CN108193314A - A kind of polypyrrole conductive fiber - Google Patents

A kind of polypyrrole conductive fiber Download PDF

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Publication number
CN108193314A
CN108193314A CN201810057314.3A CN201810057314A CN108193314A CN 108193314 A CN108193314 A CN 108193314A CN 201810057314 A CN201810057314 A CN 201810057314A CN 108193314 A CN108193314 A CN 108193314A
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Prior art keywords
polypyrrole
added
stirred
taken
insulated
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CN201810057314.3A
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Chinese (zh)
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王家浩
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Individual
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Priority to CN201810057314.3A priority Critical patent/CN108193314A/en
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    • 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
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/08Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular 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
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/0605Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
    • C08G73/0611Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
    • 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
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • 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
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/16Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent

Abstract

The invention discloses a kind of polypyrrole conductive fibers, it is made of the raw material of following weight parts:Oleic acid 24, ammonium molybdate 12, aminopropyl triethoxysilane 0.7 1, triazole monomer 20 30, dibenzoyl peroxide 0.7 1,2,6 di-tert-butyl p-cresol 0.6 1, blanc fixe 46, polyacrylonitrile 70 80, isopropanol 57.The triazole monomer of the present invention polymerize in amino alcoholic solution, obtained amino polypyrrole solution and oil acidification filler are blended, by reacting for amino and oleic acid, realize polypyrrole, filler it is effective compatible, so as to improve the mechanical stability of finished-product material and conductive stability.

Description

A kind of polypyrrole conductive fiber
Technical field
The invention belongs to fiber arts, and in particular to a kind of polypyrrole conductive fiber.
Background technology
Polypyrrole is common black, insoluble, molten, conductive polymer, polypyrrole are not aoxidized usually poly- by pyrrole monomer Conjunction obtains, and electrochemical anodic oxidation pyrroles is also the effective means for preparing polypyrrole;Polypyrrole can be used for biology, ion detection, The electrode material of the modified electrode of electrochemical capacitance and antistatic material and photoelectrochemical cell, accumulator.Further, it is also possible to as electricity Magnetic shielding material and gas separation membrane material, for electrolytic capacitor, electro-catalysis, conducting polymer composite material etc., application range It is very wide, the concern of people has been constantly subjected to since being found;
However the stability and poor mechanical property of electric polypyrrole material, in order to improve the performance of polypyrrole, greatly Quantity research person by sight concentrate on polypyrrole and other materials it is compound on, it is compound wide with the carbon materials such as carbon nanotube in recent years General expansion, result of study shows the compound performance that can significantly improve ultracapacitor with carbon nanotube, however carbon is received Mitron has the shortcomings such as of high cost, specific capacitance is low, therefore how to improve the stability_intensity of polypyrrole and mechanical property is to grind at present The emphasis studied carefully.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of polypyrrole conductive fibers.
To achieve the above object, the present invention uses following technical scheme:
A kind of polypyrrole conductive fiber, it is made of the raw material of following weight parts:
Oleic acid 2-4, ammonium molybdate 1-2, aminopropyl triethoxysilane 0.7-1, triazole monomer 20-30, diphenyl peroxide first Acyl 0.7-1, DBPC 2,6 ditertiary butyl p cresol 0.6-1, blanc fixe 4-6, polyacrylonitrile 70-80, isopropanol 5-7.
A kind of polypyrrole conductive fiber, what the triazole monomer was made of the raw material of following weight parts:
1H-1,2,3- triazoles 1-2, pyrroles 35-40, diisopropyl ethanolamine 1-2;
The preparation method of the triazole monomer, includes the following steps:
Take diisopropyl ethanolamine, be added in the deionized water of 10-14 times of its weight, stir evenly, add in 1H-1,2, 3- triazoles, raising temperature are 50-60 DEG C, add in pyrroles, are sent in reaction kettle, are passed through nitrogen, adjust temperature of reaction kettle and are 100-105 DEG C, insulated and stirred to water is done, and discharging cooling obtains the triazole monomer.
A kind of preparation method of polypyrrole conductive fiber, includes the following steps:
(1) 2,6-di-tert-butyl p-cresol is taken, is added in the absolute ethyl alcohol of 10-14 times of its weight, stirs evenly, is added in Aminopropyl triethoxysilane, raising temperature is 50-60 DEG C, and insulated and stirred 20-30 minutes obtains amino alcoholic solution;
(2) dibenzoyl peroxide is taken, is added in isopropanol, is stirred evenly;
(3) triazole monomer is taken, is added in above-mentioned amino alcoholic solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen Gas, it is 70-75 DEG C to adjust temperature of reaction kettle, adds in the aqueous isopropanol of above-mentioned dibenzoyl peroxide, and insulated and stirred 4-5 is small When, discharging obtains amino polypyrrole solution;
(4) blanc fixe, ammonium molybdate mixing are taken, is added in the deionized water of 3-5 times of mixture weight, adds in oleic acid, Insulated and stirred 1-2 hours at 60-65 DEG C, oil acidification solution is obtained;
(5) above-mentioned amino polypyrrole solution, the mixing of oil acidification solution, insulated and stirred 2-3 hours at 70-75 DEG C, mistake are taken Filter, precipitation is washed, and air drying obtains filler modified polypyrrole;
(6) filler modified polypyrrole is taken, mixes, stirs evenly with polyacrylonitrile and its each raw material, is added to mixture weight In 30-40 times of dimethylformamide of amount, melt spinning to get.
Advantages of the present invention:
For the present invention with 1H-1,2,3- triazoles are dopant, right using the aqueous solution of diisopropyl ethanolamine as reaction dissolvent Pyrrole monomer is doped modification, can effectively improve the conductive stability of finished product polypyrrole, triazole monomer of the invention It polymerize in amino alcoholic solution, obtained amino polypyrrole solution and oil acidification filler is blended, passes through amino and oleic acid Reaction, realize polypyrrole, filler it is effective compatible, so as to improve the mechanical stability of finished-product material and conductive stability.
Specific embodiment
Embodiment 1
A kind of polypyrrole conductive fiber, it is made of the raw material of following weight parts:
Oleic acid 4, ammonium molybdate 2, aminopropyl triethoxysilane 1, triazole monomer 30, dibenzoyl peroxide 1, bis- uncles of 2,6- Butyl paracresol 1, blanc fixe 6, polyacrylonitrile 80, isopropanol 7.
A kind of polypyrrole conductive fiber, what the triazole monomer was made of the raw material of following weight parts:
1H-1,2,3- triazoles 2, pyrroles 40, diisopropyl ethanolamine 2;
The preparation method of the triazole monomer, includes the following steps:
Take diisopropyl ethanolamine, be added in the deionized water of 14 times of its weight, stir evenly, add in 1H-1,2,3- Triazole, raising temperature are 60 DEG C, add in pyrroles, are sent in reaction kettle, are passed through nitrogen, and it is 105 DEG C to adjust temperature of reaction kettle, Insulated and stirred to water is done, and discharging cooling obtains the triazole monomer.
A kind of preparation method of polypyrrole conductive fiber, includes the following steps:
(1) 2,6-di-tert-butyl p-cresol is taken, is added in the absolute ethyl alcohol of 14 times of its weight, stirs evenly, adds in ammonia Propyl-triethoxysilicane, raising temperature is 60 DEG C, and insulated and stirred 30 minutes obtains amino alcoholic solution;
(2) dibenzoyl peroxide is taken, is added in isopropanol, is stirred evenly;
(3) triazole monomer is taken, is added in above-mentioned amino alcoholic solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen Gas, it is 75 DEG C to adjust temperature of reaction kettle, adds in the aqueous isopropanol of above-mentioned dibenzoyl peroxide, and insulated and stirred 5 hours goes out Material, obtains amino polypyrrole solution;
(4) blanc fixe, ammonium molybdate mixing are taken, is added in the deionized water of 5 times of mixture weight, adds in oleic acid, Insulated and stirred 2 hours at 65 DEG C, obtain oil acidification solution;
(5) above-mentioned amino polypyrrole solution, the mixing of oil acidification solution are taken, insulated and stirred 3 hours at 75 DEG C are filtered, will Precipitation washing, air drying obtain filler modified polypyrrole;
(6) filler modified polypyrrole is taken, mixes, stirs evenly with polyacrylonitrile and its each raw material, is added to mixture weight In 40 times of dimethylformamide of amount, melt spinning to get.
Embodiment 2
A kind of polypyrrole conductive fiber, it is made of the raw material of following weight parts:
Oleic acid 2, ammonium molybdate 1, aminopropyl triethoxysilane 0.7, triazole monomer 20, dibenzoyl peroxide 0.7,2,6- Di-tert-butyl p-cresol 0.6, blanc fixe 4, polyacrylonitrile 70, isopropanol 5.
A kind of polypyrrole conductive fiber, what the triazole monomer was made of the raw material of following weight parts:
1H-1,2,3- triazoles 1, pyrroles 35, diisopropyl ethanolamine 1;
The preparation method of the triazole monomer, includes the following steps:
Take diisopropyl ethanolamine, be added in the deionized water of 10 times of its weight, stir evenly, add in 1H-1,2,3- Triazole, raising temperature are 50 DEG C, add in pyrroles, are sent in reaction kettle, are passed through nitrogen, and it is 100 DEG C to adjust temperature of reaction kettle, Insulated and stirred to water is done, and discharging cooling obtains the triazole monomer.
A kind of preparation method of polypyrrole conductive fiber, includes the following steps:
(1) 2,6-di-tert-butyl p-cresol is taken, is added in the absolute ethyl alcohol of 10 times of its weight, stirs evenly, adds in ammonia Propyl-triethoxysilicane, raising temperature is 50 DEG C, and insulated and stirred 20 minutes obtains amino alcoholic solution;
(2) dibenzoyl peroxide is taken, is added in isopropanol, is stirred evenly;
(3) triazole monomer is taken, is added in above-mentioned amino alcoholic solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen Gas, it is 70 DEG C to adjust temperature of reaction kettle, adds in the aqueous isopropanol of above-mentioned dibenzoyl peroxide, and insulated and stirred 4 hours goes out Material, obtains amino polypyrrole solution;
(4) blanc fixe, ammonium molybdate mixing are taken, is added in the deionized water of 3 times of mixture weight, adds in oleic acid, Insulated and stirred 1 hour at 60 DEG C, obtains oil acidification solution;
(5) above-mentioned amino polypyrrole solution, the mixing of oil acidification solution are taken, insulated and stirred 2 hours at 70 DEG C are filtered, will Precipitation washing, air drying obtain filler modified polypyrrole;
(6) filler modified polypyrrole is taken, mixes, stirs evenly with polyacrylonitrile and its each raw material, is added to mixture weight In 30 times of dimethylformamide of amount, melt spinning to get.
Performance test:
The polypyrrole conductive fiber of the embodiment of the present invention 1:
Charge-discharge test is carried out, the specific capacitance under the conditions of 0.2A/g charge and discharge is 230.4F/g;Tensile strength is 117.2MPa;
The polypyrrole conductive fiber of the embodiment of the present invention 2:
Charge-discharge test is carried out, the specific capacitance under the conditions of 0.2A/g charge and discharge is 226.1F/g;Tensile strength 115.7MPa;
Commercially available pure polypyrrole:
Charge-discharge test is carried out, the specific capacitance under the conditions of 0.2A/g charge and discharge is 114F/g;Tensile strength is 90.3MPa;As can be seen that the composite material of the present invention has better conductive stability and mechanical property, comprehensive performance is superior.

Claims (3)

1. a kind of polypyrrole conductive fiber, which is characterized in that it is made of the raw material of following weight parts:
Oleic acid 2-4, ammonium molybdate 1-2, aminopropyl triethoxysilane 0.7-1, triazole monomer 20-30, dibenzoyl peroxide 0.7-1, DBPC 2,6 ditertiary butyl p cresol 0.6-1, blanc fixe 4-6, polyacrylonitrile 70-80, isopropanol 5-7.
2. a kind of polypyrrole conductive fiber according to claim 1, which is characterized in that the triazole monomer is by following The raw material composition of parts by weight:
1H-1,2,3- triazoles 1-2, pyrroles 35-40, diisopropyl ethanolamine 1-2;
The preparation method of the triazole monomer, includes the following steps:
Take diisopropyl ethanolamine, be added in the deionized water of 10-14 times of its weight, stir evenly, add in 1H-1,2,3- tri- Nitrogen azoles, raising temperature are 50-60 DEG C, add in pyrroles, are sent in reaction kettle, are passed through nitrogen, and adjusting temperature of reaction kettle is 100- 105 DEG C, insulated and stirred to water is done, and discharging cooling obtains the triazole monomer.
3. the preparation method of a kind of polypyrrole conductive fiber as described in claim 1-2, which is characterized in that including following step Suddenly:
(1) 2,6-di-tert-butyl p-cresol is taken, is added in the absolute ethyl alcohol of 10-14 times of its weight, stirs evenly, adds in ammonia third Ethyl triethoxy silicane alkane, raising temperature is 50-60 DEG C, and insulated and stirred 20-30 minutes obtains amino alcoholic solution;
(2) dibenzoyl peroxide is taken, is added in isopropanol, is stirred evenly;
(3) triazole monomer is taken, is added in above-mentioned amino alcoholic solution, stirs evenly, be sent in reaction kettle, be passed through nitrogen, is adjusted It is 70-75 DEG C to save temperature of reaction kettle, adds in the aqueous isopropanol of above-mentioned dibenzoyl peroxide, and insulated and stirred 4-5 hours goes out Material, obtains amino polypyrrole solution;
(4) blanc fixe, ammonium molybdate mixing are taken, is added in the deionized water of 3-5 times of mixture weight, oleic acid is added in, in 60- Insulated and stirred 1-2 hours at 65 DEG C, oil acidification solution is obtained;
(5) above-mentioned amino polypyrrole solution, the mixing of oil acidification solution are taken, insulated and stirred 2-3 hours at 70-75 DEG C, is filtered, it will Precipitation washing, air drying obtain filler modified polypyrrole;
(6) filler modified polypyrrole is taken, mixes, stirs evenly with polyacrylonitrile and its each raw material, is added to mixture weight 30- In 40 times of dimethylformamide, melt spinning to get.
CN201810057314.3A 2018-01-22 2018-01-22 A kind of polypyrrole conductive fiber Pending CN108193314A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109265590A (en) * 2018-07-11 2019-01-25 桐城市新瑞建筑工程有限公司 A kind of conductive fiber microballoon and preparation method thereof
CN112064165A (en) * 2020-09-02 2020-12-11 满遵连 Antistatic textile fabric and preparation method thereof

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CN107501932A (en) * 2017-09-04 2017-12-22 苏州宇希新材料科技有限公司 A kind of preparation method of lightweight polypyrrole material

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109265590A (en) * 2018-07-11 2019-01-25 桐城市新瑞建筑工程有限公司 A kind of conductive fiber microballoon and preparation method thereof
CN112064165A (en) * 2020-09-02 2020-12-11 满遵连 Antistatic textile fabric and preparation method thereof
CN112064165B (en) * 2020-09-02 2021-11-02 昱天(上海)新材料有限公司 Antistatic textile fabric and preparation method thereof

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Application publication date: 20180622