IP Library Granted Patent US 11,827,722
Granted Patent B2
US 11,827,722 · App. 17/356,085 · Granted Nov 28, 2023

Cellulose acetate aerogels

Inventors: Anurodh Tripathi (Raleigh, NC); Saad A. Khan (Raleigh, NC); Orlando J. Rojas (Raleigh, NC); Gregory N. Parsons (Raleigh, NC); Jeremy Kenneth Steach (Kingsport, TN); Jos Simon de Wit (Kingsport, TN); S. M. Bedarul Islam (Kingsport, TN); Jacob Donald Goodrich (Kingsport, TN)
Assignee: North Carolina State University
C08B15/005C08J9/28C08J9/36C08L1/12C08L1/14C08J2201/026C08J2201/0484C08J2205/022C08J2205/024C08J2205/026C08J2207/00C08J2301/12
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Quick Facts
Patent No.
US 11,827,722
App. No.
17/356,085
Granted
Nov 28, 2023
Kind
B2
Abstract

Mechanically strong, biodegradable and reusable aerogels are disclosed, which can be made with a cross-linked cellulose ester, and which exhibit a low density and high porosity. The aerogels disclosed herein may be used as sorbent materials and can be modified with a hydrophobic and/or oleophilic agent.

Claims (30)

1. An aerogel comprising a cross-linked cellulose ester having a degree of substitution of from about 1.0 to about 2.8, and further comprising a hydrophobic agent,

wherein the aerogel has a bulk density of from about 15 mg/cc to about 85 mg/cc, and

wherein the cellulose ester is a (C 1 -C 10 )alkyl-C(O)-functionalized cellulose.

2. The aerogel of claim 1 , wherein the degree of substitution of the cellulose ester is from about 1.8 to about 2.6.

3. The aerogel of claim 1 , wherein the cellulose ester is cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate or a combination thereof.

4. The aerogel of claim 1 , wherein the cellulose ester is cross-linked via an ester, ether or urethane linkage.

5. The aerogel of claim 4 , comprising a cross-linking agent at from about 1 wt. % to about 15 wt. %.

6. The aerogel of claim 4 , comprising the cellulose ester at from about 85 wt. % to about 99 wt. %.

7. The aerogel of claim 5 , wherein the cross-linking agent is selected from at least one of a C 7 -C 20 aromatic anhydride, a (C 5 -C 20 )cycloalkyl anhydride, a bis(halo(C 1 -C 3 )alkyl)-(C 5 -C 20 )aromatic, a bis(halo(C 1 -C 3 )alkyl)(C 3 -C 7 )cycloalkyl, a bis(isocyanato(C 1 -C 3 )alkyl)(C 5 -C 20 )aromatic, or a bis(isocyanato(C 1 -C 3 )alkyl)(C 3 -C 7 )cycloalkyl.

8. The aerogel of claim 7 , wherein the cross-linking agent is pyromelletic dianhydride (PMDA).

9. The aerogel of claim 1 , wherein the aerogel has the capacity to absorb at least about 20 grams of water per gram of aerogel.

10. The aerogel of claim 1 , wherein the hydrophobic agent is selected from at least one of a C 2 -C 20 alkyl silane, a C 3 -C 7 cycloalkyl silane, an aromatic silane, an (C 2 -C 20 )alkyl, a (C 3 -C 7 )cycloalkyl, an (C 2 -C 20 )alkyl urethane, a (C 3 -C 7 )cycloalkyl urethane, an (C 2 -C 20 )alkyl ester, a (C 3 -C 7 )cycloalkyl ester, an (C 2 -C 20 )alkyl carbonate, a (C 3 -C 7 )cycloalkyl carbonate or any mixture thereof.

11. The aerogel of claim 10 , wherein the hydrophobic agent is a C 5 -C 10 alkyl silane.

12. The aerogel of claim 1 , wherein the aerogel exhibits at least one of the following:

(a) a porosity equal to or greater than 90%,

(b) a maximum compressive stress of from about 50 kPa to about 400 kPa,

(c) a maximum strain of from about 15% to about 100%,

(d) a compression modulus of from about 20 kPa to about 500 kPa,

(e) a pore size average diameter of from about 20 μm to about 100 μm,

(f) a Brunauer-Emmett-Teller (BET) of from about 2 m 2 /g to about 5 m 2 /g, and

(g) a surface tension of from about 30 mN/m to about 60 mN/m.

13. The aerogel of claim 1 , wherein the aerogel adsorbs at least about 20 grams of oil per gram of aerogel.

14. The aerogel of claim 13 , wherein the aerogel adsorbs at least about 10 grams of oil per gram of aerogel after 5 cycles of adsorption and compression.

15. The aerogel of claim 13 , wherein the ratio of oil:water capable of being adsorbed per gram of aerogel is from about 1:5 to about 1:50.

16. An aerogel comprising:

a cross-linked cellulose ester, wherein the cellulose ester is cellulose acetate, cellulose acetate propionate, cellulose acetate butyrate or a combination thereof;

a cross-linking agent; and

a hydrophobic agent,

wherein the aerogel has a bulk density of from about 1 mg/cc to about 500 mg/cc, and wherein the aerogel has a BET of from about 2 m 2 /g to about 5 m 2 /g, an average diameter pore size of from about 20 um to about 100 um, or a combination thereof.

17. The aerogel of claim 16 , wherein the hydrophobic agent is selected from at least one of a C 2 -C 20 alkyl silane, a C 3 -C 7 cycloalkyl silane, an aromatic silane, an (C 2 -C 20 )alkyl, a (C 3 -C 7 )cycloalkyl, an (C 2 -C 20 )alkyl urethane, a (C 3 -C 7 )cycloalkyl urethane, an (C 2 -C 20 )alkyl ester, a (C 3 -C 7 )cycloalkyl ester, an (C 2 -C 20 )alkyl carbonate, a (C 3 -C 7 )cycloalkyl carbonate or any mixture thereof.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 23, 2021
From: TRIPATHI, ANURODH; KHAN, SAAD A.; ROJAS, ORLANDO J.; PARSONS, GREGORY N.
To: NORTH CAROLINA STATE UNIVERSITY
Reel/Frame 056642/0223 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 23, 2021
From: STEACH, JEREMY KENNETH; DE WIT, JOS SIMON; ISLAM, SM BEDARUL; GOODRICH, JACOB DONALD
To: EASTMAN CHEMICAL COMPANY
Reel/Frame 056642/0268 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 23, 2021
From: EASTMAN CHEMICAL COMPANY
To: NORTH CAROLINA STATE UNIVERSITY
Reel/Frame 056642/0298 →
Continuity (3)
Continuation 16071646
Provisional Application 62281364 · Jan 21, 2016
Related Publication 20210380725A1 · Dec 9, 2021