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High-strength high-light-transmittance polyimide film and preparation method thereof

A technology of polyimide film and polyamic acid, which is applied in the field of high-strength and high-light-transmitting polyimide film and its preparation, can solve the problems of low film production quality, unfavorable film formation, molecular structure optimization, etc. Mechanical properties, fewer defects, minimal human and environmental impact

Inactive Publication Date: 2020-08-07
CHANGSHA ADVANCED MATERIALS IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method does not purify the monomer or optimize the molecular structure, which is not conducive to the process of forming a thin film by vacuum vapor deposition, and the quality of its thin film production is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In a reactor equipped with a stirrer, a condenser, a heating and cooling device, and a nitrogen protection device, 70.08 g of ODA (0.35 mol) and 48.03 g of TFMB (0.15 mol) were added in 800 mL of dimethylacetamide (DMAc), Heat and stir to dissolve until the solution is transparent, continue to heat to 170°C and reflux for 120 minutes, then stop heating, collect the filtrate after suction filtration, let stand to cool down to the solution temperature of 80°C, and then slowly add ethanol. Until the crystals were completely precipitated, the solid part was collected by suction filtration and washed twice with ethanol to obtain mixed diamine crystals.

[0039] Add 155.06g of ODPA (0.5mol) into m-cresol in a reactor equipped with a stirrer, condenser, heating and cooling device, and nitrogen protection device, heat and stir to dissolve until the solution is transparent, and continue heating to 190°C After refluxing for 120 minutes, stop heating, collect the filtrate after su...

Embodiment example 2

[0043]In a reactor equipped with a stirrer, a condenser, a heating and cooling device, and a nitrogen protection device, add 123.16 g of BATB (0.3 mol) and 64.03 g of TFMB (0.2 mol) into 800 mL of N-methylpyrrolidone (NMP) , heat and stir to dissolve until the solution is transparent, continue to heat to 190°C and reflux for 120 minutes, then stop heating, collect the filtrate after suction filtration, let stand and cool down to the solution temperature of 80°C, then slowly add ethanol. Until the crystals were completely precipitated, the solid part was collected by suction filtration and washed twice with ethanol to obtain mixed diamine crystals.

[0044] Add 147.11g of BTDA (0.5mol) to m-cresol in a reactor equipped with a stirrer, condenser, heating and cooling device, and nitrogen protection device, heat and stir to dissolve until the solution is transparent, and continue heating to 170°C After refluxing for 120 minutes, stop heating, collect the filtrate after suction fil...

Embodiment example 3

[0048] In a reactor equipped with a stirrer, a condenser, a heating and cooling device, and a nitrogen protection device, 70.08 g of ODA (0.35 mol) and 77.7 g of BAPP-2TF (0.2 mol) were added to 800 mL of N-methylpyrrolidone (NMP ), heat and stir to dissolve until the solution is transparent, continue to heat to 190°C and reflux for 120 minutes, then stop heating, collect the filtrate after suction filtration, let stand to cool down to the solution temperature of 80°C, and then slowly add ethanol. Until the crystals were completely precipitated, the solid part was collected by suction filtration and washed twice with ethanol to obtain mixed diamine crystals.

[0049] Add 197.11g of BPDA (0.5mol) to m-cresol in a reactor equipped with a stirrer, condenser, heating and cooling device, and nitrogen protection device, heat and stir to dissolve until the solution is transparent, and continue heating to 170°C After refluxing for 120 minutes, stop heating, collect the filtrate after ...

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Abstract

The invention relates to a high-strength high-light-transmittance polyimide film and a preparation method thereof. The invention provides a preparation method of a polyimide spinning solution with a ternary polymerization structure. The preparation method comprises the following steps: recrystallizing and purifying two diamine monomers respectively and mixing the two diamine monomers in proportion; recrystallizing the dianhydride monomers; respectively putting the mixed diamine monomers and a dianhydride monomer into two evaporation boats of vacuum coating equipment; respectively depositing the diamine and dianhydride monomers on a glass substrate with a smooth surface by adopting a vapor deposition method to obtain a uniform and transparent polyamide acid-polyimide film; and then puttinga substrate and the film into an imidization furnace, and carrying out gradient heating to obtain the polyimide film. Compared with a traditional steel belt tape casting method for preparing the polyimide film, the method has the advantages that the film prepared by the method undergoes a vapor deposition reaction in a vacuum state, so polymerization and imidization reactions are more complete, reaction defects are greatly reduced, and the overall performance of the film is more uniform. The light transmittance of the film reaches 85%, and the tensile strength of the film is 160 MPa.

Description

technical field [0001] The invention relates to a high-strength and high-transmittance polyimide film and a preparation method thereof, belonging to the technical field of polymer materials. Background technique [0002] Polyimide (PI) is a new type of material with good performance. It has excellent thermal stability, insulation performance and mechanical properties. The long-term use temperature of its products can reach above 250 ° C. Radiation performance, etc. At present, polyimide materials have been widely used in aerospace, microelectronics manufacturing, energy and communications, etc. [0003] Usually, the preparation of polyimide film is to carry out low-temperature polycondensation of diamine and dianhydride as monomers in a polar solvent to obtain a soluble polyamic acid solution, and then cast it by die-steel tape casting method Polyamic acid is flattened and formed into a film on a seamless steel belt, and then dehydrated and cyclized by heating or chemical i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08G73/10C08L79/08
CPCC08J5/18C08G73/1071C08G73/1042C08G73/1039C08J2379/08
Inventor 李衍黄活阳罗熙雯王芳刘永亮
Owner CHANGSHA ADVANCED MATERIALS IND RES INST CO LTD