Method for preparing polyimide film by microwave radiation at low temperature

A technology of polyimide film and microwave radiation, which is applied in the field of preparing polyimide film at low temperature through microwave radiation, can solve the problem of thermal performance degradation of synthetic polyimide, performance degradation of polyimide film, and unfavorable large-scale production and other issues, to achieve the effect of reducing the requirements for instruments, improving production efficiency, and facilitating industrial production and wide application

Active Publication Date: 2019-10-22
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above method, the solvent used contains carcinogens, which is not conducive to large-scale production, and the thermal performance of the synthesized polyimide is also reduced
Therefore, the existing technology has the problems of being unfavorable for large-scale production and reducing the performance of polyimide films.

Method used

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  • Method for preparing polyimide film by microwave radiation at low temperature
  • Method for preparing polyimide film by microwave radiation at low temperature
  • Method for preparing polyimide film by microwave radiation at low temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Under normal temperature and pressure conditions, in a 250ml three-necked flask, add 10 grams of ODPA and 65.8 grams of NMP and add magnets, use a magnetic stirrer to stir evenly, then add 6.45 grams of ODA, ODPA (dibasic acid anhydride) and ODA (dibasic amine ) in a molar ratio of 1:1, and the feeding of the diamine was carried out three times with an interval of 20 minutes between each feeding. The reddish-brown viscous polyimide precursor solution is product A. Put the polyimide precursor solution into the microwave equipment, and irradiate for 20 minutes under the conditions of 1000W and 70°C to obtain product B. Pour product B on a quartz glass plate, and use a wire bar coater to spread the film to obtain product C, then put it in a vacuum oven, heat for 4 hours at 80°C and a vacuum of 30kPa to remove the solvent, and obtain product D . Put product D into microwave equipment, and cure it at 2000W, 70°C for 18 hours, and finally prepare the film material. The pre...

Embodiment 2

[0041] Under normal pressure, heat the heat conduction oil in the oil bath to 80°C in advance, add 10 grams of ODPA and 78 grams of NMP to a 250ml three-necked flask and add magnets, and then load the three-necked flask to the specified temperature in advance In the oil bath pot, use a magnetic stirrer to stir, the stirring speed is 200rpm, nitrogen protection, the nitrogen outlet passes through the top of the spherical condenser to prevent the solvent from being blown out by the nitrogen flow. After fully dissolving, add 9.4 grams of MDI, the molar ratio of MDI (isocyanate) and ODPA (dibasic acid anhydride) is 1:1, the addition of isocyanate is carried out three times, and the length of addition is 1 hour. After the addition is completed, stir magnetically at room temperature for 6 Hours, make it fully react, obtain solid content and be that the polyimide precursor solution of 20% clear transparent dark reddish-brown viscous shape is B product. Put the polyimide precursor sol...

Embodiment 3

[0047] A method for preparing polyimide film at low temperature by microwave radiation, comprising the following steps:

[0048] The first step is to prepare a polyimide precursor solution to obtain product A;

[0049] In the second step, product A is subjected to microwave radiation treatment to obtain product B;

[0050] In the third step, product B is subjected to coating treatment to obtain product C;

[0051] In the fourth step, product C is heated to obtain product D;

[0052] The fifth step is to carry out imidization treatment on product D by low-temperature microwave radiation to obtain a finished product;

[0053] In the fifth step, the temperature is 60-100°C.

[0054] The preparation of polyimide precursor solution comprises the following specific steps in the first step:

[0055] A1. Add an aprotic polar solvent into a three-necked flask, then add dibasic acid anhydride, add magnetons, and stir evenly with a magnetic stirrer to obtain a solution;

[0056] A2....

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Abstract

The invention discloses a method for preparing a polyimide film by microwave radiation at a low temperature. The method comprises the following steps: 1, preparing a polyimide precursor solution to obtain a product A; 2, performing microwave radiation on the product A to obtain a product B; 3, carrying out film spreading treatment on the product B to obtain a product C; 4, heating the product C toobtain a product D; and 5, imidizing the product D by adopting low-temperature microwave radiation at 60-100 DEG C to obtain the finished film. The method can realize the low-temperature complete imidization of the polyimide film only by a low-temperature microwave radiation technology on the premise of not changing or even improving the mechanical and thermal properties of the polyimide film inorder to obtain the polyimide film having excellent performances. The method has the characteristics of facilitation of large-scale production, and ensuring of the performances of the polyimide film.

Description

technical field [0001] The invention relates to a method for preparing polyimide film, in particular to a method for preparing polyimide film at low temperature through microwave radiation. Background technique [0002] The performance of PI film is comprehensive, with excellent high and low temperature resistance, dilute acid resistance, high strength and high modulus, high creep resistance, low thermal expansion coefficient, low water absorption, low dielectric constant and dielectric loss, radiation resistance and corrosion resistance, etc. , Therefore, it is widely used in some emerging fields such as aerospace, electronic and electrical insulation, microelectronics, solar cells and lithium batteries; for example: radiation-resistant shielding materials in the aerospace field, protective layers for microelectronic devices, etc. At present, the preparation method is generally to synthesize a polyamic acid solution through polycondensation of a dibasic acid anhydride and a...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08J7/12C08G73/10C08L79/08
CPCC08J5/18C08J7/08C08J7/123C08G73/1035C08G73/1071C08G73/1025C08J2379/08
Inventor 韩世辉张帅孙高辉陈蓉蓉王君段天娇
Owner HARBIN ENG UNIV
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