Granted
Nov 15, 2022
Kind
B2
Abstract

Methods and phosphorus-containing solid catalysts for catalyzing dehydration of cyclic ethers (e.g., furans, such as 2,5-dimethylfuran) and alcohols (e.g., ethanol and isopropanol). The alcohols and cyclic ethers may be derived from biomass. One example includes a tandem Diels-Alder cycloaddition and dehydration of biomass-derived 2,5-dimethyl-furan and ethylene to renewable p-xylene. The phosphorus-containing solid catalysts are also active and selective for dehydration of alcohols to alkenes.

Claims (23)

1. A catalyst comprising:

a porous material, wherein the porous material is a molecular sieve framework comprising:

a zeolite beta (BEA) defining micropores bounded by

12-membered tetrahedral atom rings;

silicon;

aluminum; and

phosphorus coupled to the porous material,

wherein a ratio of silicon atoms to aluminum atoms in the molecular sieve framework is at least 1000:1; and

wherein when 2,5-dimethylfuran and ethylene are contacted in the presence of the catalyst, and after dehydration, p-xylene is produced in a yield of at least 90%.

2. The catalyst of claim 1 , wherein a ratio of silicon atoms to phosphorus atoms is in a range of 3:1 to 150:1.

3. A method of synthesizing the catalyst of claim 1 , the method comprising:

contacting a porous material with a phosphorus-containing compound to yield a wet porous material comprising phosphorus;

removing water from the wet porous material comprising phosphorus to yield a dry porous material comprising phosphorus; and

calcining the dry porous material comprising phosphorus to yield a catalyst comprising phosphorus coupled to the porous material.

4. The method of claim 3 , further comprising solvo-thermally synthesizing the porous material in the presence of the phosphorus-containing compound to yield the wet porous material comprising phosphorus.

5. The method of claim 3 , further comprising removing aluminum from the porous material before contacting the porous material with the phosphorus-containing compound.

6. The method of claim 3 , wherein the phosphorus-containing compound comprises phosphoric acid.

7. The method of claim 3 , wherein the phosphorus-containing compound comprises at least one of tetra(n-butyl) phosphonium hydroxide, tetramethyl phosphonium hydroxide, tetraethyl phosphonium hydroxide, and tetrapropyl phosphonium hydroxide.

8. A method for synthesizing p-xylene, the method comprising:

contacting, in the presence of the catalyst of claim 1 , biomass-derived 2,5-dimethylfuran with ethylene in a nonaqueous solvent to yield p-xylene.

9. The method of claim 8 , wherein the contacting yields a cycloadduct, and further comprising catalyzing, with the catalyst, dehydration of the cycloadduct to yield the p-xylene.

10. The catalyst of claim 1 , wherein a total pore volume of the porous material is about 0.8 cm 3 /g.

11. The catalyst of claim 1 , wherein a BET surface area obtained from argon adsorption-desorption isotherms is about 500 m 2 /g.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 14, 2021
From: LOBO, RAUL
To: UNIVERSITY OF DELAWARE
Reel/Frame 057478/0371 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 22, 2021
From: CHO, HONG JE; FAN, WEI
To: UNIVERSITY OF MASSACHUSETTS
Reel/Frame 056950/0689 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 7, 2021
From: TSAPATSIS, MICHAEL; DAUENHAUER, PAUL J.; REN, LIMIN
To: REGENTS OF THE UNIVERSITY OF MINNESOTA
Reel/Frame 056451/0804 →
CONFIRMATORY LICENSE Recorded Mar 8, 2021
From: UNIVERSITY OF MASSACHUSETTS AMHERST
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 055525/0475 →
Continuity (7)
Provisional Application 62419247 · Nov 8, 2016
Provisional Application 62419202 · Nov 8, 2016
Provisional Application 62414302 · Oct 28, 2016
Provisional Application 62410922 · Oct 21, 2016
Provisional Application 62410919 · Oct 21, 2016
Provisional Application 62402238 · Sep 30, 2016
Related Publication 20190344252A1 · Nov 14, 2019
Cited By (1)
US 12,330,133