IP Library Granted Patent US 10,589,216
Granted Patent B2
US 10,589,216 · App. 15/526,908 · Granted Mar 17, 2020

Membranes for fluid separation

Inventors: Prabir Kumar Dutta (Worthington, OH); Yanzuo Li (Columbus, OH); Bo Wang (Columbus, OH)
Assignee: Ohio State Innovation Foundation
B01D53/228B01D69/10B01D71/028B01D2053/221B01D2256/22B01D2257/404B01D2257/504C01B39/04C01B39/205C01B39/40
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Quick Facts
Patent No.
US 10,589,216
App. No.
15/526,908
Granted
Mar 17, 2020
Kind
B2
Abstract

Membranes, methods of making the membranes, and methods of using the membranes are described herein. The membranes can comprise a gas permeable support and a continuous phase comprising a selective inorganic material disposed within the gas permeable support. In some embodiments, the membranes can exhibit a CO 2 :N 2 selectivity of at least 10 at 24° C. The membranes can be bendable, such that when the membranes are wrapped around a 1.5-inch diameter cylinder and returned to a planar conformation, the CO 2 :N 2 selectivity of the membranes is at least 25% of the CO 2 :N 2 selectivity of the membranes prior to having been wrapped around the cylinder.

Claims (44)

1. A method of making alumino-silicate nanoparticles comprising:

(a) heating a first mixture comprising a silicon source, an aluminum source, a base, an organic agent, and a first solvent to produce a first population of alumino-silicate nanoparticles dispersed in a first supernatant;

(b) separating the first population of inorganic nanoparticles from the first supernatant;

(c) adding a base to the first supernatant to form a second mixture;

(d) heating the second mixture to produce a second population of alumino-silicate nanoparticles dispersed in a second supernatant; and

(e) separating the second population of inorganic nanoparticles from the second supernatant;

wherein the method comprises repeating steps (c) and (d) prior to performing step (e); and

wherein the first population of alumino-silicate nanoparticles and the second population of alumino-silicate nanoparticles each have an average particle size of 100 nm or less.

2. The method of claim 1 , wherein step (d) further comprises concentrating the second supernatant to form a concentrated supernatant, and diluting the concentrated supernatant the reform the second supernatant.

3. The method of claim 2 wherein step (d) further comprises concentrating the second supernatant to form a concentrated supernatant, heating the concentrated supernatant, and diluting the concentrated supernatant the reform the second supernatant.

4. The method of claim 1 , wherein steps (c) and (d) are repeated at least 5 times prior to performing step (e).

5. The method of claim 1 , wherein steps (c) and (d) are repeated until the yield of the second population of alumino-silicate nanoparticles is at least 75%.

6. The method of claim 2 , wherein concentrating the second supernatant comprises removing a portion of the first solvent.

7. The method of claim 6 , wherein the portion of first solvent removed is from 20% to 70% by volume of the second supernatant.

8. The method of claim 2 , wherein diluting the concentrated supernatant comprises adding a second solvent to the concentrated supernatant.

9. The method of claim 8 , wherein the second solvent added to the concentrated supernatant is from 20% to 70% by volume of the second supernatant.

10. The method of claim 8 , wherein the second solvent comprises water.

11. The method of claim 8 , wherein the second solvent further comprises a base.

12. The method of claim 1 , wherein the first solvent comprises water.

13. The method of claim 1 , wherein the silicon source comprises tetraethylorthosilane, colloidal silica, disodium metasilicate, or combinations thereof.

14. The method of claim 1 , wherein the base is selected from sodium hydroxide, potassium hydroxide, and combinations thereof.

15. The method of claim 1 , wherein the organic agent comprises tetrapropyl ammonium hydroxide, tetramethyl ammonium hydroxide, tetramethyl ammonium bromide, tetrapropyl ammonium bromide, or combinations thereof.

16. The method of claim 1 , wherein the aluminum source comprises aluminum isopropoxide, sodium aluminate, aluminum sulfate, or combinations thereof.

17. The method of claim 1 , wherein the heating is carried out at from 80-150° C.

18. The method of claim 1 , wherein the heating comprises irradiating the mixture with microwave radiation.

19. The method of claim 1 , wherein the alumino-silicate nanoparticles comprise zeolite nanoparticles.

20. The method of claim 1 , wherein the alumino-silicate nanoparticles comprise a crystalline alumino-silicate nanoparticle.

21. The method of claim 1 , wherein the alumino-silicate nanoparticles comprise zeolites having a faujasite structure.

22. A method of making alumino-silicate nanoparticles comprising:

(a) heating a first mixture comprising a silicon source, an aluminum source, a base, an organic agent, and a first solvent to produce a first population of alumino-silicate nanoparticles dispersed in a first supernatant;

(b) separating the first population of inorganic nanoparticles from the first supernatant;

(c) adding a base to the first supernatant to form a second mixture;

(d) heating the second mixture to produce a second population of alumino-silicate nanoparticles dispersed in a second supernatant; and

(e) separating the second population of inorganic nanoparticles from the second supernatant;

wherein step (d) further comprises concentrating the second supernatant to form a concentrated supernatant, and diluting the concentrated supernatant the reform the second supernatant; and

wherein the first population of alumino-silicate nanoparticles and the second population of alumino-silicate nanoparticles each have an average particle size of 100 nm or less.

23. A method of making alumino-silicate nanoparticles comprising:

(a) heating a first mixture comprising a silicon source, an aluminum source, a base, an organic agent, and a first solvent to produce a first population of alumino-silicate nanoparticles dispersed in a first supernatant;

(b) separating the first population of inorganic nanoparticles from the first supernatant;

(c) adding a base to the first supernatant to form a second mixture;

(d) heating the second mixture to produce a second population of alumino-silicate nanoparticles dispersed in a second supernatant; and

(e) separating the second population of inorganic nanoparticles from the second supernatant;

wherein the alumino-silicate nanoparticles comprise zeolites having a faujasite structure; and

wherein the first population of alumino-silicate nanoparticles and the second population of alumino-silicate nanoparticles each have an average particle size of 100 nm or less.

Assignments (2)
CONFIRMATORY LICENSE Recorded Jul 10, 2018
From: OHIO STATE UNIVERSITY
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 046514/0990 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 15, 2017
From: DUTTA, PRABIR KUMAR; LI, YANZUO; WANG, BO
To: OHIO STATE INNOVATION FOUNDATION
Reel/Frame 042722/0937 →
Continuity (2)
Provisional Application 62079421 · Nov 13, 2014
Related Publication 20170341017A1 · Nov 30, 2017