CN105862171B - The preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber - Google Patents
The preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber Download PDFInfo
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- CN105862171B CN105862171B CN201610211173.7A CN201610211173A CN105862171B CN 105862171 B CN105862171 B CN 105862171B CN 201610211173 A CN201610211173 A CN 201610211173A CN 105862171 B CN105862171 B CN 105862171B
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- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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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
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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
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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
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
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- Health & Medical Sciences (AREA)
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- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention proposes a kind of preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber, 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；Hydroxylating glass fibre is immersed in the carboxyl chitosan aqueous solution, takes out and is immersed in glutaraldehyde solution after immersion, fully rinsed with water after taking-up, obtain the glass fibre of carboxyl chitosan surface modification after drying；The glass fibre of carboxyl chitosan 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 and 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 composite conducting fiber preparation field, more particularly to a kind of cuprous sulfide/carboxyl chitosan/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/carboxyl chitosan/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.
The present invention uses following technical scheme, a kind of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber
Preparation method, its step are：
(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, immersion finishes
Afterwards, fully rinsed with water, obtain hydroxylating glass fibre after drying；
(2) the hydroxylating glass fibre for obtaining step (1) immerses the carboxyl chitosan that mass concentration is 0.5%~2%
In the aqueous solution, 30 DEG C~60 DEG C soak 1~3 hour, after immersion take out immerse mass concentration be 0.05%~1% penta
In dialdehyde solution, soaked 0.5~2 hour at 30 DEG C~50 DEG C, fully rinsed with water after taking-up, obtain carboxyl chitosan after drying
The glass fibre of surface modification；
(3) glass fibre for the carboxyl chitosan 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~85 DEG C and react 0.3~1.5 hour, rinsed after taking-up with water, dry and obtain sulphur
Change cuprous/glass fibre composite conducting fiber.
The concentration of aqueous hydrochloric acid solution is 1mol/L~3mol/L 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 present invention are：
(1) glass fibre is carried out immersion treatment by the present invention using watery hydrochloric acid first, then forms carboxylation in fiber surface
Chitosan 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；Carboxylation shell gathers
Strong interaction of hydrogen bond can be formed between sugar and fiberglass surfacing carbonyl, this strong interaction gathers carboxylation shell
Sugar is firmly adhered to fiberglass surfacing；In addition, possessing substantial amounts of amido N atoms on carboxyl chitosan macromolecular chain makes its tool
There is very strong electron acceptor, it can produce very strong complexing to copper ion, improve the sulfide of copper on the fiber surface
Absorption." bridge formation " effect in the present invention between metal sulfide and glass fiber matrix by carboxyl chitosan layer forms very strong
Adhesion, improve the content of cuprous sulfide on the glass fibers, really solve glass fibre has to metal sulfide
Absorption problem is imitated, fiber has stable, lasting conductive effect.
(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 preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber, its step are as follows：
(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 obtaining step (1) immerses the carboxyl chitosan aqueous solution that mass concentration is 0.5%
In, soaked 3 hours at 30 DEG C, immersion immerses the glutaraldehyde solution that mass concentration is 0.05% after finishing taking-up, soaks 2 at 30 DEG C
Hour, fully rinsed with water after taking-up, obtain the glass fibre of carboxyl chitosan surface modification after drying；
(3) glass fibre of the carboxyl chitosan 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 1.8 × 10-2S/cm。
Embodiment 2
The preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber, step are as follows：
(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 obtaining step (1) immerses the carboxyl chitosan aqueous solution that mass concentration is 2%
In, soaked 1 hour at 30 DEG C, immersion immerses the glutaraldehyde solution that mass concentration is 1% after finishing taking-up, soaks 0.5 at 50 DEG C
Hour, fully rinsed with water after taking-up, obtain the glass fibre of carboxyl chitosan surface modification after drying；
(3) glass fibre for the carboxyl chitosan 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 300 gram mass concentration be 2.5% sodium thiosulfate it is water-soluble
Liquid, be warming up to 85 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 5.6 × 10-2S/cm。
Embodiment 3
The preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber, step are as follows：
(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 obtaining step (1) immerses the carboxyl chitosan aqueous solution that mass concentration is 1%
In, soaked 1 hour at 50 DEG C, immersion immerses the glutaraldehyde solution that mass concentration is 0.06% after finishing taking-up, soaks 1 at 40 DEG C
Hour, fully rinsed with water after taking-up, obtain the glass fibre of carboxyl chitosan surface modification after drying；
(3) glass fibre for the carboxyl chitosan 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 8.3 × 10-1S/cm。
Embodiment 4
The preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber, step are as follows：
(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 obtaining step (1) immerses the carboxyl chitosan aqueous solution that mass concentration is 0.6%
In, soaked 2.5 hours at 35 DEG C, immersion immerses the glutaraldehyde solution that mass concentration is 0.07% after finishing taking-up, in 35 DEG C of leachings
Bubble 1.5 hours, fully rinsed with water after taking-up, obtain the glass fibre of carboxyl chitosan surface modification after drying；
(3) glass fibre for the carboxyl chitosan surface modification for preparing (2) step is placed in 150 gram mass concentration as 8%
The cupric sulfate pentahydrate aqueous solution in, 30 DEG C immersion 20 minutes after, add 400 gram mass concentration be 3% 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 2.8 × 10-1S/cm。
Embodiment 5
The preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber, step are as follows：
(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, obtain hydroxylating glass fibre after drying；
(2) the hydroxylating glass fibre for obtaining step (1) immerses the carboxyl chitosan aqueous solution that mass concentration is 1.2%
In, soaked 1.5 hours at 40 DEG C, immersion immerses the glutaraldehyde solution that mass concentration is 0.08% after finishing taking-up, in 45 DEG C of leachings
1.2 hours use is steeped, fully rinsed with water after taking-up, obtain the glass fibre of carboxyl chitosan surface modification after drying；
(3) glass fibre of the carboxyl chitosan surface modification of (2) step 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 5.3 × 10-1S/cm。
Embodiment 6
The preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber, step are as follows：
(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 obtaining step (1) immerses the carboxyl chitosan aqueous solution that mass concentration is 0.9%
In, soaked 3 hours at 60 DEG C, immersion immerses the glutaraldehyde solution that mass concentration is 0.09% after finishing taking-up, in 50 DEG C of immersions
1.5 hours use, fully rinsed with water after taking-up, obtain the glass fibre of carboxyl chitosan surface modification after drying；
(3) glass fibre for the carboxyl chitosan 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, 500 gram mass concentration of addition are 4.5% sodium thiosulfate water
Solution, be warming up to 80 DEG C and react 1.5 hours, take out rinsed with water after fiber, dry after to obtain cuprous sulfide/glass fibre compound
Conductive fiber, the electrical conductivity of fiber is 9.6 × 10-1S/cm。
Embodiment 7
The preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber, step are as follows：
(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, obtain hydroxylating glass fibre after drying；
(2) the hydroxylating glass fibre for obtaining step (1) immerses the carboxyl chitosan aqueous solution that mass concentration is 1.7%
In, soaked 1.5 hours at 50 DEG C, immersion immerses the glutaraldehyde solution that mass concentration is 0.05% after finishing taking-up, in 30 DEG C of leachings
2 hours use is steeped, fully rinsed with water after taking-up, obtain the glass fibre of carboxyl chitosan surface modification after drying；
(3) glass fibre for the carboxyl chitosan 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 78 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 2.5 × 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 cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber, it is characterised in that it is walked
Suddenly it 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 immerses the carboxyl chitosan aqueous solution that mass concentration is 0.5%~2%
In, soaked 1~3 hour at 30 DEG C~60 DEG C, the glutaraldehyde solution for immersing that mass concentration is 0.05%~1% is taken out after immersion
In, soaked 0.5~2 hour at 30 DEG C~50 DEG C, fully rinsed with water after taking-up, obtain carboxyl chitosan surface modification after drying
Glass fibre；
（3）By step（2）The glass fibre of obtained carboxyl chitosan 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, it is warming up to 75 DEG C~85 DEG C and reacts 0.3~1.5 hour, rinsed after taking-up with water, dry and obtain cuprous sulfide/carboxylic
Change chitosan/glass fibre composite conducting fiber.
2. the preparation method of cuprous sulfide/carboxyl chitosan/glass fibre composite conducting fiber according to claim 1,
It is characterized in that：The step（1）The concentration of middle aqueous hydrochloric acid solution is 1mol/L~3mol/L.
3. the preparation method of cuprous sulfide/carboxyl chitosan/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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| CN110183752B (en) * | 2019-06-20 | 2021-05-04 | 中原工学院 | Preparation method of carboxyl nitrile rubber/carboxylated chitosan composite conductive film |
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| JPH11278875A (en) * | 1998-03-26 | 1999-10-12 | Asahi Glass Co Ltd | Surface treatment of glass |
| US20010016259A1 (en) * | 1999-02-16 | 2001-08-23 | Les E. Campbell | Sizing composition for glass fibers used to reinforce thermoplastic or thermosetting matrix polymers |
| KR100676485B1 (en) * | 2006-03-24 | 2007-02-01 | (주)트라보스 | A composition for teating acrylic fiber and a method for preparing conductive acrylic fiber by using the same |
| CN101302080B (en) * | 2007-05-10 | 2011-06-15 | 西北工业大学 | Pretreatment method of chemical plating conductive magneto-conductive glass fibre |
| CN101525148A (en) * | 2009-04-03 | 2009-09-09 | 天津大学 | Method for preparing cupric oxide one dimension nano material |
| CN101733161B (en) * | 2009-12-15 | 2011-09-07 | 华南师范大学 | Photochemical preparation method of chitosan loaded metal sulfide photocatalyst |
| CN104961904A (en) * | 2015-06-16 | 2015-10-07 | 常州大学 | Surface-carboxylation chitosan membrane material and preparation method thereof |
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