CN105884214B - A kind of preparation method of electroconductive glass fibre - Google Patents
A kind of preparation method of electroconductive glass fibre Download PDFInfo
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- CN105884214B CN105884214B CN201610211331.9A CN201610211331A CN105884214B CN 105884214 B CN105884214 B CN 105884214B CN 201610211331 A CN201610211331 A CN 201610211331A CN 105884214 B CN105884214 B CN 105884214B
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- 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
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- 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
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
- C03C25/68—Chemical treatment, e.g. leaching, acid or alkali treatment by etching
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Abstract
The present invention proposes a kind of preparation method of electroconductive glass fibre, and alkali-free glass fibre is immersed in aqueous hydrochloric acid solution, after immersion, is fully rinsed with water, obtains hydroxylating glass fibre after drying；The glass fibre of polyethyleneimine surface modification is obtained after in hydroxylating glass fibre immersion aq. polyethyleneimine, 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 taking-up 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 present invention relates to conductive fiber preparation field, particularly relates to a kind of preparation method of electroconductive glass fibre.
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 preparation method of electroconductive glass fibre, solves fiber in the prior art
It is low to the absorption fastness of metal sulphur compound, the problem of electric conductivity excellent conductive fiber can not be made.
The present invention uses following technical scheme, proposes a kind of preparation method of electroconductive glass fibre, its step is：
(1) alkali-free glass fibre is immersed in aqueous hydrochloric acid solution and soaked 0.5~2 hour in 20 DEG C~50 DEG C, soaked
Bi Hou, fully rinsed with water, obtain hydroxylating glass fibre after drying；
(2) it is water-soluble to immerse the polyethyleneimine that concentration is 0.5%~2% for the hydroxylating glass fibre for obtaining step (1)
In liquid, soaked 2~6 hours at 60 DEG C~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 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, addition mass concentration is 2.5%~5% sulphur
The sodium thiosulfate aqueous solution, be warming up to 75 DEG C~90 DEG C react 0.3~1.5 hour, rinsed after taking-up with water, dry after vulcanized
Cuprous/glass fibre composite conducting fiber.
Aqueous hydrochloric acid solution concentration is 1mol/L~3mol/ in the step (1).
The mass ratio of the cupric sulfate pentahydrate aqueous solution and sodium thiosulfate solution is 1 in the step (3)：1~1：2.
The beneficial effects of the invention are as follows：
(1) glass fibre is carried out immersion treatment by the present invention using watery hydrochloric acid 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.
The immersion of watery hydrochloric acid not only makes fiberglass surfacing crack and hollow, and fiber surface is introduced into carbonyl；Polyethyleneimine
Amine is stronger hydrogen-bond donor, and strong interaction of hydrogen bond is formed between carbonyl, and this strong interaction makes polyethylene
Imines is firmly adhered to fiberglass surfacing；In addition, polyethyleneimine is a kind of typical cationic water-soluble polymer electricity
Xie Zhi, possess substantial amounts of amido N atoms on macromolecular chain and make it have very strong electron acceptor, it can produce very strong to copper ion
Complexing, improve the absorption of the sulfide of copper on the fiber surface.Metal sulfide and glass fiber matrix in the present invention
Between very strong adhesion formed by " bridge formation " of polyethyleneimine amine layer effect, improve cuprous sulfide on the glass fibers
Content, really solves effective absorption problem of the glass fibre to metal sulfide, and 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 electroconductive glass fibre, and its step is：
(1) 10 grams of alkali-free glass fibres cleaned up are immersed in the aqueous hydrochloric acid solution that 200 grams of concentration are 1mol/L,
Soaked 0.5 hour in 50 DEG C, after immersion, fully rinsed with water, obtain hydroxylating glass fibre after drying；
(2) the hydroxylating glass fibre for preparing step (1) immerses the polyethyleneimine that 200 gram mass concentration are 0.5%
In the aqueous solution, soaked 4 hours at 60 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine surface modification after drying
Glass fibre；
(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 2.0 × 10-2S/cm。
Embodiment 2
The present invention proposes a kind of preparation method of electroconductive glass fibre, and its step is：
(1) 10 grams of alkali-free glass fibres cleaned up are immersed in the aqueous hydrochloric acid solution that 150 grams of concentration are 2mol/L,
Soaked 2 hours in 20 DEG C, after immersion, fully rinsed with water, obtain hydroxylating glass fibre after drying；
(2) the hydroxylating glass fibre for preparing step (1) immerses the polyethyleneimine that 200 gram mass concentration are 0.5%
In the aqueous solution, soaked 6 hours at 90 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine surface modification after drying
Glass fibre；
(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 6.2 × 10-2S/cm。
Embodiment 3
The present invention proposes a kind of preparation method of electroconductive glass fibre, and its step is：
(1) 10 grams of alkali-free glass fibres cleaned up are immersed in the aqueous hydrochloric acid solution that 150 grams of concentration are 3mol/L,
Soaked 1 hour in 30 DEG C, after immersion, fully rinsed with water, obtain hydroxylating glass fibre after drying；
(2) the hydroxylating glass fibre for preparing step (1) immerses the polyethyleneimine that 200 gram mass concentration are 1.5%
In the aqueous solution, soaked 5 hours at 80 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine surface modification after drying
Glass fibre；
(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 1.3 × 100S/cm。
Embodiment 4
The present invention proposes a kind of preparation method of electroconductive glass fibre, and its step is：
(1) 10 grams of alkali-free glass fibres cleaned up are immersed in the aqueous hydrochloric acid solution that 150 grams of concentration are 1.5mol/L
In, soaked 1.5 hours in 30 DEG C, after immersion, fully rinsed with water, obtain hydroxylating glass fibre after drying；
(2) the hydroxylating glass fibre for preparing step (1) immerses the polyethyleneimine that 200 gram mass concentration are 1.0%
In the aqueous solution, soaked 2 hours at 90 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine surface modification after drying
Glass fibre；
(3) by step (2) prepare polyethyleneimine surface modification glass fibre be placed in 150 grams of concentration be 8% five
In the brochanite aqueous solution, after 30 DEG C are soaked 20 minutes, 280 gram mass concentration of addition are 4.5% sodium thiosulfate solution,
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 conducting
Fiber, the electrical conductivity of fiber is 4.8 × 10-1S/cm。
Embodiment 5
The present invention proposes a kind of preparation method of electroconductive glass fibre, and its step is：
(1) 10 grams of alkali-free glass fibres cleaned up are immersed in the aqueous hydrochloric acid solution that 150 grams of concentration are 2.5mol/L
In, soaked 2 hours in 30 DEG C, after immersion, fully rinsed with water, hydroxylated glass fibre will be obtained after fiber drying；
(2) the hydroxylating glass fibre for preparing step (1) immerses the polyethyleneimine that 200 gram mass concentration are 2.5%
In the aqueous solution, soaked 5 hours at 70 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine surface modification after drying
Glass fibre；
(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 9.1 × 10-1S/cm。
Embodiment 6
The present invention proposes a kind of preparation method of electroconductive glass fibre, and its step is：
(1) 20 grams of alkali-free glass fibres cleaned up are immersed in the aqueous hydrochloric acid solution that 250 grams of concentration are 2.0mol/L
In, soaked 1 hour in 40 DEG C, after immersion, fully rinsed with water, obtain hydroxylating glass fibre after drying；
(2) the hydroxylating glass fibre for preparing step (1) immerses the polyethyleneimine that 400 gram mass concentration are 0.8%
In the aqueous solution, soaked 5 hours at 80 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine surface modification after drying
Glass fibre；
(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 450 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 1.1 × 100S/cm。
Embodiment 7
The present invention proposes a kind of preparation method of electroconductive glass fibre, and its step is：
(1) 20 grams of alkali-free glass fibres cleaned up are immersed in the aqueous hydrochloric acid solution that 250 grams of concentration are 2.5mol/L
In, soaked 1 hour in 35 DEG C, after immersion, fully rinsed with water, hydroxylated glass fibre will be obtained after fiber drying；
(2) the hydroxylating glass fibre for preparing step (1) immerses the polyethyleneimine that 400 gram mass concentration are 2.8%
In the aqueous solution, soaked 5 hours at 85 DEG C, after immersion, fully rinsed with water, polyethyleneimine table will be obtained after fiber drying
The glass fibre of face 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 5.8 × 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 (3)
1. a kind of preparation method of electroconductive glass fibre, it is characterised in that its step is：
（1）Alkali-free glass fibre is immersed in aqueous hydrochloric acid solution and soaked 0.5~2 hour in 20 DEG C~50 DEG C, after immersion,
Fully rinsed with water, obtain hydroxylating glass fibre after drying；
（2）By step（1）Obtained hydroxylating glass fibre is immersed in the aq. polyethyleneimine that concentration is 0.5%~2%,
Soaked 2~6 hours at 60 DEG C~90 DEG C, after immersion, fully rinsed with water, obtain polyethyleneimine surface modification after drying
Glass fibre；
（3）By step（2）It is 2.5%~10% 5 water that the glass fibre of obtained polyethyleneimine surface modification, which is placed in mass concentration,
In copper sulfate solution, after 20 DEG C~60 DEG C are soaked 5~30 minutes, addition mass concentration is 2.5%~5% sodium thiosulfate water
Solution, be warming up to 75 DEG C~90 DEG C react 0.3~1.5 hour, rinsed after taking-up with water, dry after obtain electroconductive glass fibre.
2. the preparation method of electroconductive glass fibre according to claim 1, it is characterised in that：The step（1）Middle hydrochloric acid
Concentration of aqueous solution is 1mol/L~3mol/L.
3. the preparation method of electroconductive glass fibre according to claim 1, it is characterised in that：The step（3）In five water
The mass ratio of copper sulfate solution and sodium thiosulfate solution is 1：1~1：2.
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN109626658A (en) * | 2019-01-24 | 2019-04-16 | 黄河水利职业技术学院 | A kind of processing method of copper-contained electroplating waste water |
| CN112010572A (en) * | 2020-08-17 | 2020-12-01 | 泰山玻璃纤维有限公司 | Conductive glass fiber and preparation method thereof |
| CN113698143A (en) * | 2021-09-26 | 2021-11-26 | 武汉工程大学 | Semi-flexible asphalt mixture filled with metakaolin-based polymer and preparation method thereof |
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|---|---|---|---|---|
| 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 CN201610211331.9A patent/CN105884214B/en active Active
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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