Polyimide composite, a method of preparing thereof, and application thereof

Patent metadata

Field	Value
Publication number	US-11667759-B2
Application number	US-202016772597-A
Country	US
Kind code	B2
Filing date	Mar 31, 2020
Priority date	Dec 30, 2019
Publication date	Jun 6, 2023
Grant date	Jun 6, 2023

Abstract

A polyimide composite, a method of preparing thereof, and an application thereof are provided. A general structure of the polyimide composite is: SiO 2 -(β-CD-Ada) x /PI, and x is 3 to 5. The polyimide composite has the functions of self-repairing and anti-aging.

First claim

What is claimed is:

1. A polyimide composite, comprising: a polyimide resin and an assembly body distributed in the polyimide resin, wherein the polyimide resin is a polycondensate of an aromatic diamine and an aromatic dianhydride; the assembly body is made of β-cyclodextrin grafted SiO 2 and reacted with adamantane by an inclusion reaction; and the polyimide composite has a structural formula as follows:
SiO 2 -(β-CD-Ada) x /PI, wherein x is 3 to 5.

2. A method of preparing the polyimide composite according to claim 1 , comprising the following steps:
(1) performing a graft reaction between SiO 2 and β-cyclodextrin, wherein a product is SiO 2 -(β-CD) x , and x is 3 to 5;
(2) performing an inclusion reaction between the SiO 2 -(β-CD) x and adamantane, wherein a product is SiO 2 -(β-CD-Ada) x , and x is 3 to 5;
(3) performing a polycondensation reaction, wherein diamine compound, dianhydride compound, and sodium amantadine are reacted through the polycondensation reaction, and a product is PAA; and
(4) performing a grafting reaction and a cyclization reaction, wherein the PAA and the SiO 2 -(β-CD-Ada) x are reacted through the grafting reaction and the cyclization reaction in order to form the polyimide composite, and the polyimide composite is SiO 2 -(β-CD-Ada) x /PI, and x is 3 to 5.

3. The method of preparing the polyimide composite according to claim 2 , wherein the β-cyclodextrin is fully dissolved in a NaOH solution in the step (1), then epichlorohydrin is added, and nano-sized SiO 2 is slowly added at a stirring speed of 500 to 800 rpm, a grafting reaction is performed at 60° C., the grafting reaction is finished when viscosity occurs, then the solvent is removed by suspension distillation, a obtained dry solid is SiO 2 -(β-CD) x , and a molar ratio of SiO 2 to β-cyclodextrin is (0.25-5.0):1.

4. The method of preparing the polyimide composite according to claim 2 , wherein the SiO 2 -(β-CD) x and the adamantane are mixed in a molar ratio of (2-5):(1-3) in the step (2), and stirred for 24 to 96 hours under normal temperature conditions.

5. The method of preparing the polyimide composite according to claim 2 , wherein a structural formula of the diamine compound in the step (3) is NH 2 —Ar—NH 2 , and the Ar is selected from one of

6. The method of preparing the polyimide composite according to claim 2 , wherein a structural formula of the dianhydride compound in the step (3) is

7. The method of preparing the polyimide composite according to claim 2 , wherein the diamine compound, the dianhydride compound and the sodium adamantane are mixed in a molar ratio of (1.05-2): 1: (1.1-9.9) and dissolved in a solvent at 80° C. for 6 to 10 hours in the step (3), and the solvent is one of N-methylpyrrolidone, N, N-dimethylformamide, and toluene.

8. The method of preparing the polyimide composite according to claim 2 , wherein the PAA and the SiO 2 -(β-CD-Ada) x are mixed in a mass ratio of (5-15):(85-95) in the step (4) and stirred at 0° C. for 24 to 96 hours, and then temperature is raised to 80° C. and a reaction is performed for 5 to 18 hours; and
wherein the cyclization reaction in the step (4) comprises coating a graft reaction product on a glass substrate, baking and removing a solvent at 120° C., and then stepwise heating to 450° C., and then baking at a constant temperature for 0.8 to 1.2 hours to obtain the polyimide composite.

9. The method of preparing the polyimide composite according to claim 8 , wherein a rate of stepwise heating is 4-8° C./min.

10. A method of forming a self-preparing coating, comprising coating the polyimide composite according to claim 1 on a surface of base material for coating.

Assignees

• Wuhan China Star Optoelectronics Semiconductor Display Tech Co Ltd

Inventors

• Wang Yamin

Classifications

• C08G83/008 Primary

  Supramolecular polymers · CPC title

• C08L2201/08

  Stabilised against heat, light or radiation or oxydation · CPC title

• C08G83/001 Primary

  Macromolecular compounds containing organic and inorganic sequences, e.g. organic polymers grafted onto silica · CPC title

• C08B37/0015

  Inclusion compounds, i.e. host-guest compounds, e.g. polyrotaxanes · CPC title

• C08G2150/90

  Compositions for anticorrosive coatings · CPC title