CN107916461A - 静电纺丝法制备聚丙烯腈‑n,n‑二甲基甲酰胺纤维的方法 - Google Patents

静电纺丝法制备聚丙烯腈‑n,n‑二甲基甲酰胺纤维的方法 Download PDF

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CN107916461A
CN107916461A CN201711190415.XA CN201711190415A CN107916461A CN 107916461 A CN107916461 A CN 107916461A CN 201711190415 A CN201711190415 A CN 201711190415A CN 107916461 A CN107916461 A CN 107916461A
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fiber
dimethylformamide
electrostatic spinning
syringe
polyacrylonitrile
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王耀斌
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Shaanxi Shengmai Petroleum Co Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/02Preparation of spinning solutions
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/003Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/54Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

本发明涉及合成纤维工业技术领域,具体涉及一种静电纺丝法制备聚丙烯腈‑N,N‑二甲基甲酰胺纤维。一种静电纺丝法制备聚丙烯腈‑N,N‑二甲基甲酰胺纤维的方法,包括如下步骤:(1)电纺液的制备;(2)静电纺丝制备聚丙烯腈‑N,N‑二甲基甲酰胺纤维。本发明制成的聚丙烯腈‑N,N‑二甲基甲酰胺纤维,利用扫描电子显微镜对其微观形态进行观察,直接静电纺丝制备纤维效果要优于凝胶法制备纤维。

Description

静电纺丝法制备聚丙烯腈-N,N-二甲基甲酰胺纤维的方法
技术领域
本发明涉及合成纤维工业技术领域,具体涉及一种静电纺丝法制备聚丙烯腈-N,N-二甲基甲酰胺纤维。
背景技术
静电纺丝这一概念是在上个世纪九十年代提出的。八十多年前,Formalas就发明了一系列专利,研究了一种通过挤压并使用静电力来生产聚合物纤维的实验装置。随着纳米技术的发展,能够连续制备纳米纤维的静电纺技术因其易用性及实用性,又引起了人们的重视,并被大量研究和报道。静电纺丝是使带电荷的溶液或熔体在静电场中流动或变形,经溶剂蒸发或熔体冷却固化得到纤维状物质的一种过程,简称电纺。在电场作用下,针头处的液滴会由球形变为圆锥形(即“泰勒锥”),并从圆锥尖端延展得到纤维细丝。Taylor和Yarin等分别对这个过程进行了理论解释,其中Taylor推出了著名的临界电压公式。
静电纺丝技术在构筑一维纳米结构材料领域已发挥了非常重要的作用,应用静电纺丝技术已经成功的制备出了结构多样的纳米纤维材料。通过不同的制备方法,如改变喷头结构、控制实验条件等,可以获得实心、空心、核-壳结构的超细纤维或是蜘蛛网状结构的二维纤维膜;通过设计不同的收集装置,可以获得单根纤维、纤维束、高度取向纤维或无规取向纤维膜等。
发明内容
本发明旨在针对上述问题,提出一种静电纺丝法制备聚丙烯腈-N,N-二甲基甲酰胺纤维的方法。
本发明的技术方案在于:
一种静电纺丝法制备聚丙烯腈-N,N-二甲基甲酰胺纤维的方法,包括如下步骤:
(1)电纺液的制备:
将N,N-二甲基甲酰胺倒入烧杯中 ,将聚丙烯腈白色粉末倒入烧杯中,加入搅拌子,用保鲜膜和透明胶带进行封口密封, 放入集热式恒温加热磁力搅拌器中进行搅拌,至清澈均一淡黄色溶液为静电纺丝前驱体溶液;
(2)静电纺丝制备聚丙烯腈-N,N-二甲基甲酰胺纤维:
将上述纺丝液装入注射器中,将注射器安置在微量注射泵上,调节注射器喷射速率,将铝箔固定在接收板上,并放置在距离针头15cm 的位置上;将高压电源的正负电极分别夹在注射器的枕头和铝箔纸上,打开高压电源,开始纺丝。
所述的集热式恒温加热磁力搅拌器的工艺参数为:水浴温度为75℃,水浴磁力加热搅拌12h,磁力搅拌速率为20r/s。
所述的注射器的尺寸为内径为20mm,针管直径为0.11mm、体积为20ml。
所述的高压电源具体设置为22kV、25kV以及29kV。
所述的注射器喷射速率为3ml/h。
本发明的技术效果在于:
本发明制成的聚丙烯腈-N,N-二甲基甲酰胺纤维,利用扫描电子显微镜对其微观形态进行观察,直接静电纺丝制备纤维效果要优于凝胶法制备纤维。
具体实施方式
一种静电纺丝法制备聚丙烯腈-N,N-二甲基甲酰胺纤维的方法,包括如下步骤:
(1)电纺液的制备:
将N,N-二甲基甲酰胺倒入烧杯中 ,将聚丙烯腈 白色粉末倒入烧杯中,加入搅拌子,用保鲜膜和透明胶带进行封口密封, 放入集热式恒温加热磁力搅拌器中进行搅拌,至清澈均一淡黄色溶液为静电纺丝前驱体溶液;
(2)静电纺丝制备聚丙烯腈-N,N-二甲基甲酰胺纤维:
将上述纺丝液装入注射器中,将注射器安置在微量注射泵上,调节注射器喷射速率,将铝箔固定在接收板上,并放置在距离针头15cm 的位置上;将高压电源的正负电极分别夹在注射器的枕头和铝箔纸上,打开高压电源,开始纺丝。
其中,所述的集热式恒温加热磁力搅拌器的工艺参数为:水浴温度为75℃,水浴磁力加热搅拌12h,磁力搅拌速率为20r/s。所述的注射器的尺寸为内径为20mm,针管直径为0.11mm、体积为20ml。所述的高压电源具体设置为22kV、25kV以及29kV。所述的注射器喷射速率为3ml/h。

Claims (5)

1.一种静电纺丝法制备聚丙烯腈-N,N-二甲基甲酰胺纤维的方法,其特征在于:包括如下步骤:
(1)电纺液的制备:
将N,N-二甲基甲酰胺倒入烧杯中 ,将聚丙烯腈 白色粉末倒入烧杯中,加入搅拌子,用保鲜膜和透明胶带进行封口密封, 放入集热式恒温加热磁力搅拌器中进行搅拌,至清澈均一淡黄色溶液为静电纺丝前驱体溶液;
(2)静电纺丝制备聚丙烯腈-N,N-二甲基甲酰胺纤维:
将上述纺丝液装入注射器中,将注射器安置在微量注射泵上,调节注射器喷射速率,将铝箔固定在接收板上,并放置在距离针头15cm 的位置上;将高压电源的正负电极分别夹在注射器的枕头和铝箔纸上,打开高压电源,开始纺丝。
2.根据权利要求1所述的静电纺丝法制备聚丙烯腈-N,N-二甲基甲酰胺纤维的方法,其特征在于:所述的集热式恒温加热磁力搅拌器的工艺参数为:水浴温度为75℃,水浴磁力加热搅拌12h,磁力搅拌速率为20r/s。
3.根据权利要求2所述的静电纺丝法制备聚丙烯腈-N,N-二甲基甲酰胺纤维的方法,其特征在于:所述的注射器的尺寸为内径为20mm,针管直径为0.11mm、体积为20ml。
4.根据权利要求3所述的静电纺丝法制备聚丙烯腈-N,N-二甲基甲酰胺纤维的方法,其特征在于:所述的高压电源具体设置为22kV、25kV以及29kV。
5.根据权利要求4所述的静电纺丝法制备聚丙烯腈-N,N-二甲基甲酰胺纤维的方法,其特征在于:所述的注射器喷射速率为3ml/h。
CN201711190415.XA 2017-11-24 2017-11-24 静电纺丝法制备聚丙烯腈‑n,n‑二甲基甲酰胺纤维的方法 Withdrawn CN107916461A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110158164A (zh) * 2019-05-23 2019-08-23 天津工业大学 聚丙烯腈纳米纤维膜及其制备方法、柔性压电纳米发电机及其制备方法
CN115012070A (zh) * 2022-04-20 2022-09-06 贵州民族大学 一种黑磷纤维的制备方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110158164A (zh) * 2019-05-23 2019-08-23 天津工业大学 聚丙烯腈纳米纤维膜及其制备方法、柔性压电纳米发电机及其制备方法
CN110158164B (zh) * 2019-05-23 2020-11-03 天津工业大学 聚丙烯腈纳米纤维膜及其制备方法、柔性压电纳米发电机及其制备方法
CN115012070A (zh) * 2022-04-20 2022-09-06 贵州民族大学 一种黑磷纤维的制备方法

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Application publication date: 20180417