Preparation method of polyimide film

A polyimide film and diamine monomer technology, applied in the field of polyimide film preparation, can solve the problems of difficult process control, improve material mechanical properties, narrow processing window, etc., and achieve gel and insoluble content Low, wide film processing window, and the effect of improving processability and quality

Active Publication Date: 2022-06-14
宝珠特种材料科技(江苏)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method is relatively mature, there are many challenges in processing. For example, although polar aprotic solvents can dissolve polyamic acid, it still has poor solubility for high molecular weight polyamic acid, and is prone to phase separation to form fine gel particles. film quality; the lower polyimide molecular weight is not conducive to further improving the mechanical properties of the material; the rate of polymerization and cyclization reactions is slow and side reactions are prone to occur, and the ring-closing reaction of imide occurs simultaneously with solvent volatilization. Imide molecules do not have enough mobility to form crystals, the processing window is narrow, and the process is difficult to control

Method used

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  • Preparation method of polyimide film
  • Preparation method of polyimide film
  • Preparation method of polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 300 g of NMP (75% by mass in the total amount of the solvent), 1-ethyl-3-methylimidazolyl acetic acid were added as a solvent to a glass reaction vessel with an inner volume of 500 mL equipped with a stirrer and a nitrogen introduction and discharge pipe. Salt ([EMIM] + [Ac] - ) 100g of ionic liquid (accounting for 25% by mass in the total solvent), to which PPD 26.88g (0.249 mol), BPDA 73.12g (0.249 mol) were added, and the stirring was completely dissolved at room temperature. The reaction was stirred at 50° C. for 10 hours to obtain In the polyamic acid solution composition having a solid content concentration of 18.5% by weight, a solution viscosity of 58.0 Pa·s, and a logarithmic viscosity of 1.10, no flocs and insolubles were formed in the reaction product.

[0048] The polyamic acid solution composition was coated on a glass substrate with a doctor blade, the coating film was degassed and pre-dried at 25° C. under reduced pressure for 30 minutes, and then placed...

Embodiment 2

[0051] It was prepared in the same manner as in Example 1, except that 320 g of DMF (80 mass % of the total solvent) and 80 g of 1-ethyl-3-methylimidazolium acetate ionic liquid (20 mass % of the total solvent) were used Polyimide film.

[0052] The thermal decomposition temperature of the obtained polyimide film was 485° C., and the tensile strength was 295 MPa.

Embodiment 3

[0054] In addition to using DMF 160 g (40 mass % of the total solvent) and DEF 160 g (40 mass % of the total solvent), 1-ethyl-3-methylimidazolium acetate ionic liquid 80 g (accounting for the total solvent) A polyimide film was formed in the same manner as in Example 1 except for 20% by mass in the above.

[0055] The thermal decomposition temperature of the obtained polyimide film was 493° C., and the tensile strength was 310 MPa.

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Abstract

The invention discloses a preparation method of a polyimide film, which is characterized in that an ionic liquid with low decomposition temperature is added into a reaction system solvent as a cosolvent, and the content of the ionic liquid accounts for 3-90% of the total content of the solvent. By selecting the ionic liquid with proper decomposition temperature between 180 DEG C and 300 DEG C and utilizing high polarization energy of the ionic liquid, high solubility of an intermediate and a product polyimide is realized, and the obtained polyimide is high in molecular weight, low in content of gel and other insoluble substances, few in film defect, good in film forming flowability and high in mechanical property. It is guaranteed that the ionic liquid is stable and not decomposed in the thermal imidization process, the thermal imidization process is stable and controllable, the imidization degree is high, and side reactions are few. The ionic liquid promotes molecular motion ability and crystallization and reduces internal stress of the film.

Description

technical field [0001] The invention belongs to the field of new polymer materials, in particular to a preparation method of a polyimide film. Background technique [0002] Polyimide is a general term for a class of polymer materials with imide bonds in the main chain. It is one of the best heat-resistant varieties in engineering plastics. use. In addition, polyimide material also has excellent mechanical, thermal, electrical, chemical stability, radiation resistance and other comprehensive properties, and has been widely used in aviation, aerospace, microelectronics, nano, liquid crystal, separation membrane, laser, etc. field, becoming one of the most promising engineering plastics in the 21st century. Especially aromatic polyamides, the main chain usually has aromatic rings or aromatic heterocycles, the heat resistance can exceed 500 ℃, and the glass transition temperature can reach 400 ℃. It is a typical refractory and insoluble polymer, insoluble in common organic sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18C08L79/08
CPCC08G73/1067C08J5/18C08J2379/08Y02P20/54
Inventor 马禹汪文瀚
Owner 宝珠特种材料科技(江苏)有限公司
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