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A kind of method that prepares polyimide film by reactive terminal polyamic acid resin

A technology of polyimide film and end-capped polyamic acid, which is applied in the field of polyimide film, can solve the problems of low molecular weight of polyamic acid resin, decrease in strength and toughness of polyimide film, and affect product performance, etc. , to achieve the effects of reducing apparent viscosity, improving manufacturability, and simplifying production process

Active Publication Date: 2018-02-02
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the polyamic acid resin terminated by non-reactive monofunctional group has a lower molecular weight, which leads to a significant decrease in the strength and toughness of the prepared polyimide film, which affects the performance of the product.

Method used

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  • A kind of method that prepares polyimide film by reactive terminal polyamic acid resin
  • A kind of method that prepares polyimide film by reactive terminal polyamic acid resin
  • A kind of method that prepares polyimide film by reactive terminal polyamic acid resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Add 18.6720g (0.1727mol) of PDA and 150g of DMAc into a 500ml three-neck flask equipped with a mechanical stirrer and a spherical reflux condenser, stir mechanically at 50°C until they are completely dissolved, and then rapidly lower the ambient temperature to 25°C, Simultaneously increase the stirring rate, slowly add the mixture of dried 49.8607g (0.1695mol) s-BPDA and 1.5862g (0.0064mol) 4-PEPA while stirring, supplement 130.48gDMAc to rinse the bottle wall and the residue on the stirring paddle monomer, until the solid content of the solution is 20wt.%, continue stirring for 24h until the solution is clear, and the design molecular weight is 2×10 4 g / mol reddish-brown 4-PEPA-terminated polyamic acid resin solution, wherein the designed mole fraction of anhydride end groups in 4-PEPA accounts for 1.85% of the total anhydride groups, and its apparent viscosity at 25°C is 109000cP (109Pa· s), the intrinsic viscosity is 0.72dl / g; the obtained polyamic acid solution ...

Embodiment 2

[0049] (1) adopting the method identical with embodiment 2 steps (1) to prepare design molecular weight is 2.5 * 10 4 g / mol polyamic acid resin, wherein the design mole fraction of anhydride end groups in 4-PEPA accounts for 1.48% of the total anhydride groups, the difference is the amount of monomer added: PDA plus 18.6744g (0.1727mol), s- BPDA plus 50.0566g (0.1701mol), 4-PEPA plus 1.2665g (0.0051mol), supplemented DMAc plus 129.99g. The apparent viscosity of the obtained 4-PEPA-terminated polyamic acid resin solution at 25° C. was 111,000 cP (111 Pa·s), and the intrinsic viscosity was 0.76 dl / g.

[0050] (2) The 4-PEPA-terminated polyamic acid film was prepared by the same method as in step (2) of Example 1, except that the standard gap of the coating rod was 450 μm.

[0051] (3) The polyimide film was prepared by the same method as in step (3) of Example 1, and the main properties of the obtained film are shown in Table 2.

[0052] Table 2 Main properties of polyimide fi...

Embodiment 3

[0055] (1) adopting the method identical with embodiment 1 step (1) to prepare design molecular weight is 3.0 * 10 4 g / mol polyamic acid resin, wherein the design mole fraction of anhydride end groups in 4-PEPA accounts for 1.23% of the total anhydride groups, the difference is the amount of monomer added: PDA plus 18.7157g (0.1731mol), s- BPDA plus 50.2935g (0.1709mol), 4-PEPA plus 1.0563g (0.0043mol), supplemented DMAc plus 130.26g. The apparent viscosity of the obtained polyamic acid resin solution at 25°C was 125000cP (125Pa·s), and the intrinsic viscosity was 0.80dl / g.

[0056] (2) The 4-PEPA-terminated polyamic acid film was prepared by the same method as in step (2) of Example 1, except that the standard gap of the coating rod was 400 μm.

[0057] (3) The polyimide film was prepared by the same method as in step (3) of Example 1, and the main properties of the obtained film are shown in Table 3.

[0058] Table 3 Main properties of polyimide film

[0059] mem...

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Abstract

The invention relates to a method for preparing a polyimide film from a reactive end-capped polyamic acid resin. The preparation process is: using aromatic diamine and aromatic dianhydride, and a reactive bifunctional end-capping agent dissolved in an aprotic electrode Polyamic acid solution terminated with reactive functional groups is obtained through polycondensation reaction in a neutral solvent; the polyamic acid solution is cast on the surface of the support substrate to form a film, and heated to form a partially imidized and self-supporting polyamic acid film ; The polyamic acid film is fixed on the metal frame, and the high-strength polyimide film is obtained through heat treatment. The reactive functional group-terminated polyamic acid resin with controllable molecular weight of the present invention has the characteristics of high solid content, low solution viscosity, and excellent cast film-forming processability, and is suitable for preparing polyimide films with large thickness and high strength and toughness; The formed polyimide film has excellent mechanical properties and high temperature resistance stability, and can be used as a base material of a flexible printed circuit board, a cover film and a chip carrier of a self-adhesive tape.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, on the one hand, it relates to a method for preparing polyimide film from reactive end-capped polyamic acid resin; permanent polyimide film. Background technique [0002] Aromatic polyimide film has the characteristics of high strength, high toughness, high electrical insulation, low dielectric loss, radiation resistance, and corrosion resistance. High-tech fields such as packaging, photoelectric display, and electrical insulation have huge commercial value and broad application prospects. With the rapid development of microelectronic devices in the direction of high performance, multi-function, light weight, thin layer, miniaturization, and low cost, it puts forward higher and higher requirements for polyimide film for packaging substrates (Ree M, High performance polyimides for applications in microelectronics and flat panel displays, Macromolecular Research, 2006, 14(1): 1-33). Si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10
Inventor 杨士勇袁莉莉冀棉李强强
Owner INST OF CHEM CHINESE ACAD OF SCI