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Preparation method of polyimide nanofiber

A technology of polyimide fiber and nanofiber, which is applied in the direction of fiber treatment, fiber chemical characteristics, single-component synthetic polymer rayon, etc. Problems such as poor diameter uniformity of nanofibers, etc., to achieve good technical effects, high spinning efficiency, and good diameter uniformity

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

AI Technical Summary

Problems solved by technology

[0006] The invention mainly solves the problems in the prior art that the polyamic acid solution has a wide molecular weight distribution and many gel particles, which lead to poor uniformity of polyimide nanofiber diameter and easy formation of beads during electrospinning

Method used

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  • Preparation method of polyimide nanofiber
  • Preparation method of polyimide nanofiber
  • Preparation method of polyimide nanofiber

Examples

Experimental program
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Effect test

Embodiment 1

[0036] 1. Stock solution preparation: Dissolve 24.03g (120mmol) of diphenyl ether diamine (ODA) in 281.52g of N,N-dimethylacetamide (water content 180ppmw), at 25℃N 2 Stir under protection, after completely dissolving, add 25.65g (117.6mmol) 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 to obtain prepolymer solution 1. Dissolve 20.02g (100mmol) of diphenyl ether diamine (ODA) in 298.86g of N,N-dimethylacetamide (water content 180ppmw), at 25°C N 2 Stir under the protection, after completely dissolving, add 32.72g (150mmol) pyromellitic dianhydride (PMDA), after the completion of the addition, continue at 25 ℃ N 2 Stir for 1 h under protection at a stirring speed of 250 rpm to obtain prepolymer solution 2. Add 11.81 g of prepolymer solution 2 to prepolymer solution 1 at a rate of 0.5 g / min, and continue stirring for 1 hour to obtain a uniform transparent viscous polyamic acid solut...

Embodiment 2

[0041] Dissolve 20.02g (100mmol) diphenyl ether diamine (ODA) in 224.68g N,N-dimethylacetamide (water content 350ppmw), at 0°C N 2 Stir under protection, after completely dissolving, add 19.63g (90mmol) pyromellitic dianhydride (PMDA) at a speed of 0.1g / min, and continue at 0°C N 2 Stir under protection for 1 h at a stirring speed of 200 rpm to obtain prepolymer solution 1. Dissolve 20.02g (100mmol) of diphenyl ether diamine (ODA) in 267.98g of N,N-dimethylacetamide (water content 180ppmw), at 25°C N 2Stir under the protection, after completely dissolving, add 27.27g (125mmol) pyromellitic dianhydride (PMDA), after adding, continue to 2 Stir for 1 h under protection at a stirring speed of 250 rpm to obtain prepolymer solution 2. Add 34.77g of prepolymer solution 2 to prepolymer solution 1 at a rate of 1 g / min, and continue stirring for 1 hour to obtain a uniform transparent viscous polyamic acid solution. After testing, the polyamic acid solution has an apparent viscosity o...

Embodiment 3

[0045] 1. Stock solution preparation: according to the stock solution preparation process of Example 1.

[0046] 2. Electrospinning: Using needle-free electrospinning technology, the above solution is vacuum degassed after 3 μm filtration and then added to the closed storage tank of the high-voltage electrospinning device. The spinning temperature is room temperature, the humidity is 55%, and the high-pressure The output voltage of the power supply is 40KV, and the distance between the receiving screen and a single electrode is 40cm. The storage tank moves back and forth repeatedly, and the polymer is uniformly coated on the electrode wire, and Taylor-Vibe is generated from the surface of the electrode to produce polyamic acid nanofibers.

[0047] The remaining steps are according to Example 1.

[0048] The obtained polyimide nanofibers have an average diameter of 700 nm, a diameter standard deviation of 15 nm, good uniformity, and no beads appear.

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Abstract

The invention relates to a preparation method of polyimide nanofiber, and mainly aims to solve the problems of poor diameter uniformity of the polyimide nanofiber and tendency to form beads in electrostatic spinning due to wide molecular weight distribution and large quantity of gel particles during preparation of the polyimide nanofiber with a two-step process in the prior art. The preparation method of the polyimide nanofiber comprises the following steps: dissolving X mole of diamine in an organic solvent, and adding Y mole of dianhydride for reacting to obtain a prepolymer solution 1; dissolving Z mole of diamine in an organic solvent, adding K mole of dianhydride for reacting to obtain a prepolymer solution 2; adding the prepolymer solution 2 into the prepolymer solution 1 to obtain apolyamide acid solution; deaerating and filtering the polyamide acid solution, and performing electrostatic spinning and amination to obtain uniform polyimide nanofiber. By adopting the preparation method, the problems are well solved. The preparation method can be applied to the continuous production of the polyimide nanofiber.

Description

technical field [0001] The invention relates to a preparation method of polyimide nanofibers Background technique [0002] As a high-performance engineering plastic, polyimide (PI) is widely used in aerospace, electrical insulation, atomic energy industry, In fields with harsh conditions such as national defense construction, environmental industry, protection industry, medical and health care, etc. [0003] Electrospinning technology is a simple and economical method to prepare fine fibers. The polyimide nanofibers prepared by electrospinning not only retain many excellent properties of polyimide materials, but also have a wide distribution of diameters, and the nanofiber membrane has a large specific surface area, many pores and small pore diameters, and has good properties. Filterability, adsorption, physical (heat, light, electromagnetic, etc.) properties and other advantages. Therefore, PI nanofibrous membranes have potential applications in filtration, electronic ma...

Claims

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Application Information

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IPC IPC(8): D01F6/74C08G73/10D01D1/10D01D5/00
CPCC08G73/1071D01D1/103D01D1/106D01D5/003D01F6/74
Inventor 陈雪崔晶孙旭阳刘京妮陈大为
Owner CHINA PETROLEUM & CHEM CORP
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