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Polyamic acid solution, preparation method and applications thereof

A polyamic acid and amine solution technology, applied in the direction of single-component synthetic polymer rayon, fiber chemical characteristics, textiles and papermaking, etc., can solve the problem of low gel particle content, narrow molecular weight distribution of polyamic acid solution, and difficult control Problems such as product quality decline, to achieve the effect of not being prone to defects, reducing bad spots and defects, and improving quality

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

AI Technical Summary

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 uneven and there are many gel particles, and the technical process is difficult to control the decline in product quality. The molecular weight distribution of the amic acid solution is narrow and the gel particle content is very low, it 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 solution, preparation method and applications thereof
  • Polyamic acid solution, preparation method and applications thereof
  • Polyamic acid solution, preparation method and applications thereof

Examples

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Effect test

Embodiment 1

[0042] Dissolve 23.38g (116.77mmol) of diphenyl ether diamine (ODA) in 273.94g of N,N-dimethylacetamide (DMAc), stir at 25°C, after complete dissolution, add 24.96g (114.43mmol) Perphthalic dianhydride (PMDA), fully reacted to obtain prepolymer solution 1 (dianhydride, diamine molar ratio 0.98, solid content 15%, the same below). Using the same method, 19.41g (96.92mmol) ODA, 289.68g DMAc, and 31.71g (145.38mmol) PMDA were used to prepare prepolymer solution 2 (molar ratio 1.50, solid content 15%). 11.36 g of prepolymer solution 2 was added to prepolymer solution 1 at a rate of 22.0 g / h, and fully stirred at 25° C. to obtain a final polyamic acid solution (molar ratio 0.994, solid content 15%). The apparent viscosity of the final solution was measured to be 290 Pa·s, and the molecular weight distribution was 1.44. After passing the solution through a 2 μm glass fiber filter membrane, the filter screen was irradiated by ultraviolet fluorescent lamps without foreign matter.

Embodiment 2

[0044]Dissolve 2002.4g (10mol) ODA in 23089.0g DMAc, stir at 25°C, after complete dissolution, add 2072.1g (9.5mol) PMDA, and obtain prepolymer solution 1 (molar ratio 0.95, solid content 15 %). In the same way, 1001.2 g (5 mol) ODA, 14944.0 g DMAc, and 1635.9 g (7.5 mol) PMDA were used to prepare prepolymer solution 2 (molar ratio 1.50, solid content 15%). 2757.5 g of prepolymer solution 2 was added to prepolymer solution 1 at a rate of 460 g / h, and fully stirred at 25° C. to obtain a final polyamic acid solution (molar ratio 0.99, solid content 15%). The measured apparent viscosity of the final solution was 248 Pa·s, and the molecular weight distribution was 1.42. After passing the solution through a 2 μm glass fiber filter membrane, the filter screen was irradiated by ultraviolet fluorescent lamps without foreign matter.

Embodiment 3

[0046] Dissolve 2002.4g (10mol) ODA in 27837.0g N-methylpyrrolidone (NMP), stir at 0°C, after completely dissolving, add 1090.6g (5mol) PMDA, and obtain prepolymer solution 1 (mol) after fully reacting Ratio 0.5, solid content 10%). In the same way, 1001.2g (5mol) ODA, 28641.6g NMP, and 2181.2g (10mol) PMDA were used to prepare prepolymer solution 2 (molar ratio 2.0, solid content 10%). Add 31,824.0 g of prepolymer solution 2 to prepolymer solution 1 at a rate of 10,000.0 g / h, and stir thoroughly at 0° C. to obtain a final polyamic acid solution (molar ratio 1, solid content 10%). The measured apparent viscosity of the final solution was 168 Pa·s, and the molecular weight distribution was 1.38. After passing the solution through a 2 μm glass fiber filter membrane, the filter screen was irradiated by ultraviolet fluorescent lamps without foreign matter.

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Abstract

The invention relates to a polyamic acid 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 thatthe 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 comprises a mixed solution of a prepolymer solution 1 and a prepolymer solution 2, wherein the prepolymer solution 1 is obtained by carrying out a reactionon X moles of diamine and Y moles of dianhydride, the prepolymer solution 2 is obtained by carrying out a reaction on Z moles of diamine and K moles of dianhydride, Y / X is more than or equal to 0.5 and is less than or equal to 0.98, and K / Z is more than or equal to 1.02 and is less than or equal to 2.0. With the technical scheme, the problem in the prior art is 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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