Method for producing exfoliated graphite-polymer composite material

Patent metadata

Field	Value
Publication number	US-9884934-B2
Application number	US-201213978875-A
Country	US
Kind code	B2
Filing date	Jan 20, 2012
Priority date	Feb 4, 2011
Publication date	Feb 6, 2018
Grant date	Feb 6, 2018

Abstract

Provided is a production method which can attain exfoliating treatment of graphite and a process of grafting a polymer onto exfoliated graphite simultaneously and thus makes it possible to easily obtain an exfoliated graphite-polymer composite material in a short time. A method for producing an exfoliated graphite-polymer composite material includes a step of mixing graphite or primary exfoliated graphite, a depolymerizable monomer of which the polymer is decomposed by heating to generate radicals and also to form a monomer or an oligomer, or the polymer A of the monomer, or a polymer B which forms radicals at a temperature close to its decomposition temperature to obtain a mixture; and a heating step of putting the mixture in a non-open container to heat the mixture to a first temperature range from the ceiling temperature or higher to the onset decomposition temperature or lower, or to a temperature higher than the first temperature range.

First claim

The invention claimed is:

1. A method for producing an exfoliated graphite-polymer composite material, the method comprising:
a step of mixing graphite or primary exfoliated graphite with a depolymerizable monomer of which the polymer is decomposed by heating to generate radicals and also to form a monomer or an oligomer, or a polymer A of the monomer, or a polymer B which generates radicals at a temperature equal to or higher than its onset decomposition temperature to obtain a mixture;
a heating step of putting said mixture in a non-open container to heat said mixture to a first temperature range or to a temperature higher than the first temperature range when a temperature range from a ceiling temperature of said polymer A or B or higher to an onset decomposition temperature or lower of said polymer A or B defined as the first temperature range, and heating the mixture to a second temperature range exceeding the onset decomposition temperature but not exceeding a decomposition-completion temperature when a temperature at which 10% by weight of said polymer A or B is decomposed is defined as the onset decomposition temperature and a temperature at which 90% by weight of said polymer A or B is decomposed is defined as the decomposition-completion temperature, and
a step of repeating a step of heating the mixture to said first temperature range and a step of heating the mixture to said second temperature range.

2. A method for producing an exfoliated graphite-polymer composite material, the method comprising:
a step of mixing graphite or primary exfoliated graphite with a depolymerizable monomer of which the polymer is decomposed by heating to generate radicals and also to form a monomer or an oligomer, or a polymer A of the monomer, or a polymer B which generates radicals at a temperature equal to or higher than its onset decomposition temperature to obtain a mixture;
a heating step of putting said mixture in a non-open container to heat said mixture to a first temperature range or to a temperature higher than the first temperature range when a temperature range from a ceiling temperature of said polymer A or B or higher to an onset decomposition temperature or lower of said polymer A or B is defined as the first temperature range, and heating the mixture to a second temperature range exceeding the onset decomposition temperature but not exceeding a &composition-completion temperature when a temperature at which 10% by weight of said polymer A or B is decomposed is defined as the onset decomposition temperature and a temperature at which 90% by weight of said polymer A or B is decomposed is defined as the decomposition-completion temperature; and
a heating step of heating the mixture to a third temperature range higher than the decomposition-completion temperature,
wherein the heating step of heating die mixture to said second temperature range and the heating step of heating the mixture to said third temperature range are repeated.

3. The method for producing an exfoliated graphite-polymer composite material according to claim 1 , wherein the onset decomposition temperature is a temperature at which the equation, (X−R)/(A 0 −R)=0.9, is satisfied, and the decomposition-completion temperature is a temperature at which the equation, (Y−R)/(A 0 −R)=0.1, is satisfied, when the weight of a decomposed residue at a temperature higher than the decomposition-completion temperature of said polymer A or B and at a temperature of 1000° C. or lower is R, the maximum weight of the polymer A or B in the first temperature range is A 0 , the weight of the polymer A or B at the onset decomposition temperature is X, and the weight of the polymer A or B at the decomposition-completion temperature is Y.

4. The method for producing an exfoliated graphite-polymer composite material according to claim 1 , wherein two or more types of monomers or polymers are used as said monomer or polymer A or B.

5. A method for producing an exfoliated graphite-polymer composite material, the method comprising:
a step consisting of mixing graphite or primary exfoliated graphite with a depolymerizable monomer of which the polymer is decomposed by heating to generate radicals and also to form a monomer or an oligomer, or a polymer A of the monomer, or a polymer B which generates radicals at a temperature equal to or higher than its onset decomposition temperature to obtain a mixture;
a step consisting of putting said mixture into a container and closing the container with only the mixture therein; and
a heating step of heating said mixture in the closed container to a first temperature range or to a temperature higher than the first temperature range to obtain exfoliated graphite by delamination of the graphite or primary exfoliated graphite and graft the polymer A or polymer B to the exfoliated graphite when a temperature range from a ceiling temperature of said polymer A or B or higher to an onset decomposition temperature or lower of said polymer A or B is defined as the first temperature range.

6. The method for producing an exfoliated graphite-polymer composite material according to claim 1 , wherein said mixture does not contain a polymerization initiator.

7. An exfoliated graphite-polymer composite material obtained by the method for producing an exfoliated graphite-polymer composite material as claimed in claim 1 , the composite material having an X-ray diffraction peak intensity of 50% or less of the X-ray diffraction peak intensity derived from the untreated graphite layer crystal at 26.4 degree.

8. The method for producing an exfoliated graphite-polymer composite material according to claim 2 , wherein the onset decomposition temperature is a temperature at which the equation, (X−R)/(A 0 −R)=0.9, is satisfied, and the decomposition-completion temperature is a temperature at which the equation, (Y−R)/(A 0 −R)=0.1, is satisfied, when the weight of a decomposed residue at a temperature higher than the decomposition-completion temperature of said polymer A or B and at a temperature of 1000° C. or lower is R, the maximum weight of the polymer A or B in the first temperature range is A 0 , the weight of the polymer A or B at the onset decomposition temperature is X, and the weight of the polymer A or B at the decomposition-completion temperature is Y.

9. The method for producing an exfoliated graphite-polymer composite material according to claim 2 , wherein two or more types of monomers or polymers are used as said monomer or polymer A or B.

10. The method for producing an exfoliated graphite-polymer composite material according to claim 2 , wherein said mixture does not contain a polymerization initiator.

Assignees

• Nakasuga Akira
• Nozato Shouji
• Wada Takuya
• Yoshitani Hiroshi
• Sekisui Chemical Co Ltd

Inventors

• Nakasuga Akira
• Nozato Shouji
• Wada Takuya
• Yoshitani Hiroshi

Classifications

• C08F292/00 Primary

  Macromolecular compounds obtained by polymerising monomers on to inorganic materials · CPC title

• C08F8/50

  Partial depolymerisation · CPC title

• C01B32/225

  Expansion; Exfoliation · CPC title

• C08K3/04

  Carbon · CPC title

• C08F2/44

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