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Method for preparing polyimide film from reactive end-capped polyamic acid resin

A technology of polyimide film and end-capped polyamic acid, applied in the field of polyimide film, can solve the problems of low molecular weight of polyamic acid resin, affecting product performance, and decreasing the strength and toughness of polyimide film. , to achieve the effects of high strength, high toughness, heat resistance stability, simplified production process and simple operation

Active Publication Date: 2015-12-16
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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  • Method for preparing polyimide film from reactive end-capped polyamic acid resin
  • Method for preparing polyimide film from reactive end-capped polyamic acid resin
  • Method for preparing polyimide film from reactive end-capped 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] The main properties of table 2 polyimid...

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 reactive end-capped polyamic acid resin. The method includes the preparing process that aromatic diamine, aromatic dianhydride and a reactive bifunctional end-capping agent are dissolved in aprotic polar solvent and subjected to a polycondensation reaction to obtain a solution of polyamide acid with the ends capped by reactive functional groups; the polyamide acid solution forms a film shape on the surface of a supporting base plate through tape casting, and a polyamide acid glue film which is partially imidized and has self-supporting performance is formed through heating; the polyamide acid glue film is fixed to a metal frame and subjected to heat treatment to obtain the high-strength and high-toughness polyimide film. The polyamide acid resin with the ends capped by the reactive functional groups and controllable molecular weight has the advantages of high solid content, low solution viscosity and excellent tape casting film forming manufacturability and is suitable for preparing the thick, high-strength and high-toughness polyimide film. The formed polyimide film has excellent mechanical properties and high-temperature stability and can be used for a base material and a covering film of a flexible printed circuit board and a chip carrier with 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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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
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