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Thermoplastic polyimide resin composite film with low dielectric property and preparation method thereof

A technology of polyimide resin and composite film, which is applied in the field of thermoplastic polyimide resin composite film and its preparation, can solve the influence of polyimide matrix mechanical properties and heat resistance performance, and reduce polyimide film Difficult to control the electrical constant and the uniformity of inorganic fillers, etc., to achieve good melt processability, increase and reduce water absorption, and improve the effect of anisotropy

Active Publication Date: 2021-11-05
烟台丰鲁精细化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] CN109228586B discloses a kind of low dielectric polyimide multilayer composite film, introduces cage type polysilsesquioxane through thermosetting polyimide layer and thermoplastic polyimide adhesive layer, and it is dispersed in polyimide After the imide is added, introducing molecular-sized holes into the polyimide can effectively reduce the dielectric constant of the polyimide film, but it adopts a multi-layer composite structure, and it is difficult to control the adhesion and thickness, which increases the process. complexity of
[0007] CN106750435B discloses a method for preparing a low dielectric constant ordered porous polyimide film, in which polyimide is grafted on the surface of amino-modified silica microspheres in the form of chemical bonds to prepare a polyimide composite The ordered porous polyimide film with low dielectric constant can be prepared by using a thin film made of polyimide, but it needs to etch away the silicon dioxide in the hydrofluoric acid etching solution, which will have a negative impact on the mechanical properties and heat resistance of the polyimide matrix. certain influence
[0008] In summary, despite the above-mentioned improvements, the matrix polyimide still has problems such as poor solubility and difficulty in controlling the uniformity of inorganic fillers.
And there is no relevant information about the melt processing method of low dielectric polyimide and the blending modification with LCP resin

Method used

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  • Thermoplastic polyimide resin composite film with low dielectric property and preparation method thereof
  • Thermoplastic polyimide resin composite film with low dielectric property and preparation method thereof
  • Thermoplastic polyimide resin composite film with low dielectric property and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Add 8.0058g (0.025mol) 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl monomer, 9.6105g (0.025mol) 9,9-bis( 4-Amino-3-fluorophenyl) fluorene monomer, 180mL N,N-dimethylacetamide, stirring at room temperature under nitrogen protection, after the diamine monomer is completely dissolved, add 4.5833g (0.01mol) p- Phenyl-bis trimellitate dianhydride monomer: 20.7155g (0.0398mol) bisphenol A type diether dianhydride monomer, 50mL N,N-dimethylacetamide; react at room temperature for 22 hours, add 0.1185 g (0.0008mol) phthalic anhydride monomer, and react at room temperature for 4 hours to obtain a polyamic acid solution.

[0056] Add 34ml of a mixed solution of acetic anhydride and pyridine (30mL of acetic anhydride and 4mL of pyridine), continue the reaction at room temperature for 6 hours, slowly pour the reaction solution into 3L of deionized water to precipitate, filter, and wash the obtained filter cake twice with deionized water , and then dried in a vacuum oven at 120° C....

Embodiment 2

[0059] Add 336.23g (1mol) 2,2'-bis(trifluoromethyl)-4,4'-diaminophenylether monomer into a dry and clean 50L double-layer glass reactor, 1567.98g (4mol) 9, 9-bis(4-aminophenyl)fluorene monomer, 17L N,N-dimethylacetamide, stirring at room temperature under the protection of nitrogen, after the diamine monomer is completely dissolved, slowly add 458.33g (1mol) p- Phenyl-bis trimellitate dianhydride monomer: 1601.19g (3.98mol) 4,4'-triphenylene ether tetracarboxylic dianhydride monomer, 1L N,N-dimethylacetamide; normal temperature reaction After 18 hours, 11.85 g (0.08 mol) of phthalic anhydride monomer was added and reacted at room temperature for 4 hours to obtain a polyamic acid solution.

[0060] Add 2.83L of a mixed solution of acetic anhydride and pyridine (2.04L of acetic anhydride, 0.79L of pyridine), continue the reaction at room temperature for 6 hours, dilute the reaction solution with 54L of N,N-dimethylacetamide and slowly pour it into 360L Precipitated in deionized...

Embodiment 3～14 and comparative example 1～2

[0063] Replace the diamine and dianhydride with the ratios shown in the following Table 1 and Table 2 to carry out resin polymerization respectively, and conduct heat preservation reaction at 0-50°C for 1h-24h polymerization to obtain polyamic acid with a solid content of 10-30% solution.

[0064] Then, in the same manner as in Example 1, a 25 μm thick polyimide film was prepared.

[0065] For the polyimide films obtained in Examples and Comparative Examples, the properties of the prepared polyimide films were measured according to the above-mentioned method, and the results are summarized in Table 1 and Table 2.

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Abstract

The invention relates to a thermoplastic polyimide resin composite film with low dielectric property, and belongs to the technical field of composite film materials, the polyimide resin composite film is prepared by blending and modifying polyimide resin and LCP resin, according to the parts by weight, the polyimide resin is prepared from the following components in parts by weight: 20 to 100 parts of p-phenylene-biphenyl trimellitate dianhydride monomer, 0 to 80 parts of other copolymerized dianhydride monomer, 20 to 80 parts of diamine monomer containing fluorine group, and 20 to 80 parts of diamine monomer containing large side group. The polyimide resin has the characteristics of good solubility and good melt processability, the processing cost of polyimide is reduced, the molecular structure contains ester groups, the compatibility can be improved by blending modification with the LCP resin, the anisotropy problem caused by crystal orientation of the LCP resin is improved, the composite film is prepared, the dielectric property is further improved, and the water absorption rate is further reduced.

Description

technical field [0001] The invention relates to a thermoplastic polyimide resin composite film with low dielectric properties and a preparation method thereof, belonging to the technical field of composite film materials. Background technique [0002] In the era of big data, the information processing of electronic products is constantly developing in the direction of high-frequency signal transmission and high-speed digitalization. In the future, the transmission frequency above 10GHz will become a trend. To ensure that electronic products have good signal transmission quality under the condition of high-frequency signal transmission, it is necessary to have a good distance between the transmission line in the conductive copper foil of the circuit board and the connected electronic components. Impedance matching state to avoid signal reflection, scattering, attenuation and delay. The dielectric constant of the insulating layer material in contact with the conductive lines ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08G73/10C08J5/18
CPCC08J5/18C08G73/1071C08G73/1042C08G73/1039C08G73/1007C08J2379/08
Inventor 刘洋初金军辛乐民徐伟杰丰佩川
Owner 烟台丰鲁精细化工有限责任公司
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