Graphene reinforced polyethylene terephthalate

Patent metadata

Field	Value
Publication number	US-9890263-B2
Application number	US-201615177541-A
Country	US
Kind code	B2
Filing date	Jun 9, 2016
Priority date	Jul 8, 2015
Publication date	Feb 13, 2018
Grant date	Feb 13, 2018

Abstract

A composition and a method are provided for graphene reinforced polyethylene terephthalate (PET). Graphene nanoplatelets comprising a suitable initial surface area are added to a solvent for producing PET. In some embodiments, the solvent comprises ethylene glycol. The solvent and graphene nanoplatelets are sonicated to disperse the nanoplatelets within the solvent. The solvent and graphene nanoplatelets are centrifuged to remove nanoplatelet agglomerates within the solvent. A supernatant solution of dispersed graphene nanoplatelets and solvent is decanted and then used for in-situ polymerization of the graphene reinforced PET comprising a continuous matrix of PET with a dispersed graphene reinforcement phase. The graphene reinforcements comprise a minimal number of layers of two-dimensional mono-atomic carbon sheets. In some embodiments, the number of layers ranges between 1 layer and 7 layers. The graphene reinforced PET preferably comprises a concentration of graphene nanoplatelets being less than substantially 2% weight fraction of the graphene reinforced PET.

First claim

What is claimed is:

1. A method for preparing graphene reinforced polyethylene terephthalate (PET), comprising:
obtaining graphene nanoplatelets;

adding the graphene nanoplatelets to a solvent comprising ethylene glycol suitable for producing PET;
sonicating the solvent and graphene nanoplatelets so as to cause a homogeneous dispersion of the graphene nanoplatelets within the solvent;
centrifuging the solvent and graphene nanoplatelets to remove larger graphene nanoplatelets that are not suitably dispersed within the solvent;
decanting a supernatant solution of graphene nanoplatelets dispersed in the solvent;
using the supernatant solution for in-situ polymerization of the graphene reinforced PET, wherein using the supernatant solution for in-situ polymerization further comprises performing an ester interchange reaction to produce a PET monomer, followed by performing a polycondensation reaction so as to produce a PET polymer chain; and
wherein performing the ester interchange reaction comprises charging the solution of graphene nanoplatelets dispersed in the solvent and powdered dimethyl terephthalate (DMT) into a reactor under nitrogen purge at a molar ratio of 2.3:1 with an excess of ethylene glycol.

2. The method of claim 1 , wherein sonicating comprises immersing the solvent and graphene nanoplatelets in a bath sonicator for a period of time and operating the bath sonicator at a frequency suitable for dispersing the graphene nanoplatelets within the solvent.

3. The method of claim 2 , wherein sonicating comprises selecting the period of time so as to desirably reduce a number of layers comprising the graphene nanoplatelets.

4. The method of claim 2 , wherein the frequency is an ultrasonic and the period of time ranges between at least 24 hours and 96 hours.

5. The method of claim 1 , wherein centrifuging comprises subjecting the solvent and graphene nanoplatelets to a rotational speed of centrifugation ranging between at least 1500 RPM and 4500 RPM.

6. The method of claim 1 , wherein performing the ester interchange reaction further comprises including a catalyst comprising manganese acetate (Mn(CH 3 COO) 2 ) at a concentration of 82 parts-per-million (ppm).

7. The method of claim 1 , wherein performing the polycondensation reaction further comprises including a catalyst comprising antimony trioxide (Sb 2 O 3 ) at a concentration of 300 ppm.

8. The method of claim 1 , wherein performing the polycondensation reaction further comprises adding a suitable concentration of isophthalic acid (C 6 H 4 (COH) 2 ) so as to limit the crystallinity of PET.

9. The method of claim 1 , wherein performing the polycondensation reaction further comprises adding stabilized cobalt at a concentration of 65 ppm so as to control a final color of the PET.

10. The method of claim 1 , wherein the graphene nanoplatelets comprise a surface area of 750 m 2 /g.

11. The method of claim 1 , wherein the graphene reinforced polyethylene terephthalate comprises a concentration of graphene nanoplatelets being less than substantially 2% weight fraction of the graphene reinforced polyethylene terephthalate.

Assignees

• Niagara Bottling Llc

Inventors

• Hanan Jay Clarke
• Shabafrooz Vahid
• Bandla Sudheer

Classifications

• C08L67/02

  Polyesters derived from dicarboxylic acids and dihydroxy compounds (C08L67/06 takes precedence) · CPC title

• C08K2201/011

  Nanostructured additives · CPC title

• C08K3/042 Primary

  Graphene or derivatives, e.g. graphene oxides · CPC title

• C08G63/866

  Antimony or compounds thereof · CPC title

• C08G63/83

  Alkali metals, alkaline earth metals, beryllium, magnesium, copper, silver, gold, zinc, cadmium, mercury, manganese, or compounds thereof {(C08G63/823 takes precedence)} · CPC title