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Polyimide/rod-like clay nano-composite film and preparation method thereof

A rod-shaped clay and polyimide technology, which is applied in the field of polyimide/rod-shaped clay nanocomposite film and its preparation, can solve the problems of affecting the strength of the composite film, limited clay dispersion ability, complicated preparation process, etc., and achieve excellent thermal Stability, prevention of agglomeration, and good transparency

Inactive Publication Date: 2009-09-30
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A variety of polyimide / clay nanocomposites have been involved in the above studies, but the clays used are mostly discoid or layered clays such as bentonite. The disadvantage is that complex surface treatment is required before compounding with polyimide. Such as ion exchange, coupling agent treatment and organic grafting, etc., the preparation process is complicated, the development cost is high, and the dispersion ability of this kind of clay in polyimide is very limited, which affects the strength of the composite film to a certain extent
So far, there is no report on the preparation of polyimide / (without surface treatment) rod-shaped clay nanocomposite film by in-situ polymerization

Method used

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  • Polyimide/rod-like clay nano-composite film and preparation method thereof
  • Polyimide/rod-like clay nano-composite film and preparation method thereof
  • Polyimide/rod-like clay nano-composite film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Add 158g of sepiolite to 30ml of N,N-dimethylacetamide, and ultrasonically disperse it under stable mechanical stirring for 3 hours, then add 1.50g of 4,4'-diaminodiphenyl ether, and wait for 4,4 After '-diaminodiphenyl ether was completely dissolved, 1.65 g of pyromellitic dianhydride was added, and the polymerization reaction was mechanically stirred at 15° C. for 2 hours to obtain a polyamic acid (10% solid content) / sepiolite mixed solution;

[0027] 2) Put the mixed solution to stand for defoaming, pour it on a glass plate to scrape and coat it to form a film, and dry it in an oven at 50°C for 10 hours, then transfer it to a curing oven for thermal imidization. The heating program is: from room temperature Raise the temperature to 135°C within 1 hour and keep the temperature for 2 hours, then raise the temperature to 300°C within 2 hours and keep the temperature for 3 hours, cool to room temperature, peel the film from the glass plate to obtain (4,4'-ODA-PMDA) pol...

Embodiment 2

[0028] 1) Add 0.252g of sepiolite to 30ml of N,N-dimethylacetamide, and ultrasonically disperse it under stable mechanical stirring for 3 hours, then add 1.50g of 4,4'-diaminodiphenyl ether, and in 15 ℃ mechanically stirred and polymerized for 2 hours to obtain a polyamic acid (10% solid content) / sepiolite mixed solution;

[0029] 2) method of operation is the same as step 1 in embodiment 1), obtains (4,4 '-ODA-PMDA) polyimide / sepiolite (8%) nanocomposite film

Embodiment 3

[0031] 1) Add 0.378g of sepiolite to 30ml of N,N-dimethylacetamide, and ultrasonically disperse it under stable mechanical stirring for 3 hours, then add 1.50g of 4,4'-diaminodiphenyl ether, wait for 4, After 4'-diaminodiphenyl ether was completely dissolved, 1.65g of pyromellitic dianhydride was added, and the polymerization reaction was mechanically stirred at 15°C for 2 hours to obtain a polyamic acid (10% solid content) / sepiolite mixed solution, After static defoaming;

[0032] 2) The operation method is the same as step 1) in Example 1 to obtain (4,4'-ODA-PMDA) polyimide / sepiolite (12%) nanocomposite film.

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Abstract

The invention provides a polyimide / rod-like clay nano-composite film and a preparation method thereof, which belong to the field of polymer materials. The composite film provided by the invention takes polyimide as a matrix and takes rod-like clay as a disperse phase, wherein the mass fraction of the polyimide matrix is 70 to 99.9 percent; the mass fraction of the rod-like clay is 0.1 to 30 percent; and the rod-like clay is sepiolite, attapulgite or a mixture of the two in arbitrary mixture ratio. The preparation method obtains the polyimide / rod-like clay nano-composite film by dispersing the rod-like clay in an organic solvent, adding diamine and dianhydride to the organic solvent, mechanically stirring the organic solvent for 1 to 3 hours at a temperature of between 0 and 30 DEG C, obtaining a polyimide / rod-like clay mixed solution, smearing a glass plate with the mixed solution to form a film, volatilizing the solvent and performing hot imidization. The preparation method is simple. The obtained composite film has the advantages of excellent mechanical properties, dimension stability, good thermal stability, chemical stability and the like.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a polyimide / rod-shaped clay nanocomposite film with low linear expansion coefficient, high strength and high modulus and a preparation method thereof. Background technique [0002] Polyimide film (PI) is an excellent high and low temperature resistant material with excellent mechanical properties, dielectric properties, corrosion resistance and radiation resistance, so it is widely used in machinery, electronics, aerospace, national defense construction , new energy and environmental industries and many other fields. However, its high thermal expansion limits its application in flexible printed circuit boards, electrical insulating varnishes, buffer materials, and interlayer packaging materials. In practical applications, polyimide films are usually combined with inorganic materials such as metals to form organic / inorganic heterogeneous composite materials, thereby r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08K7/10C08G73/10C08J5/18
Inventor 武德珍余韵吴战鹏齐胜利
Owner BEIJING UNIV OF CHEM TECH
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