Polyimide with novel structure and preparation method of transparent polyimide film

A technology of polyimide and transparent film, which is applied in the field of preparation of polyimide and its transparent film, can solve problems such as inability to process and shape, and achieve the goal of improving transparency, good thermal performance and transparency, and large economic benefits Effect

Inactive Publication Date: 2015-04-29
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, after chemical imidization of polyimide acid, polyimide is difficult to dissolve in polar solvents, and it cannot be processed and formed to form a polyimide film.

Method used

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  • Polyimide with novel structure and preparation method of transparent polyimide film
  • Polyimide with novel structure and preparation method of transparent polyimide film
  • Polyimide with novel structure and preparation method of transparent polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve the mixed diamine of 1.162g (0.0043mol) 1,1-bis(4-aminophenyl)cyclohexane BAPC and 13.871g (0.0433mol) TFMB into 30g of strictly dry NMP at room temperature, nitrogen protection, Add 14.471g (0.0466mol) ODPA to it after mechanical stirring until completely dissolved, continue stirring for 1 hour under nitrogen protection, then add 0.496g (0.002mol) 4-PEPA to it, continue stirring for 24 hours under nitrogen protection to form a solid content of 50wt % polyamic acid solution with end-capping agent.

[0031] 4.15g of pyridine, 5.30g of triethylamine and 42.86g of acetic anhydride were added to the polyamic acid solution, stirred at room temperature for 24h, and the polyimide prepolymer solution was obtained after the reaction was completed, and the polyimide prepolymer The solution is precipitated into methanol, filtered, washed, and dried at 60°C to obtain a polyimide prepolymer solid, which is dissolved in NMP with the same mass as the polyimide prepolymer soli...

Embodiment 2

[0034] At room temperature, 6.614g (0.0247mol) of 1,1-bis(4-aminophenyl)cyclohexane BAPC and 7.898g (0.0247mol) of TFMB were dissolved in 20g of strictly dry NMP, under nitrogen protection, and mechanically stirred until After completely dissolving, add 14.992g (0.0484mol) ODPA thereinto, add 0.496g (0.002mol) 4-PEPA to it after continuing to stir 1h under nitrogen protection, continue to stir 24h under nitrogen protection to generate the belt with solid content of 60wt%. Polyamic acid solution of capping agent.

[0035]Add 4.298g (0.0544mol) of pyridine, 5.495g (0.0544mol) of triethylamine (0.0544mol) and 44.395g (0.4352mol) of acetic anhydride into the polyamic acid solution, stir at room temperature for 24h, and obtain the polyimide preform after the reaction is completed. Polymer solution, the polyimide prepolymer solution is precipitated into methanol, filtered, washed, and dried at 60°C to obtain a polyimide prepolymer solid, which is dissolved in a polyimide prepolymer ...

Embodiment 3

[0038] At room temperature, 2.143g (0.0080mol) of 1,1-bis(4-aminophenyl)cyclohexane BAPC and 12.796g (0.0400mol) of TFMB were dissolved in 45g of strictly dried NMP, under nitrogen protection, and mechanically stirred until After completely dissolving, add 14.565g (0.0470mol) ODPA thereinto, continue to stir 1h under nitrogen protection, add 0.496g (0.002mol) 4-PEPA to it after 1h, continue to stir 24h under nitrogen protection to generate solid content and be 40wt% ribbon Polyamic acid solution of capping agent.

[0039] Add 7.423g (0.094mol) of pyridine, 1.186g (0.0117mol) of triethylamine and 43.131g (0.4229mol) of acetic anhydride to the polyamic acid solution, stir at room temperature for 24h, and obtain the polyimide preform after the reaction. Polymer solution, the polyimide prepolymer solution is precipitated into methanol, filtered, washed, and dried at 60°C to obtain a polyimide prepolymer solid, which is dissolved in a polyimide prepolymer The polyimide prepolymer ...

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Abstract

The invention discloses polyimide with novel structure and a preparation method of a transparent polyimide film. The method comprises the steps: a, mixing a fluorine-containing aromatic diamine monomer with alicyclic diamine in a molar ratio of 1-10:1 to form mixed diamine under the protection of nitrogen or argon; dissolving the mixed diamine into a polar solvent; completely dissolving under a constant temperature and adding ether-containing aromatic dianhydride; adding an end-capping reagent to synthesize a fluorine-containing polyamide acid of which the molecular weight is 20000-10<6>; b, adding a catalyst and a dewatering agent to fluorine-containing polyamide acid solution, wherein the catalyst is a mixture prepared from pyridine and triethylamine; reacting for 24 hours at a constant temperature, and washing by using excessive amount of organic solvent to produce fluorine-containing polyamide powder; c, drying the polyamide powder at the temperature of 60 DEG C, and dissolving into a polar solvent to obtain the fluorine-containing polyamide acid solution of which the solid content is 40-60 percent. The polyimide is simple in process, energy-saving, environment-friendly and high in economic benefit.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a method for preparing polyimide with a novel structure and a transparent film thereof. Background technique [0002] Polyimide has excellent mechanical properties, heat resistance, low temperature resistance, flame retardancy, solvent resistance and electrical properties. It can be used as a structural composite material and is widely used in aerospace, aviation, precision machinery, microelectronic devices and Transparent conductive film, TFT substrate and flexible printed circuit substrate, etc. [0003] The performance of polyimide is closely related to its molecular structure. Adjusting the molecular structure can properly modify its performance to meet special application requirements. "Polyimides: Synthesis, Characterization and Application" explains that most polyimide materials are insoluble and infusible, so the precursor polyimide acid solution is usually us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18C08L79/08
Inventor 刘继延郭文勇陈妤红于洁尤庆亮胡思前徐瑛
Owner JIANGHAN UNIVERSITY
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