Composition containing graphene and graphene nanoplatelets and preparation process thereof

Patent metadata

Field	Value
Publication number	US-12534586-B2
Application number	US-202318520592-A
Country	US
Kind code	B2
Filing date	Nov 28, 2023
Priority date	Jan 27, 2016
Publication date	Jan 27, 2026
Grant date	Jan 27, 2026

Abstract

A process for preparing a composition from graphite material by contacting the graphite material with a main solvent comprising at least 10% by weight, with respect to a total weight of the main solvent, of a vinyl aromatic monomer alone or in a mixture up to 50% by weight with additional copolymerizable monomers, thereby forming a starting composition; subjecting to an ultrasound treatment with a frequency spectrum ranging between 18 kHz and 1000 kHz, at a pressure equal to or higher than 2 bar absolute and in a container or sonication chamber wherein no separated phase of fluid at the gaseous phase contacts said composition; and polymerizing at least 1% of the vinyl aromatic monomer present in the main solvent, wherein the composition is at least partially polymerized and contains graphene and graphene nanoplatelets durably dispersed in the solvent, and the composition is without any evident formations of deposits or separated phases for at least 30 days.

First claim

The invention claimed is:

1 . A process for preparing a composition from graphite material, comprising:
combining a graphite and a styrene monomer to form a mixture; subjecting the mixture to ultrasound treatment to exfoliate the graphite to graphene and graphene nanoplatelets, and to simultaneously polymerize the styrene monomer to form a polystyrene, and decanting and/or separating by centrifugation the produced mixture comprising the polystyrene, the exfoliated graphene, unpolymerized styrene and non-exfoliated graphite to remove graphite not completely exfoliated, wherein the ultrasound treatment is conducted at a frequency spectrum ranging from 18 kHz to 20 KHz and an ultrasound power of 60 to 110 W/cm 3 in a degassed environment at a pressure of from 12 to 25 bar absolute and at a temperature ranging from 20° C. to 200° C. for 0.5 seconds to 5 minutes; and wherein the graphene and the graphene nanoplatelets have an average thickness higher than or equal to the thickness of a single graphene layer up to 50 nm, the thickness being measured on samples of graphene and graphene nanoplatelets deposited on a silicon wafer coated with silicon oxide, with intermittent contact atomic force microscopy, called AFM tapping mode, said composition comprising:
a solvent having an interfacial tension different from that of graphite material and comprising 10 to 70% by weight of the polystyrene and 20 to 80% by weight of the styrene monomer, and
the graphene and the graphene nanoplatelets (GRS) stably dispersed without any evident formations of deposits or separated phases for at least 30 days in the solvent in a mass concentration of 0.05 to 5% by weight.

2 . The process according to claim 1 , wherein said combining the graphite and the styrene monomer and subjecting the mixture to ultrasound treatment are carried out simultaneously or sequentially.

3 . The process according to claim 1 , wherein said combining the graphite and the styrene monomer and subjecting the mixture to ultrasound treatment are carried out according to a continuous mode or according to a discontinuous mode.

4 . The process according to claim 1 , wherein, the produced mixture is decanted and is further subjected to centrifugation in order to separate any remaining not-exfoliated graphite material.

5 . The process according to claim 1 , wherein, the produced mixture is decanted, and after the decanting, polymerization of the styrene is completed, thereby forming polystyrene composites, polystyrene nano-composites or a polystyrene master batch containing the graphene and the graphene nanoplatelets.

6 . The process according to claim 1 , wherein the composition containing the graphene and the graphene nanoplatelets stably dispersed in the solvent is partially or completely polymerized directly during the ultrasound treatment.

7 . The process according to claim 1 , wherein the styrene, optionally comprises further polymerizable co-monomers.

8 . The process according to claim 1 , wherein a non-graphitic carbon is present in addition to the graphite material.

9 . The process according to claim 8 , wherein the non-graphitic carbon is selected from the group consisting of coke, carbon black, and graphitized coke.

10 . The process according claim 1 , wherein the graphite material is selected from the group consisting of synthetic graphite, natural graphite, expanded graphite, highly ordered pyrolytic graphite, vein graphite, and intercalated graphite.

11 . The process according to claim 1 , wherein a secondary solvent different from the styrene is added during the ultrasound treatment.

12 . The process according to claim 1 , wherein the pressure is kept stable by a direct expansion tank or by an indirect expansion tank.

13 . The process according to claim 1 , wherein the ultrasounds are transmitted according to a direct mode; or according to an indirect mode; or in pulses, alternating active periods wherein the starting composition is subjected to ultrasounds, and passive periods in which said composition is not subjected to ultrasounds or is subjected to ultrasounds of power at least 10 times lower than the transmission power during the active period, and a ratio between the active period and the sum of the active and passive periods ranging between 0.0001 and 1.

Assignees

• Versalis Spa

Inventors

• Felisari Riccardo
• Autieri Viviana

Classifications

• C08K2201/016

  Additives defined by their aspect ratio · CPC title

• C08K2201/011

  Nanostructured additives · CPC title

• C08K3/04

  Carbon · CPC title

• C08F2/44

  Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers · CPC title

• C08F12/08

  Styrene · CPC title