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Colorless transparent non-fluorine polyimide film with low thermal expansion coefficient and preparation method and application thereof

A technology of polyimide film and low thermal expansion coefficient is applied in the field of preparation of colorless transparent non-fluorine polyimide film with low thermal expansion coefficient, which can solve problems such as no systematic reports.

Active Publication Date: 2020-04-21
威海新元科盛新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no systematic report in the relevant research protocol literature

Method used

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  • Colorless transparent non-fluorine polyimide film with low thermal expansion coefficient and preparation method and application thereof
  • Colorless transparent non-fluorine polyimide film with low thermal expansion coefficient and preparation method and application thereof
  • Colorless transparent non-fluorine polyimide film with low thermal expansion coefficient and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Embodiment 1 prepares a colorless transparent polyimide film by the polymerization of hydrogenated pyromellitic dianhydride (HPMDA) and 2-methyl-4,4'-diaminobenzanilide (MeDABA):

[0058]Add 24.1290g (0.1mol) MeDABA and 100g NMP into a 500mL three-neck flask equipped with a heating mantle, mechanical stirring, thermometer, water separator, and reflux condenser. Nitrogen gas was introduced and a clear solution was obtained after mechanical stirring for 20 min. 22.4170 g (0.1 mol) HPMDA was added under stirring, and the viscosity of the system gradually increased. Add 8.6g of NMP and stir at room temperature for 30min to obtain a viscous solution. Add 0.5g pyridine and 150mL toluene as catalyst and azeotropic dehydrating agent respectively. When the system temperature rises to 130-140°C, the toluene / water azeotrope evaporates out of the water separator. Keep reflux for dehydration until no water drops come out of the system. Continue to heat up to 180°C and keep the t...

Embodiment 2

[0069] Embodiment 2 prepares a colorless transparent polyimide film by the polymerization of hydrogenated pyromellitic dianhydride (HPMI) and 2-chloro-4,4'-diaminobenzoanilide (ClDABA):

[0070] Resin and film preparation are as in Example 1, the difference is that 2-methyl-4,4'-diaminobenzanilide (MeDABA) is replaced by 2-chloro-4,4'-diaminobenzanilide (ClDABA ). Typical chemical structures of the as-prepared films are shown below.

[0071]

[0072] Number average molecular weight M n =37634 g / mol, n=83.

[0073] Infrared spectrum as attached figure 1 shown;

[0074] XRD spectrum is attached figure 2 shown;

[0075] The TGA spectrum is attached image 3 shown;

[0076] The DSC spectrum is attached Figure 4 shown;

[0077] The TMA spectrum is attached Figure 5 shown;

[0078] The UV-Vis spectrum is attached Figure 6 shown.

[0079] The performance data are shown in Table 1.

Embodiment 3

[0080] Example 3 Preparation of colorless transparent polymer by polymerization of hydrogenated 3,3',4,4'-biphenyltetracarboxylic dianhydride (HBPDA) and 2-methyl-4,4'-diaminobenzoanilide (MeDABA) Imide film:

[0081] The preparation of the resin and film was as in Example 1, except that hydrogenated pyromellitic dianhydride (HPMI) was replaced by hydrogenated 3,3',4,4'-biphenyltetracarboxylic dianhydride (HBPDA). Typical chemical structures of the as-prepared films are shown below.

[0082]

[0083] Number average molecular weight M n =26295 g / mol, n=51.

[0084] Infrared spectrum as attached figure 1 shown;

[0085] XRD spectrum is attached figure 2 shown;

[0086] The TGA spectrum is attached image 3 shown;

[0087] The DSC spectrum is attached Figure 4 shown;

[0088] The TMA spectrum is attached Figure 5 shown;

[0089] The UV-Vis spectrum is attached Figure 6 shown.

[0090] The performance data are shown in Table 1.

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Abstract

The invention discloses a preparation method and application of a colorless transparent non-fluorine polyimide film with a low thermal expansion coefficient. The film is prepared from an alicyclic dianhydride monomer and an aromatic diamine monomer containing a rigid amide bond and an alkyl or chlorine substituent through a high-temperature solution polycondensation method. The alicyclic dianhydride monomer can be hydrogenated pyromellitic dianhydride (HPMDA) or hydrogenated biphenyl tetracarboxylic dianhydride (HBPDA); the aromatic diamine monomer containing the rigid amide bond and the alkylor chlorine substituent can be selected from 2-methyl-4, 4'-diaminobenzanilide, 2-chloro-4, 4'-diaminobenzanilide, 2, 3'-dimethyl-4, 4'-diaminobenzanilide and the like. According to the invention, the coefficient of thermal expansion (CTE) of the film can be significantly reduced on the premise of maintaining good solubility of the PI resin and good optical transparency of the PI film. And the CTE value can be further reduced after the film is compounded with the silicon dioxide colloid.

Description

technical field [0001] The invention belongs to the field of functional polyimide films, and relates to a preparation method and application of a colorless and transparent non-fluorine polyimide film with low thermal expansion coefficient. Background technique [0002] In view of the dark color of traditional polyimide (PI) film, the application in the field of optoelectronics is greatly limited. At the same time, combined with the urgent application demand for colorless, transparent and high temperature resistant polymer optical film in the manufacture of advanced optoelectronic devices, people A series of colorless and transparent PI (CPI) films have been developed. The colorless and transparent means of traditional PI thin films is mainly to minimize the formation of charge transfer complexes (CTC) between its molecular chains or inside the molecular chains. At present, the more common methods are mainly to prepare CPI films by introducing fluorine-containing groups or a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/14C08J5/18C08K3/36C08L79/08
CPCC08G73/14C08J5/18C08J2379/08C08K3/36
Inventor 李璐姜岗岚张健李霄原伟涛王学伟
Owner 威海新元科盛新材料有限公司
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