Preparation method of polymer film containing nano fullerene

A nano-fullerene and fullerene technology, which is applied in the field of material doping and modification, can solve the problems of affecting the heat resistance of polymer materials, lowering the thermal decomposition temperature, and not having universal applicability, so as to achieve good storage stability , Inhibit viscosity decrease, improve storage stability

Active Publication Date: 2021-06-01
北京市科学技术研究院分析测试研究所(北京市理化分析测试中心)
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the harsh anaerobic dry low-temperature environment cannot be applied to more scenes with water and oxygen at room temperature or even higher temperature. Molecular additives affect the heat resistance of polymer materials, especially the thermal decomposition temperature will be greatly reduced

Method used

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  • Preparation method of polymer film containing nano fullerene
  • Preparation method of polymer film containing nano fullerene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 polyimide / fullerene hybrid film PI / AC 60 -0.5%

[0028] Step (1): In a three-neck flask equipped with mechanical stirring, nitrogen inlet and outlet, and a thermometer, add 10.81 grams (0.10 moles) of p-phenylenediamine (p-PDA) and 160 grams of N-methyl-2-pyrrolidone, Stir under nitrogen protection until completely dissolved; add 29.42 grams (0.10 moles) of 3,3',4,4'-biphenyltetracarboxylic dianhydride (s-BPDA), stir until completely dissolved, and react at 20°C After 12 hours, a polyamic acid solution with a solid content of about 20 wt % was obtained.

[0029] Step (2): Weigh 0.18 g of methyl carbamate-modified C60 fullerene, add it into the above polyamic acid solution, and stir rapidly until the mixture is uniform.

[0030] Step (3): After filtering the above-mentioned polyamic acid / fullerene precursor solution and vacuum defoaming, it is coated on a glass plate or a stainless steel plate with a flat surface. Under nitrogen atmosphere, bake at 80°C f...

Embodiment 2

[0031] Embodiment 2 polyimide / fullerene hybrid film PI / AC 60 -1.0%

[0032] Step (1): In a three-necked flask equipped with mechanical stirring, nitrogen inlet and outlet, and a thermometer, add 10.81 grams (0.10 moles) of p-phenylenediamine (p-PDA) and 230 grams of N,N-diethylacetamide , stirred under nitrogen protection until completely dissolved; added 29.42 g (0.10 moles) of 3,3',4,4'-biphenyltetracarboxylic dianhydride (s-BPDA), stirred until completely dissolved, at 25°C React for 16 hours to obtain a polyamic acid solution with a solid content of about 15 wt%.

[0033] Step (2): Weigh 0.36 g of methyl carbamate-modified C60 fullerene, add it into the polyamic acid solution, and stir rapidly until the mixture is uniform.

[0034] Step (3): After filtering the above-mentioned polyamic acid / fullerene precursor solution and vacuum defoaming, it is coated on a glass plate or a stainless steel plate with a flat surface. Under nitrogen atmosphere, bake at 60°C for 2 hours, ...

Embodiment 3

[0035] Embodiment 3 polyimide / fullerene hybrid film PI / AC 60 -2.0%

[0036] Step (1): In a three-neck flask equipped with mechanical stirring, nitrogen inlet and outlet, and a thermometer, add 10.81 grams (0.10 moles) of p-phenylenediamine (p-PDA) and 230 grams of N,N-dimethylacetamide , stirred under nitrogen protection until completely dissolved; added 29.42 grams (0.10 moles) of 3,3',4,4'-biphenyltetracarboxylic dianhydride (s-BPDA), stirred until completely dissolved, at 15°C React for 24 hours to obtain a polyamic acid solution with a solid content of about 15 wt%.

[0037] Step (2): Weigh 0.72 g of methyl carbamate-modified C60 fullerene, add it to the above polyamic acid solution, and stir rapidly until the mixture is uniform.

[0038] Step (3): After filtering the above-mentioned polyamic acid / fullerene precursor solution and vacuum defoaming, it is coated on a glass plate or a stainless steel plate with a flat surface. Under nitrogen atmosphere, bake at 80°C for 1 ho...

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Abstract

The invention relates to a method for doping modified polyimide containing nano fullerene, wherein the method comprises the following steps: firstly, reacting diamine with dianhydride in an organic solvent to obtain polyamide acid; adding amino-acid ester or substituted amino-acid ester modified nano fullerene, and uniformly mixing to obtain a polyamide acid/fullerene precursor solution; and coating the precursor solution to prepare a film, and performing high-temperature thermal imidization to obtain the polyimide/fullerene hybrid film. According to the method, the storage stability of the polyamide acid solution can be effectively improved, and particularly, the problem of viscosity reduction caused by molecular chain degradation at a relatively high storage temperature can be inhibited; and meanwhile, due to the introduction of the nano fullerene, and on the basis of not influencing the surface smoothness of the polyimide film, the scratch resistance and the heat-conducting property of the film material are improved.

Description

technical field [0001] The invention belongs to the field of material doping and modification, and relates to a method for doping and modifying polymer materials, in particular to a method for preparing a polyimide film containing nano fullerenes. Background technique [0002] Polyimide is an important class of high-performance polymer materials, which has a very wide range of applications in aviation, aerospace, electronics, microelectronics, new energy and other fields. The imidization method of polyimide includes thermal imidization method and chemical imidization method. Most polyimides can only choose thermal imidization method due to their poor solubility. The method is to obtain polyimide through high-temperature thermal imidization treatment of polyamic acid or other polyamic acid derivatives. [0003] For the precursor of polyamic acid and its derivatives, its storage stability is poor, and obvious degradation can occur at higher temperature or even room temperatur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08K9/04C08K3/04C08J5/18
CPCC08J5/18C08K9/04C08K3/045C08J2379/08C08L79/08Y02E10/549
Inventor 张梅刘伟丽刘珊珊崔芃王尉胡光辉
Owner 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心)
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