Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of uniform polyimide film

A technology of polyimide film and polyamic acid film, which is applied in the field of preparation of uniform polyimide film, can solve the problems of uneven surface of polyimide film, uneven polyamic acid solution, wide molecular weight distribution, etc. , to achieve the effects of easy and stable control of the processing process, reduction of film defects, and narrow molecular weight distribution

Active Publication Date: 2022-02-01
CHINA PETROLEUM & CHEM CORP +1
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] What the present invention is to solve is the problems of uneven polyamic acid solution and wide molecular weight distribution in the prior art, which lead to uneven surface of polyimide film, unstable process and decreased product quality.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of uniform polyimide film
  • Preparation method of uniform polyimide film
  • Preparation method of uniform polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 1. Stock solution preparation: Add 1.0814kg (10mol) p-phenylenediamine (PDA) and 35.39kg N,N-dimethylacetamide (water content 180ppmw) into the reaction kettle,2 Protect and stir until the monomer is completely dissolved, add 2.8773kg (9.78mol) 3,3′,4,4′-biphenyltetraacid dianhydride (BPDA) powder at a rate of 1.4kg / h, and continue to heat at 25°C after the addition is complete. N 2 Stirring under protection for 2 hours at a stirring speed of 250 rpm, a uniform transparent viscous polyamic acid solution was obtained. After testing, the apparent viscosity of the polyamic acid solution at 25°C was 21Pa·s, the number average molecular weight was 167000, and the molecular weight distribution was 1.37. foreign body. The polyamic acid solution is filtered through 5 μm and 0.5 μm filter materials, and then degassed under reduced pressure to obtain a polyamic acid film-forming stock solution.

[0050] 2. Cast film formation: the polyamic acid stock solution is controlled by a...

Embodiment 2

[0056] 1. Stock solution preparation: Add 2.0024kg (10mol) 4,4'-diphenyl ether diamine (ODA) and 21.98kg N,N-dimethylacetamide (water content 460ppmw) into the reaction kettle, 2 Protect and stir until the monomer is completely dissolved, add 2.8773kg (9.78mol) 3,3',4,4'-biphenyltetraacid dianhydride (BPDA) powder at a rate of 0.96kg / h, and continue at 0°C after the addition is complete N 2 Stirring for 4 hours under protection at a stirring speed of 200 rpm, a uniform transparent viscous polyamic acid solution was obtained. After testing, the polyamic acid solution has an apparent viscosity of 74Pa·s, a number average molecular weight of 172000, and a molecular weight distribution of 1.41 at 25°C. After passing the solution through a 2μm glass fiber filter membrane, the filter screen is exposed to ultraviolet fluorescent lamps. No foreign matter. The polyamic acid solution is filtered through 8 μm and 1 μm filter materials, and then degassed under reduced pressure to obtain...

Embodiment 3

[0060] 1. Preparation of stock solution: Add 1.0012kg (5mol) 4,4'-diphenyl ether diamine (ODA) and 22.16kg N,N-dimethylacetamide (water content 460ppmw) into the reaction kettle, at 20°C N 2 Stir under protection, after completely dissolving, add 1.4416kg (4.9mol) 3,3′,4,4′-biphenyltetraacid dianhydride (BPDA) powder at a rate of 2.88kg / h, continue to heat at 20°C after the addition is complete N 2 Stir for 1 h under protection at a stirring speed of 400 rpm to obtain a uniform transparent viscous polyamic acid solution. After testing, the polyamic acid solution has an apparent viscosity of 60Pa·s, a number average molecular weight of 163000, and a molecular weight distribution of 1.20 at 25°C. After passing the solution through a 2μm glass fiber filter membrane, the filter screen is exposed to ultraviolet fluorescent lamps. No foreign matter. The polyamic acid solution is filtered through 10 μm and 1 μm filter materials, and then degassed under reduced pressure to obtain a...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
thicknessaaaaaaaaaa
tensile strengthaaaaaaaaaa
glass transition temperatureaaaaaaaaaa
Login to View More

Abstract

The invention provides a method for preparing a uniform polyimide film, which mainly solves the problems in the prior art that the surface of the polyimide film is uneven and there are many gel particles, which cause the film preparation process to be difficult to control and the product performance to decline. By adopting a preparation method of polyimide film, it is prepared from polyamic acid solution through filtration, defoaming, film casting, solvent pre-baking, thermal stretching and thermal imidization, characterized in that the polyimide The amic acid solution has the following characteristics: (a) the polyamic acid solution used has a molecular weight distribution of 1.2 to 1.5 measured by gel permeation chromatography; (b) the polyamic acid solution used is filtered through a 2 μm glass fiber filter membrane, and the filtered The technical proposal that the film has no foreign matter under a microscope solves this problem well, and can be used in the industrial production of polyimide film.

Description

technical field [0001] The invention relates to a preparation method of a uniform polyimide film. Background technique [0002] As the engineering plastic with the best heat resistance that has been industrially produced, polyimide material has excellent thermal stability, mechanical properties, low temperature resistance, outstanding insulation performance, and solvent resistance. It has a wide range of applications in many fields such as microelectronics and mechanization. Polyimide film is one of the most demanded polyimide products today. Its excellent corona resistance, radiation resistance, dielectric properties and dimensional stability make the demand for high-performance polyimide film materials continue Increase. [0003] Due to the large number of imide rings and benzene ring structures in the main chain of polyimide, there is a strong intermolecular force between the molecular chains, which makes the molecular chain structure of polyimide tight, showing the cha...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10
CPCC08G73/1042C08G73/1046C08G73/105C08G73/1067C08G73/1071C08J5/18C08J2379/08
Inventor 刘京妮崔晶孙旭阳陈大为陈雪
Owner CHINA PETROLEUM & CHEM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products