CN105884213B - The preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber - Google Patents
The preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber Download PDFInfo
- Publication number
- CN105884213B CN105884213B CN201610211174.1A CN201610211174A CN105884213B CN 105884213 B CN105884213 B CN 105884213B CN 201610211174 A CN201610211174 A CN 201610211174A CN 105884213 B CN105884213 B CN 105884213B
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- Prior art keywords
- glass fibre
- polyethyleneimine
- fiber
- composite conducting
- water
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/26—Macromolecular compounds or prepolymers
- C03C25/28—Macromolecular compounds or prepolymers obtained by reactions involving only carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/42—Coatings containing inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/62—Surface treatment of fibres or filaments made from glass, minerals or slags by application of electric or wave energy; by particle radiation or ion implantation
- C03C25/6293—Plasma or corona discharge
Abstract
The present invention proposes a kind of preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber, and glass fibre is surface-treated using vacuum plasma；The glass fibre of polyethyleneimine surface modification is obtained after in glass fibre immersion aq. polyethyleneimine Jing Guo plasma treatment, after immersion, fully being rinsed, dried with water；The glass fibre of polyethyleneimine surface modification is placed in the cupric sulfate pentahydrate aqueous solution, sodium thiosulfate solution is added after immersion, after reaction take out fiber rinsed with water, dry after obtain cuprous sulfide/glass fibre composite conducting fiber.Electroconductive glass fibre is prepared using the technique of the present invention, device therefor investment cost is low, simple to operate, reaction condition is gentle, the loss of strong applicability, high treating effect, fibre property is few, reliable in quality, and can reduce environmental pollution, suitable for industrialized production.
Description
Technical field
The invention belongs to the post processing field of glass fibre, more particularly to a kind of cuprous sulfide/polyethyleneimine/glass fibers
Tie up the preparation method of composite conducting fiber.
Background technology
In recent years, developing rapidly and popularizing with computer, telecommunications, micro-wave oven etc., in human lives' working environment
Electromagnetic radiation is increasingly serious, thus caused Electromagnetic Interference is to the normal work of electronic equipment and the physiological health of the mankind
Bring many negative effects.To prevent electrostatic interference and Electromagnetic Interference, from 20th century mid-term so far, develop various anti-
The material of electrostatic and electromagnetic shielding.Recent decades, the emphasis of research have more turned to conductive fiber, conductive fiber it is antistatic
Effect is more significantly lasting, and is not influenceed by ambient humidity, after conductive layer reaches certain proportion up to certain thickness or conductive component,
Development and application with excellent electro-magnetic screen function, therefore conductive fiber are increasingly taken seriously.
Glass fibre is a kind of new function material and structural material in inorganic non-metallic material.Due to it have it is non-ignitable
Property, high temperature resistant, anticorrosive, intensity is high, density is small, moisture absorption is low and a series of extension excellent specific properties such as small, be widely used to pass
System industry, agricultural, construction industry and electronics, communication, nuclear energy, Aeronautics and Astronautics, weapons, naval vessels and ocean development, genetic engineering etc.
High and new technology industry, turn into the new and high technology material of the indispensable sustainable development of the 21 century mankind.In recent years, many researchs
Person attempts, by modified glass-fiber the methods of modern chemistry, physics, to prepare electroconductive glass fibre as polymer composite
Conductive filler material, for solving the problems, such as Contamination of Electromagnetic Wave.Chemical plating is as material surface metalized technology,
As preparing one of conventional technology of electroconductive glass fibre, but traditional glass fibre chemistry plating during its plating because needing
Slightly flower, sensitization, activation process, not only complex process, and the heavy metal palladium price needed in activation process is held high are carried out to matrix
Expensive, these all limit the further development that electroless plating method prepares electroconductive glass fibre.Therefore, new, effective prepare is developed
The method of electroconductive glass fibre has great importance.
Metal sulfide all has special performance in optics, optical electro-chemistry, catalysis, environmental protection etc..They have good
Good chemically and thermally stability, is a kind of good photoelectric material.Conductive fiber is produced using the characteristic of metal sulfide
Method is at most fiber surface chemical reaction method in current apply, and this method mainly by chemical treatment, that is, passes through reaction
The dipping of liquid, absorption is produced in fiber surface, then metal sulfide is covered in fiber surface by chemical reaction.The method
Advantage is that technique is simple, cost is relatively low, and the intensity to fiber, flexibility, slipping equivalent damage are less.In 20th century 80
Age, day are originally developed into this kind of conductive fiber.Someone is also specially studied conductive compositions and electrical conduction mechanism, such as Japan
The conductive acrylic fibre of the sulfide of the surface covering copper of development, is first to handle acrylic fibers in copper ions solution, is then reducing
Handled in agent, the Cu on fiber2+Become Cu+It is complexed with-CN, further forms the conductive material of the sulfide of copper.Due to this
A little conductive materials form network on fibre structure, therefore electric conductivity is fine.Domestic patent 87104625.3,
201510188325.1,200810084225.4 etc. be all in this way production conductive fiber.Because polyacrylonitrile is fine
Cyano group in dimension can produce complexing with copper ion, make fiber conductive；Common fiberglass surfacing lacks and copper ion
The group of complexing, conductive materials can not be just complexed with fiber, therefore have impact on absorption and suction of the fiber to metal sulphur compound
Attached fastness, therefore the excellent conductive fiber of electric conductivity can not be made.
The content of the invention
It is an object of the present invention to provide a kind of system of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber
Preparation Method, solves in the prior art that fiber is low to the absorption fastness of metal sulphur compound, can not be made that electric conductivity is excellent to lead
The problem of electric fiber.
Deficiency, the present invention propose a kind of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber for more than
Preparation method, its step is：
(1) glass fibre is surface-treated using vacuum plasma, treatment conditions are：Working gas be oxygen or
Person's air, back end vacuum are 1~5Pa, and operating pressure is 50~100Pa, and discharge power is 100~200W, processing time 2
~6 minutes；
(2) glass fibre by plasma treatment that step (1) obtains is immersed in mass concentration as 0.5%~2%
Aq. polyethyleneimine in, 60 DEG C~90 DEG C soak 2~6 hours, after immersion, fully rinsed with water, dry after
Obtain the glass fibre of polyethyleneimine surface modification；
(3) glass fibre for the polyethyleneimine surface modification for obtaining step (2) be placed in mass concentration for 2.5%~
In the 10% cupric sulfate pentahydrate aqueous solution, after 20 DEG C~60 DEG C are soaked 5~30 minutes, it is 2.5%~5% to add mass concentration
Sodium thiosulfate solution, be warming up to 75 DEG C~90 DEG C and react 0.3~1.5 hour, take out after being rinsed, dried with water after fiber
Obtain cuprous sulfide/glass fibre composite conducting fiber.
The mass ratio of step (3) the cupric sulfate pentahydrate aqueous solution and sodium thiosulfate solution is 1：1~1：2.
The beneficial effects of the invention are as follows：
(1) present invention is handled glass fibre using vacuum plasma first, then forms poly- second in fiber surface
Alkene imine layer, composite conducting glass fibre is obtained in fiber surface generation cuprous sulfide using chemical reaction method on this basis.
Vacuum plasma processing not only makes fiberglass surfacing crack and hollow, and fiber surface is introduced into carbonyl；Polyethylene
Imines is stronger hydrogen-bond donor, and strong interaction of hydrogen bond is formed between carbonyl, and this strong interaction makes poly- second
Alkene imines is firmly adhered to fiberglass surfacing；In addition, polyethyleneimine is a kind of typical cationic water-soluble polymer
Electrolyte, possess substantial amounts of amido N atoms on macromolecular chain and make it have very strong electron acceptor, it can be produced very to copper ion
Strong complexing, improve the absorption of the sulfide of copper on the fiber surface.In the present invention metal sulfide with it is fiberglass-based
Very strong adhesion is formed by " bridge formation " effect of polyethyleneimine amine layer between body, improves cuprous sulfide on the glass fibers
Content, really solve effective absorption problem of the glass fibre to metal sulfide, fiber has stable, lasting conductive effect
Fruit.
(2) electroconductive glass fibre is prepared using the technique of the present invention, device therefor investment cost is low, simple to operate, reaction
Mild condition, strong applicability, high treating effect, fibre property loss are few, reliable in quality, and can reduce environmental pollution, and fit
For industrialized production.
Embodiment
Embodiment 1
The present invention proposes a kind of preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber, its
Step is：
(1) alkali-free glass fibre cleaned up is subjected to vacuum plasma processing, work atmosphere is air, back end vacuum
It is 2 minutes to spend for 5Pa, operating pressure 100Pa, discharge power 200W, processing time；
(2) glass fibre by plasma treatment prepared by step (1) is immersed in the poly- second that mass concentration is 0.5%
In the alkene imines aqueous solution, soaked 4 hours at 60 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine table after drying
The glass fibre of face modification；
(3) glass fibre of the polyethyleneimine surface modification of step (2) preparation is placed in into 150 gram mass concentration is
In the 2.5% cupric sulfate pentahydrate aqueous solution, after 60 DEG C are soaked 5 minutes, 150 gram mass concentration of addition are 2.5% thiosulfuric acid
Sodium water solution, be warming up to 75 DEG C react 1.5 hours, take out fiber after rinsed with water, dry after obtain cuprous sulfide/glass fibre
Composite conducting fiber, the electrical conductivity of fiber is 3.4 × 10-2S/cm。
Embodiment 2
The present invention proposes a kind of preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber, its
Step is：
(1) alkali-free glass fibre cleaned up is subjected to vacuum plasma processing, work atmosphere is oxygen, back end vacuum
It is 6 minutes to spend for 5Pa, operating pressure 80Pa, discharge power 150W, processing time；
(2) glass fibre by plasma treatment prepared by step (1) is immersed in the poly- second that mass concentration is 0.5%
In the alkene imines aqueous solution, soaked 6 hours at 90 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine table after drying
The glass fibre of face modification；
(3) glass fibre for the polyethyleneimine surface modification for preparing step (2) is placed in 150 gram mass concentration as 5%
The cupric sulfate pentahydrate aqueous solution in, 60 DEG C immersion 5 minutes after, add 150 gram mass concentration be 5% sodium thiosulfate it is water-soluble
Liquid, be warming up to 90 DEG C react 0.3 hour, take out fiber after rinsed with water, dry after obtain cuprous sulfide/glass fibre composite guide
Electric fiber, the electrical conductivity of fiber is 9.2 × 10-1S/cm。
Embodiment 3
The present invention proposes a kind of preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber, its
Step is：
(1) alkali-free glass fibre cleaned up is subjected to vacuum plasma processing, work atmosphere is oxygen, back end vacuum
It is 5 points to spend for 1Pa, operating pressure 50Pa, discharge power 100W, processing time；
(2) glass fibre by plasma treatment prepared by step (1) is immersed in the poly- second that mass concentration is 1.5%
In the alkene imines aqueous solution, soaked 5 hours at 80 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine table after drying
The glass fibre of face modification；
(3) glass fibre for the polyethyleneimine surface modification for preparing step (2) is placed in 150 gram mass concentration as 10%
The cupric sulfate pentahydrate aqueous solution in, 20 DEG C immersion 30 minutes after, add 300 gram mass concentration be 5% sodium thiosulfate it is water-soluble
Liquid, be warming up to 80 DEG C react 1.0 hours, take out fiber after rinsed with water, dry after obtain cuprous sulfide/glass fibre composite guide
Electric fiber, the electrical conductivity of fiber is 1.6 × 100S/cm。
Embodiment 4
The present invention proposes a kind of preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber, and it is walked
Suddenly it is：
(1) alkali-free glass fibre cleaned up is subjected to vacuum plasma processing, work atmosphere is oxygen, back end vacuum
It is 3 minutes to spend for 3Pa, operating pressure 70Pa, discharge power 150W, processing time；
(2) glass fibre by plasma treatment prepared by step (1) is immersed in the poly- second that mass concentration is 1.0%
In the alkene imines aqueous solution, soaked 2 hours at 90 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine table after drying
The glass fibre of face modification；
(3) glass fibre for the polyethyleneimine surface modification for preparing step (2) is placed in 150 gram mass concentration as 8%
The cupric sulfate pentahydrate aqueous solution in, 30 DEG C immersion 20 minutes after, add 300 gram mass concentration be 4% sodium thiosulfate it is water-soluble
Liquid, be warming up to 75 DEG C react 1.0 hours, take out fiber after rinsed with water, dry after obtain cuprous sulfide/glass fibre composite guide
Electric fiber, the electrical conductivity of fiber is 9.8 × 10-1S/cm。
Embodiment 5
The present invention proposes a kind of preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber, and it is walked
Suddenly it is：
(1) alkali-free glass fibre cleaned up is subjected to vacuum plasma processing, work atmosphere is oxygen, back end vacuum
It is 4 minutes to spend for 2Pa, operating pressure 90Pa, discharge power 150W, processing time；
(2) 200 gram mass concentration are immersed in as 2.5% by plasma treatment of glass fiber by prepared by step (1)
In aq. polyethyleneimine, soaked 5 hours at 70 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine after drying
The glass fibre of amine surface modification；
(3) glass fibre of the polyethyleneimine surface modification of step (2) preparation is placed in into 150 gram mass concentration is
In the 4.5% cupric sulfate pentahydrate aqueous solution, after 40 DEG C are soaked 15 minutes, 150 gram mass concentration of addition are 4.5% thiosulfuric acid
Sodium water solution, be warming up to 80 DEG C react 1.0 hours, take out fiber after rinsed with water, dry after obtain cuprous sulfide/glass fibre
Composite conducting fiber, the electrical conductivity of fiber is 5.2 × 10-1S/cm。
Embodiment 6
The present invention proposes a kind of preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber, and it is walked
Suddenly it is：
(1) alkali-free glass fibre cleaned up is subjected to vacuum plasma processing, work atmosphere is oxygen, back end vacuum
It is 5 minutes to spend for 4Pa, operating pressure 60Pa, discharge power 120W, processing time；
(2) it is immersed in the polyethylene that mass concentration is 0.8% by plasma treatment of glass fiber by prepared by step (1)
In the imines aqueous solution, soaked 5 hours at 80 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine surface after drying
The glass fibre of modification；
(3) glass fibre for the polyethyleneimine surface modification for preparing step (2) is placed in 250 gram mass concentration as 9%
The cupric sulfate pentahydrate aqueous solution in, 40 DEG C immersion 15 minutes after, add 400 gram mass concentration be 5% sodium thiosulfate it is water-soluble
Liquid, be warming up to 80 DEG C react 1.5 hours, take out fiber after rinsed with water, dry after obtain cuprous sulfide/glass fibre composite guide
Electric fiber, the electrical conductivity of fiber is 1.8 × 100S/cm。
Embodiment 7
The present invention proposes a kind of preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber, and it is walked
Suddenly it is：
(1) alkali-free glass fibre cleaned up is subjected to vacuum plasma processing, work atmosphere is oxygen, back end vacuum
It is 5.5 minutes to spend for 3Pa, operating pressure 70Pa, discharge power 140W, processing time；
(2) the change glass fibre by plasma treatment prepared by step (1) is immersed in into 400 gram mass concentration is
In 2.8% aq. polyethyleneimine, soaked 5 hours at 85 DEG C, after immersion, fully rinsed with water, obtained after drying
The glass fibre of polyethyleneimine surface modification；
(3) glass fibre for the polyethyleneimine surface modification for preparing step (2) is placed in 250 gram mass concentration as 3%
The cupric sulfate pentahydrate aqueous solution in, 40 DEG C immersion 15 minutes after, add 250 gram mass concentration be 3% sodium thiosulfate it is water-soluble
Liquid, be warming up to 80 DEG C react 1.5 hours, take out fiber after rinsed with water, dry after obtain cuprous sulfide/glass fibre composite guide
Electric fiber, the electrical conductivity of fiber is 7.6 × 10-1S/cm。
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all spirit in invention
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (2)
1. a kind of preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber, it is characterised in that it is walked
Suddenly it is：
（1）Glass fibre is surface-treated using vacuum plasma, treatment conditions are：Working gas is oxygen or sky
Gas, back end vacuum are 1~5Pa, and operating pressure is 50~100Pa, and discharge power is 100~200W, and processing time is 2~6
Minute；
（2）By step（1）The obtained glass fibre by plasma treatment is immersed in the poly- second that mass concentration is 0.5%~2%
In the alkene imines aqueous solution, soaked 2~6 hours at 60 DEG C~90 DEG C, after immersion, fully rinsed with water, gathered after drying
The glass fibre of aziridine surface modification；
（3）By step（2）The glass fibre of obtained polyethyleneimine surface modification is placed in five that mass concentration is 2.5%~10%
In the brochanite aqueous solution, after 20 DEG C~60 DEG C are soaked 5~30 minutes, the thiosulfuric acid that mass concentration is 2.5%~5% is added
Sodium water solution, be warming up to 75 DEG C~90 DEG C react 0.3~1.5 hour, take out fiber after rinsed with water, dry after obtain vulcanization Asia
Copper/polyethyleneimine/glass fibre composite conducting fiber.
2. the preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber according to claim 1,
It is characterized in that：The step（3）The mass ratio of middle the cupric sulfate pentahydrate aqueous solution and sodium thiosulfate solution is 1：1~1：2.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610211174.1A CN105884213B (en) | 2016-04-07 | 2016-04-07 | The preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber |
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|---|---|---|---|
| CN201610211174.1A CN105884213B (en) | 2016-04-07 | 2016-04-07 | The preparation method of cuprous sulfide/polyethyleneimine/glass fibre composite conducting fiber |
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| CN105884213B true CN105884213B (en) | 2018-03-27 |
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| CN107902888A (en) * | 2017-11-21 | 2018-04-13 | 安徽玉然经编科技有限公司 | A kind of processing method for improving glass fibre electric conductivity |
| CN111906872B (en) * | 2020-08-10 | 2021-05-28 | 中原工学院 | Conductive wood with electric heating function and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030268A (en) * | 1987-07-01 | 1989-01-11 | 徐文治 | Cuprous sulfide conducting polypropylene nitrile fiber, yarn, knitting wool and preparation method |
| GB2210069A (en) * | 1987-09-17 | 1989-06-01 | Courtaulds Plc | Electrically conductive cellulosic fibres |
| CN101660264A (en) * | 2009-09-11 | 2010-03-03 | 北京化工大学 | Method for preparing polyimide/silver composite conductive fiber |
| CN104805684A (en) * | 2015-04-21 | 2015-07-29 | 常熟市翔鹰特纤有限公司 | Manufacture method of conductive fire-retardant acrylic fiber |
-
2016
- 2016-04-07 CN CN201610211174.1A patent/CN105884213B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030268A (en) * | 1987-07-01 | 1989-01-11 | 徐文治 | Cuprous sulfide conducting polypropylene nitrile fiber, yarn, knitting wool and preparation method |
| GB2210069A (en) * | 1987-09-17 | 1989-06-01 | Courtaulds Plc | Electrically conductive cellulosic fibres |
| CN101660264A (en) * | 2009-09-11 | 2010-03-03 | 北京化工大学 | Method for preparing polyimide/silver composite conductive fiber |
| CN104805684A (en) * | 2015-04-21 | 2015-07-29 | 常熟市翔鹰特纤有限公司 | Manufacture method of conductive fire-retardant acrylic fiber |
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