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CN-122011387-A - Tear-resistant high-temperature-resistant film material and preparation method thereof

CN122011387ACN 122011387 ACN122011387 ACN 122011387ACN-122011387-A

Abstract

The invention belongs to the technical field of polyimide film materials, and discloses a tearing-resistant high-temperature-resistant film material and a preparation method thereof. Firstly preparing diamine monomer containing a bisimidazole structure, then carrying out chain extension crosslinking reaction on the diamine monomer and polyamide acid prepolymer to construct a three-dimensional crosslinked network, and finally obtaining the film material through imidization reaction and post-treatment. In the molecular structure of the film, the bisimidazole structural unit is connected with the polyimide main chain through a chemical bond to form a cross-linked network, and nitrogen atoms on an imidazole ring of the film and groups such as main chain carbonyl form hydrogen bond interaction, so that the film is used as a sacrificial bond to break and dissipate energy preferentially when stressed, and crack expansion is effectively prevented. The material has high temperature resistance, high strength, high toughness and excellent tear resistance, and can meet the requirements of the severe fields such as flexible display, aerospace high-temperature sealing and the like.

Inventors

  • MAI YONGFA
  • MAI ZHIHENG

Assignees

  • 广东纳美恒新材料科技有限公司

Dates

Publication Date
20260512
Application Date
20260312

Claims (6)

  1. 1. The preparation method of the tear-resistant and high-temperature-resistant film material is characterized by comprising the following steps of: (1) Preparing diamine monomer containing bisimidazole structure, namely taking aromatic aminobenzoic acid derivative and aromatic diamine compound as raw materials, and performing cyclization reaction in an acidic dehydration medium to obtain diamine monomer containing bisimidazole structure; (2) Preparing polyamic acid prepolymer solution, namely dissolving aromatic diamine monomer in polar aprotic solvent, stirring and dissolving, adding aromatic dianhydride monomer, and carrying out polymerization reaction under the low-temperature condition to obtain polyamic acid prepolymer solution; (3) Crosslinking modification reaction, namely mixing the diamine monomer containing the bisimidazole structure prepared in the step (1) with the polyamic acid prepolymer solution prepared in the step (2) to perform chain extension crosslinking reaction to obtain a modified polyamic acid prepolymer; (4) And (3) imidization reaction, namely mixing the modified polyamide acid prepolymer prepared in the step (3) with a dehydrating agent, carrying out imidization reaction, and carrying out post-treatment to obtain the tear-resistant and high-temperature-resistant polyimide film material.
  2. 2. The method for producing a tear-resistant and high temperature resistant film material according to claim 1, wherein in the step (1), the aromatic diamine compound is one or more of 3,3' -diaminobiphenyl, 4' -diaminobiphenyl, and 3,4' -diaminobiphenyl, and the aromatic aminobenzoic acid derivative is one or more of para aminobenzoic acid, meta aminobenzoic acid, and ortho aminobenzoic acid.
  3. 3. The method for preparing a tear-resistant and high temperature resistant film material according to claim 1, wherein in the step (2), the aromatic diamine monomer is one or more of 4,4' -diaminodiphenyl ether, 3,4' -diaminodiphenyl ether and 3,3' -diaminodiphenyl ether, and the aromatic dianhydride monomer is one or more of pyromellitic dianhydride, 3', 4' -biphenyl tetracarboxylic dianhydride and 3,3', 4' -diphenyl ether tetracarboxylic dianhydride.
  4. 4. The method for producing a tear-resistant and heat-resistant film material according to claim 1, wherein in the step (3), the diamine monomer having a bisimidazole structure is added in an amount of 2 to 25mol% based on the molar amount of the aromatic diamine monomer.
  5. 5. The method for preparing the tear-resistant and high-temperature-resistant film material according to claim 1, wherein in the step (4), the dehydrating agent is a mixture of acetic anhydride and a tertiary amine compound, the molar ratio of the acetic anhydride to the tertiary amine compound is 1:0.8-1.2, and the tertiary amine compound is one or more of triethylamine, pyridine and N, N-dimethylaniline.
  6. 6. A tear-resistant and high temperature resistant film material prepared by the method of any one of claims 1-5.

Description

Tear-resistant high-temperature-resistant film material and preparation method thereof Technical Field The invention belongs to the technical field of polyimide film materials, and particularly relates to a tearing-resistant high-temperature-resistant film material and a preparation method thereof. Background With the rapid development of flexible electronics, aerospace equipment, and new generation display technologies, there is an increasing need for high performance polymer film materials. Particularly, in application scenes such as flexible display substrates, sealing of high-temperature fuel pumps of aircraft engines, flexible copper-clad plates and the like, the film material is required to have excellent high-temperature resistance (the long-term use temperature is more than 300 ℃ and the thermal expansion coefficient is low), and also has excellent mechanical strength, tear resistance and folding resistance. Polyimide (PI) has been widely used in the above fields as a high-performance polymer due to its excellent thermal stability, mechanical properties and electrical insulation properties. For example, commercial polyimide films such as Kapton series from dupont and Upilex series from yu industrial company are high-performance polymer materials excellent in combination properties on the market at present. However, with the continuous expansion of application scenes and the improvement of performance requirements, the traditional polyimide materials have the limitations in certain aspects that firstly, the thermal performance is still provided with a room for improvement, particularly the thermal expansion coefficient is high, the application of the polyimide materials as high-precision base materials is limited, secondly, the tear resistance and toughness are insufficient, catastrophic failure are easy to occur when complex stress or tiny damage is born, thirdly, the strength can be improved by a method for reinforcing polyimide by most inorganic nano fillers (such as graphene and carbon nano tubes), but the ductility and toughness are often sacrificed. In recent years, researchers have attempted to improve both heat resistance and mechanical properties of polyimide through molecular structural design. For example, the introduction of a rigid heterocyclic structure (such as imidazole and oxazole) in the main chain of CN120059183a can increase the rigidity and linearity of the molecular chain, which is beneficial to reduce the thermal expansion coefficient and improve the thermal stability, however, the scheme adopts a linear copolymerization structure, while introducing a rigid unit and hydrogen bond, but lacking an effective three-dimensional crosslinking network, when subjected to complex stress or micro damage, the crack is easy to propagate along the molecular chain, and the tear resistance and toughness are still further improved. With the development of ultrathin and foldable flexible electronic devices, higher requirements are put on the tear resistance of film materials, and the conventional linear polyimide materials are difficult to meet. How to organically combine these molecular design concepts to develop a polyimide film material with ultrahigh heat resistance, excellent tear resistance and good processability is still a technical problem to be solved in the field. Disclosure of Invention The invention aims to provide a tearing-resistant high-temperature-resistant film material and a preparation method thereof, and the tearing-resistant high-temperature-resistant film material provided by the invention has high temperature resistance, high strength, high toughness and excellent tearing resistance, and can meet the harsh requirements of the fields of flexible display, aerospace and the like. In order to achieve the above object, the present invention provides the following technical solutions: The invention provides a preparation method of a tearing-resistant high-temperature-resistant film material, which comprises the following steps: (1) Preparing diamine monomer (BID) containing bisimidazole structure, namely taking aromatic aminobenzoic acid derivative and aromatic diamine compound as raw materials, and performing cyclization reaction in an acidic dehydration medium to obtain diamine monomer containing bisimidazole structure; (2) Preparing polyamic acid prepolymer solution, namely dissolving aromatic diamine monomer in polar aprotic solvent, stirring and dissolving, adding aromatic dianhydride monomer, and carrying out polymerization reaction under the low-temperature condition to obtain polyamic acid prepolymer solution; (3) Crosslinking modification reaction, namely mixing the diamine monomer containing the bisimidazole structure prepared in the step (1) with the polyamic acid prepolymer solution prepared in the step (2) to perform chain extension crosslinking reaction to obtain a modified polyamic acid prepolymer; (4) And (3) imidization reaction, namely mixing the modified poly