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Polyamic acid raw solution, preparation method and applications thereof

A technology of polyamic acid and solution, applied in the field of polyamic acid stock solution and its preparation and application, can solve the problems of difficult to control product quality decline, narrow molecular weight distribution of polyamic acid stock solution, low content of gel particles, etc. , The effect of narrow component distribution and less gel particles

Active Publication Date: 2019-04-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] One of the technical problems to be solved by the present invention is that in the prior art, the polyamic acid stock solution is not uniform and the process process caused by many gel particles is difficult to control the decline in product quality. A polyamic acid stock solution is provided. The molecular weight distribution of the amic acid stock solution is narrow and the gel particle content is very low, which is easy to control stably in the subsequent processing process, and the product is not easy to produce defects, and high-performance polyimide products can be obtained

Method used

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  • Polyamic acid raw solution, preparation method and applications thereof
  • Polyamic acid raw solution, preparation method and applications thereof
  • Polyamic acid raw solution, preparation method and applications thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Dissolve 24.03g (120mmol) diphenyl ether diamine (ODA) in 283.62g N,N-dimethylacetamide (water content 180ppmw), at 25°C N 2 Stir under protection, after completely dissolving, add 26.02g (119.28mmol) pyromellitic dianhydride (PMDA) at a speed of 0.5g / min, and continue at 25°C N 2 Stir for 1 h under protection at a stirring speed of 250 rpm, and a uniform transparent viscous polyamic acid solution is obtained. After testing, the polyamic acid solution has an apparent viscosity of 290Pa·s, a number-average molecular weight of 202,000, and a molecular weight distribution of 1.38 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 is generated.

Embodiment 2

[0059] Dissolve 20.02g (100mmol) of diphenyl ether diamine (ODA) in 238.28g of N,N-dimethylacetamide (water content 350ppmw), at 0℃N 2 Stir under protection, after completely dissolving, add 22.03g (101mmol) pyromellitic dianhydride (PMDA) at a speed of 0.1g / min, and continue at 0°C N 2 Stir for 1 h under protection at a stirring speed of 200 rpm to obtain a uniform transparent viscous polyamic acid solution. After testing, the polyamic acid solution has an apparent viscosity of 210Pa·s, a number average molecular weight of 223000, 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 is produced.

Embodiment 3

[0061] Dissolve 24.03g (120mmol) diphenyl ether diamine (ODA) in 283.62g N,N-dimethylformamide (water content 460ppmw), at 20°C N 2 Stir under protection, after completely dissolving, add 26.02g (119.28mmol) pyromellitic dianhydride (PMDA) at a speed of 0.85g / min, and continue at 20°C 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 70 Pa s, a number average molecular weight of 181,000, and a molecular weight distribution of 1.20 at 25°C. After the solution is passed through a 2 μm glass fiber filter membrane, the filter screen is exposed to ultraviolet fluorescent lamps. No foreign matter is produced.

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Abstract

The invention provides a polyamic acid raw solution, a preparation method and applications thereof. In the prior art, the polyamic acid raw solution is non-uniform, and has more gel particles, such that the process is not easily controlled, and the quality of the product is reduced. A purpose of the present invention is mainly to solve the problems in the prior art. According to the technical scheme, a polyamic acid solution is provided, and is characterized in that (a) the gel permeation chromatography determination results show that the molecular weight distribution of the polyamic acid is 1.2-1.5, and (b) after the solution is filtered with a 2 [mu]m glass fiber filtering membrane, no foreign matter is generated by irradiating the filtering screen under an ultraviolet fluorescent lamp.With the technical scheme, the problems in the prior art are well solved. The product of the present invention can be used in the industrial production of polyimide materials.

Description

technical field [0001] The invention relates to a polyamic acid solution with narrow molecular weight distribution and homogenization, its preparation method and application. Background technique [0002] Polyimide is a kind of polymer with excellent comprehensive performance, which has excellent heat resistance, low temperature resistance, self-lubrication, radiation resistance and flame retardancy, as well as excellent mechanical properties and dielectric properties . [0003] The main chain of ordinary polyimide contains a large number of imide ring structures. Due to the electronic polarization and crystallinity, there is a strong force between the polyimide molecular chains, which makes the polyimide molecular chains tightly packed. As a result, it is insoluble and infusible and difficult to process and shape, which seriously affects its application value. In order to solve the solubility problem, the precursor of polyimide-polyamic acid solution is usually synthesize...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J5/18C08L79/08D01F6/74
CPCC08G73/1071C08J5/18C08J2379/08D01F6/74
Inventor 崔晶孙旭阳陈雪刘京妮陈大为
Owner CHINA PETROLEUM & CHEM CORP
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