WO2017214742A1 - 一种聚酰胺酸磁性纳米复合纤维的制备方法 - Google Patents

一种聚酰胺酸磁性纳米复合纤维的制备方法 Download PDF

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WO2017214742A1
WO2017214742A1 PCT/CN2016/000326 CN2016000326W WO2017214742A1 WO 2017214742 A1 WO2017214742 A1 WO 2017214742A1 CN 2016000326 W CN2016000326 W CN 2016000326W WO 2017214742 A1 WO2017214742 A1 WO 2017214742A1
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polyamic acid
diaminodiphenyl ether
polyamide acid
mixed solution
pyromellitic anhydride
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PCT/CN2016/000326
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English (en)
French (fr)
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杨磊
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杨磊
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
    • C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products

Definitions

  • the invention relates to the technical field of preparation of polyamic acid, in particular to a preparation process of a polyamic acid magnetic nano composite fiber.
  • Polyamide commonly known as nylon (Nylon), is a generic term for polymers containing amide groups in the repeating units of macromolecular backbones.
  • the polyamic acid can be obtained by ring-opening polymerization of a caprolactam, or the polyamic acid obtained by polycondensation of a diamine and a dibasic acid, etc., which is a kind of free shuttle group derived from an aromatic diamine and an aromatic amine.
  • the linear polymer with the main chain of acid amine structure has good comprehensive properties, including mechanical properties, heat resistance, abrasion resistance, chemical resistance and self-lubricity, and has low friction coefficient and certain resistance. It is flammable, easy to process, and can be restored to its original shape after being pulled.
  • the present invention provides a preparation process of a polyamic acid magnetic nanocomposite fiber, which is obtained by combining a polyamic acid with Fe 3 O 4 to obtain a magnetic nanocomposite fiber, which has good electrical conductivity and is easy to obtain raw materials;
  • the fiber length can be freely controlled, and the strength is large and the gas permeability is good, which can effectively solve the problems in the background art.
  • a preparation process of a polyamic acid magnetic nano composite fiber comprising the following steps:
  • the pyromellitic anhydride and diaminodiphenyl ether are weighed according to the molar mass ratio, the pyromellitic anhydride is 40g-50g, the diaminodiphenyl ether is 80g-100g;
  • the receiving plate is covered with a layer of aluminum foil receiving plate and connected to the other pole of the high voltage power supply, the distance between the spinneret and the collecting plate is adjusted, the spinning time is set, the power is turned on, and the spinning is started.
  • the pyromellitic anhydride and the diaminodiphenyl ether are all chemically pure.
  • the N,N-dimethylacetamide and the nano Fe 3 O 4 are of analytical grade.
  • the diaminodiphenyl ether in the step (4) is added to the three-necked bottle five times, and the amount of each addition is equal, and each is 20 g to 25 g.
  • the metal needle of the syringe has a model number of 12 # and 15 cm.
  • the distance between the spinneret and the collecting plate in the step (7) is 16-18 cm, and the spinning time is 5 h-6 h.
  • the invention combines polyamic acid with Fe 3 O 4 to obtain magnetic nano-composite fiber, has good electrical conductivity, and the raw material is simple and easy to obtain; the generated fiber length can be adjusted by adjusting the distance between the spinneret and the distance between the collecting plates. Fibers of different lengths are obtained, and the length of the fiber can be freely controlled to meet different needs; the fiber produced by the invention has high strength and good gas permeability, and the joint is smooth and not easy to break.
  • a preparation process of a polyamic acid magnetic nano composite fiber comprising the following steps:
  • the pyromellitic anhydride and diaminodiphenyl ether are weighed according to the molar mass ratio, the tetrazoic acid anhydride is 45 g, and the diaminodiphenyl ether is 90 g;
  • the diaminodiphenyl ether is gradually added to the mixed solution several times to obtain a polyamic acid solution
  • the receiving plate is covered with a layer of aluminum foil receiving plate and connected to the other pole of the high voltage power supply, the distance between the spinneret and the collecting plate is adjusted, the spinning time is set, the power is turned on, and the spinning is started.
  • the pyromellitic anhydride and the diaminodiphenyl ether are all chemically pure.
  • the N,N-dimethylacetamide and the nano Fe 3 O 4 are of analytical grade.
  • the diaminodiphenyl ether in the step (4) is added to the three-necked bottle 5 times, and the amount of each addition is equal, both being 18 g.
  • the metal needle of the syringe has a model number of 12 # and 15 cm.
  • the distance between the spinneret and the collecting plate in the step (7) is 16-18 cm, and the spinning time is 5 h-6 h.
  • a preparation process of a polyamic acid magnetic nano composite fiber comprising the following steps:
  • the pyromellitic anhydride and diaminodiphenyl ether are weighed according to the molar mass ratio, the pyromellitic anhydride is 40g-50g, the diaminodiphenyl ether is 80g-100g;
  • the diaminodiphenyl ether is gradually added to the mixed solution several times to obtain a polyamic acid solution
  • the receiving plate is covered with a layer of aluminum foil receiving plate and connected to the other pole of the high voltage power supply, the distance between the spinneret and the collecting plate is adjusted, the spinning time is set, the power is turned on, and the spinning is started.
  • the pyromellitic anhydride and the diaminodiphenyl ether are all chemically pure.
  • the N, N- dimethylacetamide and Fe 3 O 4 nano analytical grade According to the above aspect, the N, N- dimethylacetamide and Fe 3 O 4 nano analytical grade.
  • the diaminodiphenyl ether in the step (4) is added to the three-necked bottle five times, and the amount of each addition is equal, and each is 20 g to 25 g.
  • the metal needle of the syringe has a model number of 12 # and 15 cm.
  • the distance between the spinneret and the collecting plate in the step (7) is 17 cm, and the spinning time is 5.5.
  • a preparation process of a polyamic acid magnetic nano composite fiber comprising the following steps:
  • the pyromellitic anhydride and diaminodiphenyl ether are weighed in a molar ratio, the pyromellitic anhydride is 40g-50g, and the diaminodiphenyl ether is 80g-100g;
  • the diaminodiphenyl ether is gradually added to the mixed solution several times to obtain a polyamic acid solution
  • the receiving plate is covered with a layer of aluminum foil receiving plate and connected to the other pole of the high voltage power supply, the distance between the spinneret and the collecting plate is adjusted, the spinning time is set, the power is turned on, and the spinning is started.
  • the pyromellitic anhydride and the diaminodiphenyl ether are all chemically pure.
  • the N,N-dimethylacetamide and the nano Fe 3 O 4 are of analytical grade.
  • the diaminodiphenyl ether in the step (4) is added to the three-necked bottle five times, and the amount of each addition is equal, and each is 20 g to 25 g.
  • the temperature of the water bath heating in the step (2) is 45 °C.
  • the distance between the spinneret and the collecting plate in the step (7) is 17 cm, and the spinning time is 6 h.
  • an advantage of the present invention is that the present invention combines a polyamic acid with Fe 3 O 4 to obtain a magnetic nanocomposite fiber, which has good electrical conductivity, and the raw material is simple and easy to obtain; the length of the produced fiber can be adjusted by adjusting the spinneret and collecting The distance between the distances between the plates is obtained to obtain fibers of different lengths, and the length of the fibers can be freely controlled to meet different needs; the fibers obtained by the invention have high strength and good gas permeability, and the joints are smooth and not easy to break.

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

Abstract

一种聚酰胺酸磁性纳米复合纤维的制备方法，包括如下步骤：在10摄氏度以下，将均苯四甲酸酐与二氨基二苯醚按照摩尔质量等比例称重，在250ml的三口瓶中加入称好的均苯四甲酸酐，并加入12g-15g的N，N-二甲基甲酰胺，通入保护氮气；均苯四甲酸酐完全溶解后，将二氨基二苯醚分5次逐步加入到混合液中，得到聚酰胺酸溶液；在聚酰胺酸溶液中加入16g-20g的纳米Fe 3O 4颗粒，并利用搅拌棒不断搅拌，得到黑色粘稠状的聚酰胺酸/Fe 3O 4混合溶液；将得到的聚酰胺酸/Fe 3O 4混合溶液分次装入20ml的注射器中，固定于高压静电纺丝装置上，注射器的金属针头与高压电源的一极相连；在接收板上覆上一层铝箔，接收板与高压电源的另一极相连，调整喷丝头与接收板之间的距离，并设置纺丝时间，打开电源进行纺丝。

Description

一种聚酰胺酸磁性纳米复合纤维的制备工艺 技术领域
本发明涉及聚酰胺酸制备技术领域，具体涉及一种聚酰胺酸磁性纳米复合纤维的制备工艺。
背景技术
聚酰胺俗称尼龙(Nylon)，它是大分子主链重复单元中含有酰胺基团的高聚物的总称。聚酰胺酸可由内酸胺开环聚合制得，也可由二元胺与二元酸缩聚等得到的聚酰胺酸是由芳族二元胺与芳族缩胺而成的一类含游离梭基、主链为酸胺结构的线型聚合物，具有良好的综合性能，包括力学性能、耐热性、耐磨损性、耐化学药品性和自润滑性，且摩擦系数低，有一定的阻燃性，易于加工，在被拉扯后可恢复原形，可洗、快干、吸水少、防虫，是一种制作手套的常见材料。但普通的手套仅用普通的聚酯胺制成，没有导电性能，对于现在习惯使用智能手机的用户来说，冬天带上手套时因为手套不能导电，传递人体电流，隔着手套就无法进行操作，必须脱掉手套忍受寒冷进行操作。
发明内容
针对以上问题，本发明提供了一种聚酰胺酸磁性纳米复合纤维的制备工艺，将聚酰胺酸与Fe3O4复合得到磁性纳米复合纤维，具有良好的导电性能，原料简单易得；产生的纤维长度可以自由控制，且强度大透气性好，可以有效解决背景技术中的问题。
为了实现上述目的，本发明采用的技术方案如下：一种聚酰胺酸磁性纳米复合纤维的制备工艺，包括如下步骤：
(1)在10摄氏度以下，将均苯四甲酸酐与二氨基二苯醚按照摩尔质量等比例称重，均苯四甲酸酐为40g-50g，二氨基二苯醚为80g-100g；
(2)在250ml的三口瓶中，加入步骤(1)中称好的均苯四甲酸酐，并加入12g-15g的N，N-二甲基甲酰胺；
(3)在三口瓶中通入保护氮气；
(4)均苯四甲酸酐完全溶解后，将二氨基二苯醚分多次逐步加入到混 合液中，得到聚酰胺酸溶液；
(5)在聚酰胺酸溶液中加入16g-20g的纳米Fe3O4颗粒，并利用搅拌棒不断搅拌，得到黑色粘稠状的聚酰胺酸/Fe3O4混合溶液；
(6)将得到的黑色粘稠状的聚酰胺酸/Fe3O4混合溶液分次装入的20ml的注射器中，固定于高压静电纺丝装置上，注射器的金属针头与高压电源的一极相连；
(7)在接收板上覆上一层铝箔接收板与高压电源的另一极相连，调整喷丝头与收集板之间的距离，并设置纺丝时间，打开电源，开始纺丝。
根据上述技术方案，所述均苯四甲酸酐、二氨基二苯醚均为化学纯。
根据上述技术方案，所述N，N-二甲基乙酰胺和纳米Fe3O4为分析纯。
根据上述技术方案，所述步骤(4)中的二氨基二苯醚分5次加入三口瓶中，且每次加入的量相等，均为20g-25g。
根据上述技术方案，所述注射器的金属针头的型号为12#、15cm。
根据上述技术方案，所述步骤(7)中的喷丝头与收集板之间的距离为16-18cm，纺丝时间为5h-6h。
本发明的有益效果：
本发明将聚酰胺酸与Fe3O4复合得到磁性纳米复合纤维，具有良好的导电性能，原料简单易得；产生的纤维长度可以通过调节喷丝头与收集板之间的距离之间的距离得到不同长度的纤维，实现自由控制纤维长度，以适应不同的需要；本发明制取的纤维强度大透气性好，节点光滑不易断裂。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1：
一种聚酰胺酸磁性纳米复合纤维的制备工艺，包括如下步骤：
(1)在10摄氏度以下，将均苯四甲酸酐与二氨基二苯醚按照摩尔质量等比例称重，均苯四甲酸酐为45g，二氨基二苯醚为90g；
(2)在250ml的三口瓶中，加入步骤(1)中称好的均苯四甲酸酐，并加入13g的N，N-二甲基甲酰胺；
(3)在三口瓶中通入保护氮气；
(4)均苯四甲酸酐完全溶解后，将二氨基二苯醚分多次逐步加入到混合液中，得到聚酰胺酸溶液；
(5)在聚酰胺酸溶液中加入17g的纳米Fe3O4颗粒，并利用搅拌棒不断搅拌，得到黑色粘稠状的聚酰胺酸/Fe3O4混合溶液；
(6)将得到的黑色粘稠状的聚酰胺酸/Fe3O4混合溶液分次装入的20ml的注射器中，固定于高压静电纺丝装置上，注射器的金属针头与高压电源的一极相连；
(7)在接收板上覆上一层铝箔接收板与高压电源的另一极相连，调整喷丝头与收集板之间的距离，并设置纺丝时间，打开电源，开始纺丝。
根据上述技术方案，所述均苯四甲酸酐、二氨基二苯醚均为化学纯。
根据上述技术方案，所述N，N-二甲基乙酰胺和纳米Fe3O4为分析纯。
根据上述技术方案，所述步骤(4)中的二氨基二苯醚分5次加入三口瓶中，且每次加入的量相等，均为18g。
根据上述技术方案，所述注射器的金属针头的型号为12#、15cm。
根据上述技术方案，所述步骤(7)中的喷丝头与收集板之间的距离为16-18cm，纺丝时间为5h-6h。
实施例2：
一种聚酰胺酸磁性纳米复合纤维的制备工艺，包括如下步骤：
(1)在10摄氏度以下，将均苯四甲酸酐与二氨基二苯醚按照摩尔质量等比例称重，均苯四甲酸酐为40g-50g，二氨基二苯醚为80g-100g；
(2)在250ml的三口瓶中，加入步骤(1)中称好的均苯四甲酸酐，并加入12g-15g的N，N-二甲基甲酰胺；
(3)在三口瓶中通入保护氮气；
(4)均苯四甲酸酐完全溶解后，将二氨基二苯醚分多次逐步加入到混合液中，得到聚酰胺酸溶液；
(5)在聚酰胺酸溶液中加入18g的纳米Fe3O4颗粒，并利用搅拌棒不断搅拌，得到黑色粘稠状的聚酰胺酸/Fe3O4混合溶液；
(6)将得到的黑色粘稠状的聚酰胺酸/Fe3O4混合溶液分次装入的20ml的注射器中，固定于高压静电纺丝装置上，注射器的金属针头与高压电源的一极相连；
(7)在接收板上覆上一层铝箔接收板与高压电源的另一极相连，调整喷丝头与收集板之间的距离，并设置纺丝时间，打开电源，开始纺丝。
根据上述技术方案，所述均苯四甲酸酐、二氨基二苯醚均为化学纯。
根据上述技术方案，所述N，N-二甲基乙酰胺和纳米Fe3O4为分析纯。
根据上述技术方案，所述步骤(4)中的二氨基二苯醚分5次加入三口瓶中，且每次加入的量相等，均为20g-25g。
根据上述技术方案，所述注射器的金属针头的型号为12#、15cm。
根据上述技术方案，所述步骤(7)中的喷丝头与收集板之间的距离为17cm，纺丝时间为5.5。
实施例3：
一种聚酰胺酸磁性纳米复合纤维的制备工艺，包括如下步骤：
((1)在10摄氏度以下，将均苯四甲酸酐与二氨基二苯醚按照摩尔质量等比例称重，均苯四甲酸酐为40g-50g，二氨基二苯醚为80g-100g；
(2)在250ml的三口瓶中，加入步骤(1)中称好的均苯四甲酸酐，并加入12g-15g的N，N-二甲基甲酰胺；
(3)在三口瓶中通入保护氮气；
(4)均苯四甲酸酐完全溶解后，将二氨基二苯醚分多次逐步加入到混合液中，得到聚酰胺酸溶液；
(5)将16g-20g的纳米Fe3O4颗粒在N，N-二甲基甲酰胺溶液中进行超声震荡处理，得到纳米Fe3O4溶液；
(6)在聚酰胺酸溶液中加入步骤(5)中制取的纳米Fe3O4溶液，并利用搅拌棒不断搅拌，得到黑色粘稠状的聚酰胺酸/Fe3O4混合溶液；
(7)将得到的黑色粘稠状的聚酰胺酸/Fe3O4混合溶液分次装入的20ml 的注射器中，固定于高压静电纺丝装置上，注射器的金属针头与高压电源的一极相连；
(8)在接收板上覆上一层铝箔接收板与高压电源的另一极相连，调整喷丝头与收集板之间的距离，并设置纺丝时间，打开电源，开始纺丝。
根据上述技术方案，所述均苯四甲酸酐、二氨基二苯醚均为化学纯。
根据上述技术方案，所述N，N-二甲基乙酰胺和纳米Fe3O4为分析纯。
根据上述技术方案，所述步骤(4)中的二氨基二苯醚分5次加入三口瓶中，且每次加入的量相等，均为20g-25g。
根据上述技术方案，所述步骤(2)中水浴加热的温度为45℃。
根据上述技术方案，所述步骤(7)中的喷丝头与收集板之间的距离为17cm，纺丝时间为6h。
基于上述，本发明的优点在于，本发明将聚酰胺酸与Fe3O4复合得到磁性纳米复合纤维，具有良好的导电性能，原料简单易得；产生的纤维长度可以通过调节喷丝头与收集板之间的距离之间的距离得到不同长度的纤维，实现自由控制纤维长度，以适应不同的需要；本发明制取的纤维强度大透气性好，节点光滑不易断裂。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (6)

  1. 一种聚酰胺酸磁性纳米复合纤维的制备工艺，其特征在于，包括如下步骤：
    (1)在10摄氏度以下，将均苯四甲酸酐与二氨基二苯醚按照摩尔质量等比例称重，均苯四甲酸酐为40g-50g，二氨基二苯醚为80g-100g；
    (2)在250ml的三口瓶中，加入步骤(1)中称好的均苯四甲酸酐，并加入12g-15g的N，N-二甲基甲酰胺；
    (3)在三口瓶中通入保护氮气；
    (4)均苯四甲酸酐完全溶解后，将二氨基二苯醚分多次逐步加入到混合液中，得到聚酰胺酸溶液；
    (5)在聚酰胺酸溶液中加入16g-20g的纳米Fe3O4颗粒，并利用搅拌棒不断搅拌，得到黑色粘稠状的聚酰胺酸/Fe3O4混合溶液；
    (6)将得到的黑色粘稠状的聚酰胺酸/Fe3O4混合溶液分次装入的20ml的注射器中，固定于高压静电纺丝装置上，注射器的金属针头与高压电源的一极相连；
    (7)在接收板上覆上一层铝箔接收板与高压电源的另一极相连，调整喷丝头与收集板之间的距离，并设置纺丝时间，打开电源，开始纺丝。
  2. 根据权利要求1所述的一种聚酰胺酸磁性纳米复合纤维的制备工艺，其特征在于，所述均苯四甲酸酐、二氨基二苯醚均为化学纯。
  3. 根据权利要求1所述的一种聚酰胺酸磁性纳米复合纤维的制备工艺，其特征在于，所述N，N-二甲基乙酰胺和纳米Fe3O4颗粒为分析纯。
  4. 根据权利要求1所述的一种聚酰胺酸磁性纳米复合纤维的制备工艺，其特征在于，所述步骤(4)中的二氨基二苯醚分5次加入三口瓶中，且每次加入的量相等，均为20g-25g。
  5. 根据权利要求2所述的一种聚酰胺酸磁性纳米复合纤维的制备工艺，其特征在于，所述注射器的金属针头的型号为12#、15cm。
  6. 根据权利要求1所述的一种聚酰胺酸磁性纳米复合纤维的制备工艺，其特征在于，所述步骤(7)中的喷丝头与收集板之间的距离为16-18cm，纺丝时间为5h-6h。
PCT/CN2016/000326 2016-06-13 2016-06-22 一种聚酰胺酸磁性纳米复合纤维的制备方法 WO2017214742A1 (zh)

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