IP Library Granted Patent US 9,790,334
Granted Patent B2
US 9,790,334 · App. 14/776,022 · Granted Oct 17, 2017

Polymer-graphene nanocomposites

Inventors: Allen David Clauss (Madison, WI); Guiquan Pan (Middleton, WI); Nicholas Richard Wietfeldt (Madison, WI); Matthew Clayton Hall (Madison, WI); David D. Taft (Traverse City, MI)
Assignee: RELIANCE INDUSTRIES LIMITED
C08J3/226B82Y30/00C08J3/2053C08J5/005C08K3/04C08L39/06C08L77/06C08J2323/06C08J2323/12C08J2339/06C08J2363/00C08J2377/06C08K2201/011
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Quick Facts
Patent No.
US 9,790,334
App. No.
14/776,022
Granted
Oct 17, 2017
Kind
B2
Abstract

Provided herein is technology relating to polymer-graphene nanocomposites and particularly, but not exclusively, to methods for producing polymer-graphene nanocomposites using master batches comprising graphene and a polymer or polymer precursor. The resulting polymer-graphene nanocomposites comprise a high degree of exfoliation and dispersion of graphene nanoplatelets within the polymer matrix.

Claims (25)

1. A master batch composition for making a polymer nanocomposite, the master batch composition comprising a polymer, wherein the polymer is a poly(vinyl lactam), a polyacrylamide, a thermoplastic polymer, thermoset polymer, polyethylene polymer, polypropylene polymer, polycarbonate polymer, unsaturated polyester, polyvinylchloride, or epoxy vinyl ester, or epoxy and at least 20% by weight exfoliated graphene.

2. The master batch composition of claim 1 comprising graphene and a poly(vinylpyrrolidone) in a weight ratio of 1:1 to 1:4.

3. The master batch composition of claim 1 comprising graphene and a thermoplastic polymer in a weight ratio of 1:1 to 1:4.

4. The master batch composition of claim 1 wherein the average thickness of the graphene is less than 10 atomic layers, a minimum of 5% of the graphene is single atomic layer graphene, and the oxygen content of the graphene is less than 1%.

5. The master batch composition of claim 1 wherein less than 10% of the graphene nanoplatelets have a maximum diameter of less than 0.5 microns.

6. The master batch composition of claim 1 comprising a poly(vinylpyrrolidone) that has a number average molecular weight of less than or equal to approximately 10,000 u.

7. A method of making a master batch composition for producing a polymer nanocomposite, the method comprising:

a) mixing a slurry of graphene, wherein the slurry of graphene is produced by:

i) treating graphite in an N-alkyl-pyrrolidone to produce solvent exfoliated graphene in the N-alkyl-pyrrolidone;

ii) removing most of the N-alkyl-pyrrolidone to produce a concentrated solution or dispersion of graphene in the N-alkyl-pyrrolidone; and

iii) adding a solvent to the graphene in N-alkyl-pyrrolidone to produce the slurry of graphene in the solvent system in a solvent system with a polymer; and

b) removing the solvent system to produce a master batch comprising from 20% to 60% exfoliated graphene.

8. The method of claim 7 wherein the mixing is high shear mixing.

9. The method of claim 7 wherein the polymer is a polyvinyl lactam or a thermoplastic polymer.

10. The method of claim 7 wherein the solvent is xylenes or methanol.

11. The method of claim 7 wherein the concentrated solution or dispersion of graphene in the N-alkyl-pyrrolidone comprises 2% to 8% graphene.

12. The method of claim 7 comprising filtration to remove the N-alkyl-pyrrolidone.

13. The method of claim 7 wherein the solvent system comprises 2% to 30% N-alkyl-pyrrolidone and 70% to 98% solvent.

14. A method of making a graphene/thermoplastic master batch consisting of the steps:

a) concentrating a solution or stable dispersion of exfoliated graphene above the solubility and stable dispersion limit of the exfoliated graphene;

b) dissolving a thermoplastic polymer in the graphene/solvent slurry in a ratio of 1:1 to 1:5 graphene to polymer; and

c) removing the solvent with continuous mixing to isolate the resultant graphene/polymer master batch as a solid.

15. A method of making a graphene/polymer master batch, the method comprising:

a) exfoliating graphene in a polymerizable solvent, wherein the polymerizable solvent is N-vinyl pyrrolidone or N,N-dimethyl acrylamide to provide a dispersion of exfoliated graphene in the polymerizable solvent;

b) polymerizing the polymerizable solvent to produce a graphene/polymer master batch.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 11, 2016
From: XOLVE, INC.
To: RELIANCE INDUSTRIES LIMITED
Reel/Frame 037762/0687 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 14, 2015
From: CLAUSS, ALLEN DAVID; PAN, GUIQUAN; WIETFELDT, NICHOLAS RICHARD; HALL, MATTHEW CLAYTON; TAFT, DAVID D.
To: XOLVE, INC.
Reel/Frame 036558/0899 →
Continuity (2)
Provisional Application 61787407 · Mar 15, 2013
Related Publication 20160032061A1 · Feb 4, 2016