CN112430863A - High-thermal-conductivity carbon nanotube-polyvinyl alcohol composite fiber and preparation method thereof - Google Patents
High-thermal-conductivity carbon nanotube-polyvinyl alcohol composite fiber and preparation method thereof Download PDFInfo
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- CN112430863A CN112430863A CN202011325536.2A CN202011325536A CN112430863A CN 112430863 A CN112430863 A CN 112430863A CN 202011325536 A CN202011325536 A CN 202011325536A CN 112430863 A CN112430863 A CN 112430863A
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- polyvinyl alcohol
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- composite fiber
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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Abstract
The invention relates to the technical field of polyvinyl alcohol and discloses a high-thermal-conductivity carbon nano tube-polyvinyl alcohol composite fiber, wherein carboxyl of a carbon nano tube and hydroxyl of polyvinyl alcohol are subjected to esterification reaction, so that the carbon nano tube and the polyvinyl alcohol are organically combined through the connection of chemical bonds, and then the carbon nano tube-polyvinyl alcohol composite fiber is obtained through an electrostatic spinning method, under the connection action of chemical bonds, the interface acting force and the bonding force of the carbon nano tubes and the polyvinyl alcohol fibers are improved, so that the carbon nano tubes are highly dispersed in a matrix of the polyvinyl alcohol fibers, avoids the agglomeration between carbon nano tube particles, generates good stress transfer effect between the carbon nano tube particles and the carbon nano tube particles, greatly improves the tensile strength and the Young modulus of the polyvinyl alcohol fiber, meanwhile, the highly dispersed carbon nano tubes form a three-dimensional heat conduction network in the polyvinyl alcohol fibers, so that the heat conduction performance and the heat conduction performance of the composite fibers are improved.
Description
Technical Field
The invention relates to the technical field of polyvinyl alcohol, in particular to a carbon nano tube-polyvinyl alcohol composite fiber with high heat conductivity and a preparation method thereof.
Background
The polyvinyl alcohol has good film forming property, thermal stability, solvent resistance and biocompatibility, and stable mechanical property, the performance of the polyvinyl alcohol is between rubber and plastic, the polyvinyl alcohol fiber is synthetic fiber spun by using the polyvinyl alcohol as a raw material, and the polyvinyl alcohol fiber has high strength, large modulus, good wear resistance, strong weather resistance, no toxicity and no pollution, and has important use value in the aspects of fiber weaving, packaging materials, framework materials, hose materials, non-woven fabrics, papermaking and the like, so that the mechanical property of the polyvinyl alcohol is further improved, and new functions such as thermal conductivity, flame retardance and the like are endowed, and the polyvinyl alcohol fiber becomes a research hotspot.
The carbon nano tube is formed by coaxially winding a plurality of graphite sheets, has a plurality of excellent mechanical, electrical and thermal properties, is one of the most ideal functional fillers of high polymer materials, but the carbon nano tube is mainly used as a reinforcing filler at present, and is simply and physically mixed with high polymer materials such as polyvinyl alcohol and the like, so that the compounding technology is single, the interface acting force and the bonding force of the carbon nano tube and the polyvinyl alcohol are weak, and the carbon nano tube with high specific surface energy is easy to agglomerate, so that the reinforcing effect of the carbon nano tube on the polyvinyl alcohol cannot be completely exerted.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the carbon nano tube-polyvinyl alcohol composite fiber with high heat conductivity and the preparation method thereof, and the carbon nano tube-polyvinyl alcohol composite fiber has higher mechanical properties such as tensile strength, Young modulus and the like and has stronger heat conductivity.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a high-thermal-conductivity carbon nanotube-polyvinyl alcohol composite fiber comprises the following steps:
(1) adding distilled water and carbon nano tubes into a conical flask, adding isoamyl nitrite and 5-amino isophthalic acid after ultrasonic dispersion, heating to 80-100 ℃, carrying out reflux reaction for 20-30h, carrying out centrifugal separation, and washing with ethanol and distilled water to obtain the carboxylated carbon nano tubes.
(2) Adding a dimethyl sulfoxide solvent, a carboxylated carbon nanotube and polyvinyl alcohol into a reaction bottle, adding a condensing agent and a catalyst after ultrasonic dispersion, heating to 40-70 ℃, reacting for 6-12h, adding methanol for precipitation, filtering, washing with methanol and acetone, and drying to obtain the polyvinyl alcohol grafted carbon nanotube.
(3) Preparing 6-10% of spinning solution of polyvinyl alcohol grafted carbon nano tubes by mass fraction, and performing electrostatic spinning process through an electrostatic spinning device to prepare the carbon nano tube-polyvinyl alcohol composite fiber with high heat conductivity.
Preferably, the mass ratio of the carbon nanotubes, the isoamyl nitrite and the 5-aminoisophthalic acid in the step (1) is 10:55-100: 40-80.
Preferably, the condensing agent in the step (2) is dicyclohexylcarbodiimide, and the catalyst is 4-dimethylaminopyridine.
Preferably, the mass ratio of the carboxylated carbon nanotubes, the polyvinyl alcohol, the dicyclohexylcarbodiimide and the 4-dimethylaminopyridine in the step (2) is 0.3-1.5:100:20-35: 3-6.
Preferably, the electrostatic spinning device in the step (3) comprises a receiving plate, the receiving plate is movably connected with a rotating guide wheel, the rotating guide wheel is movably connected with a screw rod, a supporting block is fixedly connected to the upper portion of the electrostatic spinning device, an injector is fixedly connected to the upper portion of the supporting block, dispersion liquid is arranged in the injector, a piston is movably connected to the injector, and a spinning needle head is fixedly connected to the lower portion of the injector.
Preferably, the spinning voltage is controlled to be 18-22Kv in the electrostatic spinning process in the step (3), the distance between a spinning needle head and a receiving plate is 15-20cm, and the spinning flow rate is 0.4-0.8 mL/h.
(III) advantageous technical effects
Compared with the prior art, the invention has the following chemical experiment principle and beneficial technical effects:
in the high-heat-conductivity carbon nanotube-polyvinyl alcohol composite fiber, isoamyl nitrite and amino of 5-amino isophthalic acid are subjected to diazotization reaction to obtain a diformylbenzene diazonium salt intermediate, diazotization functional groups on a benzene ring are unstable under heating and are removed to form carbonium ions, the carbonium ions attack the carbon nanotubes to react to obtain carboxylated carbon nanotubes, a large number of arylcarboxyl functional groups are uniformly bonded on a matrix of the carbon nanotubes, carboxyl groups are further subjected to esterification reaction with hydroxyl groups of polyvinyl alcohol under the activation action of dicyclohexylcarbodiimide and 4-dimethylaminopyridine to organically combine the carbon nanotubes with the polyvinyl alcohol through the connection of chemical bonds, and then the carbon nanotube-polyvinyl alcohol composite fiber is obtained through an electrostatic spinning method, so that the interface acting force and the binding force of the carbon nanotubes and the polyvinyl alcohol fiber are obviously improved under the connection action of the chemical bonds, the carbon nano tubes are highly dispersed in the matrix of the polyvinyl alcohol fiber, so that the agglomeration among carbon nano tube particles is avoided, and a good stress transfer effect is generated between the polyvinyl alcohol fiber and the carbon nano tubes, so that the mechanical properties of the polyvinyl alcohol fiber, such as tensile strength, Young modulus and the like, are greatly improved, and meanwhile, the highly dispersed carbon nano tubes form a three-dimensional heat-conducting network in the polyvinyl alcohol fiber, so that the heat-conducting property and the heat-conducting property of the composite fiber are improved.
Drawings
FIG. 1 is a schematic view of the construction of an electrospinning apparatus;
fig. 2 is a schematic view of the adjustment of the receiving plate structure.
1-an electrostatic spinning device; 2-receiving a board; 3-rotating the guide wheel; 4-screw rod; 5-a support block; 6-a syringe; 7-dispersion liquid; 8-a piston; 9-spinning needle.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: a preparation method of a high-thermal-conductivity carbon nanotube-polyvinyl alcohol composite fiber comprises the following steps:
(1) adding distilled water, carbon nano tubes with the mass ratio of 10:55-100:40-80, isoamyl nitrite and 5-amino isophthalic acid into a conical flask, carrying out ultrasonic dispersion uniformly, heating to 80-100 ℃, carrying out reflux reaction for 20-30h, carrying out centrifugal separation, washing with ethanol and distilled water, and obtaining the carboxylated carbon nano tubes.
(2) Adding a dimethyl sulfoxide solvent, a carboxylated carbon nano tube, polyvinyl alcohol, a condensing agent dicyclohexylcarbodiimide and a catalyst 4-dimethylaminopyridine into a reaction bottle according to the mass ratio of 0.3-1.5:100:20-35:3-6, uniformly dispersing by ultrasonic, heating to 40-70 ℃, reacting for 6-12h, adding methanol for precipitation, filtering, washing with methanol and acetone, and drying to obtain the polyvinyl alcohol grafted carbon nano tube.
(3) Preparing a spinning solution of polyvinyl alcohol grafted carbon nanotubes with the mass fraction of 6-10%, and performing an electrostatic spinning process through an electrostatic spinning device, wherein the electrostatic spinning device comprises a receiving plate, the receiving plate is movably connected with a rotating guide wheel, the rotating guide wheel is movably connected with a screw, a supporting block is fixedly connected above the electrostatic spinning device, an injector is fixedly connected above the supporting block, dispersion liquid is arranged in the injector, the injector is movably connected with a piston, a spinning needle head is fixedly connected below the injector, the spinning voltage is controlled to be 18-22Kv, the distance between the spinning needle head and the receiving plate is 15-20cm, and the spinning flow rate is 0.4-0.8mL/h, so that the carbon nanotube-polyvinyl alcohol composite fiber with high heat conductivity is prepared.
Example 1
(1) Adding distilled water, carbon nano tubes with the mass ratio of 10:55:40, isoamyl nitrite and 5-amino isophthalic acid into a conical flask, carrying out ultrasonic dispersion uniformly, heating to 80 ℃, carrying out reflux reaction for 20 hours, carrying out centrifugal separation, and washing with ethanol and distilled water to obtain the carboxylated carbon nano tubes.
(2) Adding dimethyl sulfoxide solvent, carboxylated carbon nanotubes, polyvinyl alcohol, a condensing agent dicyclohexylcarbodiimide and a catalyst 4-dimethylaminopyridine in a mass ratio of 0.3:100:20:3 into a reaction bottle, uniformly dispersing by ultrasonic, heating to 40 ℃, reacting for 6 hours, adding methanol for precipitation, filtering, washing with methanol and acetone, and drying to obtain the polyvinyl alcohol grafted carbon nanotube.
(3) Preparing a spinning solution of polyvinyl alcohol grafted carbon nanotubes with the mass fraction of 6%, and performing an electrostatic spinning process through an electrostatic spinning device, wherein the electrostatic spinning device comprises a receiving plate, the receiving plate is movably connected with a rotating guide wheel, the rotating guide wheel is movably connected with a screw, a supporting block is fixedly connected above the electrostatic spinning device, an injector is fixedly connected above the supporting block, dispersion liquid is arranged inside the injector, the injector is movably connected with a piston, a spinning needle head is fixedly connected below the injector, the spinning voltage is controlled to be 18Kv, the distance between the spinning needle head and the receiving plate is 15cm, and the spinning flow rate is 0.4mL/h, so that the carbon nanotube-polyvinyl alcohol composite fiber with high heat conductivity is prepared.
Example 2
(1) Adding distilled water, carbon nano tubes with the mass ratio of 10:65:50, isoamyl nitrite and 5-amino isophthalic acid into a conical flask, carrying out ultrasonic dispersion uniformly, heating to 90 ℃, carrying out reflux reaction for 30h, carrying out centrifugal separation, and washing with ethanol and distilled water to obtain the carboxylated carbon nano tubes.
(2) Adding dimethyl sulfoxide solvent, carboxylated carbon nanotubes, polyvinyl alcohol, a condensing agent dicyclohexylcarbodiimide and a catalyst 4-dimethylaminopyridine in a mass ratio of 0.6:100:25:4 into a reaction bottle, uniformly dispersing by ultrasonic, heating to 40 ℃, reacting for 12 hours, adding methanol for precipitation, filtering, washing with methanol and acetone, and drying to obtain the polyvinyl alcohol grafted carbon nanotube.
(3) Preparing a spinning solution of polyvinyl alcohol grafted carbon nanotubes with the mass fraction of 10%, and performing an electrostatic spinning process through an electrostatic spinning device, wherein the electrostatic spinning device comprises a receiving plate, the receiving plate is movably connected with a rotating guide wheel, the rotating guide wheel is movably connected with a screw, a supporting block is fixedly connected above the electrostatic spinning device, an injector is fixedly connected above the supporting block, dispersion liquid is arranged inside the injector, the injector is movably connected with a piston, a spinning needle head is fixedly connected below the injector, the spinning voltage is controlled to be 20Kv, the distance between the spinning needle head and the receiving plate is 20cm, and the spinning flow rate is 0.6mL/h, so that the carbon nanotube-polyvinyl alcohol composite fiber with high heat conductivity is prepared.
Example 3
(1) Adding distilled water, carbon nano tubes with the mass ratio of 10:80:65, isoamyl nitrite and 5-amino isophthalic acid into a conical flask, carrying out ultrasonic dispersion uniformly, heating to 90 ℃, carrying out reflux reaction for 25 hours, carrying out centrifugal separation, and washing with ethanol and distilled water to obtain the carboxylated carbon nano tubes.
(2) Adding dimethyl sulfoxide solvent, carboxylated carbon nanotubes, polyvinyl alcohol, a condensing agent dicyclohexylcarbodiimide and a catalyst 4-dimethylaminopyridine into a reaction bottle in a mass ratio of 1:100:30:5, uniformly dispersing by ultrasonic, heating to 60 ℃, reacting for 8 hours, adding methanol for precipitation, filtering, washing with methanol and acetone, and drying to obtain the polyvinyl alcohol grafted carbon nanotubes.
(3) Preparing a spinning solution of polyvinyl alcohol grafted carbon nanotubes with the mass fraction of 8%, and performing an electrostatic spinning process through an electrostatic spinning device, wherein the electrostatic spinning device comprises a receiving plate, the receiving plate is movably connected with a rotating guide wheel, the rotating guide wheel is movably connected with a screw, a supporting block is fixedly connected above the electrostatic spinning device, an injector is fixedly connected above the supporting block, dispersion liquid is arranged inside the injector, the injector is movably connected with a piston, a spinning needle head is fixedly connected below the injector, the spinning voltage is controlled to be 20Kv, the distance between the spinning needle head and the receiving plate is 18cm, and the spinning flow rate is 0.6mL/h, so that the carbon nanotube-polyvinyl alcohol composite fiber with high heat conductivity is prepared.
Example 4
(1) Adding distilled water, carbon nano tubes with the mass ratio of 10:100:80, isoamyl nitrite and 5-amino isophthalic acid into a conical flask, carrying out ultrasonic dispersion uniformly, heating to 100 ℃, carrying out reflux reaction for 30h, carrying out centrifugal separation, and washing with ethanol and distilled water to obtain the carboxylated carbon nano tubes.
(2) Adding dimethyl sulfoxide solvent, carboxylated carbon nanotubes, polyvinyl alcohol, a condensing agent dicyclohexylcarbodiimide and a catalyst 4-dimethylaminopyridine in a mass ratio of 1.5:100:35:6 into a reaction bottle, uniformly dispersing by ultrasonic, heating to 70 ℃, reacting for 12 hours, adding methanol for precipitation, filtering, washing with methanol and acetone, and drying to obtain the polyvinyl alcohol grafted carbon nanotube.
(3) Preparing a spinning solution of polyvinyl alcohol grafted carbon nanotubes with the mass fraction of 10%, and performing an electrostatic spinning process through an electrostatic spinning device, wherein the electrostatic spinning device comprises a receiving plate, the receiving plate is movably connected with a rotating guide wheel, the rotating guide wheel is movably connected with a screw, a supporting block is fixedly connected above the electrostatic spinning device, an injector is fixedly connected above the supporting block, dispersion liquid is arranged inside the injector, the injector is movably connected with a piston, a spinning needle head is fixedly connected below the injector, the spinning voltage is controlled to be 22Kv, the distance between the spinning needle head and the receiving plate is 20cm, and the spinning flow rate is 0.8mL/h, so that the carbon nanotube-polyvinyl alcohol composite fiber with high heat conductivity is prepared.
Comparative example 1
(1) Adding distilled water, carbon nano tubes with the mass ratio of 10:40:30, isoamyl nitrite and 5-amino isophthalic acid into a conical flask, carrying out ultrasonic dispersion uniformly, heating to 100 ℃, carrying out reflux reaction for 24 hours, carrying out centrifugal separation, and washing with ethanol and distilled water to obtain the carboxylated carbon nano tubes.
(2) Adding dimethyl sulfoxide solvent, carboxylated carbon nanotubes, polyvinyl alcohol, a condensing agent dicyclohexylcarbodiimide and a catalyst 4-dimethylaminopyridine in a mass ratio of 0.1:100:15:2 into a reaction bottle, uniformly dispersing by ultrasonic, heating to 70 ℃, reacting for 12 hours, adding methanol for precipitation, filtering, washing with methanol and acetone, and drying to obtain the polyvinyl alcohol grafted carbon nanotube.
(3) Preparing a spinning solution of polyvinyl alcohol grafted carbon nanotubes with the mass fraction of 10%, and performing an electrostatic spinning process through an electrostatic spinning device, wherein the electrostatic spinning device comprises a receiving plate, the receiving plate is movably connected with a rotating guide wheel, the rotating guide wheel is movably connected with a screw, a supporting block is fixedly connected above the electrostatic spinning device, an injector is fixedly connected above the supporting block, dispersion liquid is arranged inside the injector, the injector is movably connected with a piston, a spinning needle head is fixedly connected below the injector, the spinning voltage is controlled to be 20Kv, the distance between the spinning needle head and the receiving plate is 18cm, and the spinning flow rate is 0.6mL/h, so that the carbon nanotube-polyvinyl alcohol composite fiber with high heat conductivity is prepared.
The thermal conductivity of the carbon nanotube-polyvinyl alcohol composite fiber with high thermal conductivity was measured using a thermal conductivity meter using a hot plate shield method of EP 500E.
And testing the tensile strength and Young modulus of the high-thermal-conductivity carbon nanotube-polyvinyl alcohol composite fiber by using a CMT-200 microcomputer control electronic universal testing machine.
Claims (6)
1. A high heat conduction carbon nanotube-polyvinyl alcohol composite fiber is characterized in that: the preparation method of the high-thermal-conductivity carbon nanotube-polyvinyl alcohol composite fiber comprises the following steps:
(1) adding distilled water and carbon nano tubes into a conical flask, adding isoamyl nitrite and 5-amino isophthalic acid after ultrasonic dispersion, heating to 80-100 ℃, carrying out reflux reaction for 20-30h, carrying out centrifugal separation, washing with ethanol and distilled water, and preparing carboxylated carbon nano tubes;
(2) adding a dimethyl sulfoxide solvent, a carboxylated carbon nanotube and polyvinyl alcohol into a reaction bottle, adding a condensing agent and a catalyst after ultrasonic dispersion, heating to 40-70 ℃, reacting for 6-12 hours, adding methanol for precipitation, filtering, washing with methanol and acetone, and drying to obtain a polyvinyl alcohol grafted carbon nanotube;
(3) preparing 6-10% of spinning solution of polyvinyl alcohol grafted carbon nano tubes by mass fraction, and performing electrostatic spinning process through an electrostatic spinning device to prepare the carbon nano tube-polyvinyl alcohol composite fiber with high heat conductivity.
2. The carbon nanotube-polyvinyl alcohol composite fiber having high thermal conductivity according to claim 1, wherein: the mass ratio of the carbon nano tube, the isoamyl nitrite and the 5-amino isophthalic acid in the step (1) is 10:55-100: 40-80.
3. The carbon nanotube-polyvinyl alcohol composite fiber having high thermal conductivity according to claim 1, wherein: the condensing agent in the step (2) is dicyclohexylcarbodiimide, and the catalyst is 4-dimethylaminopyridine.
4. The carbon nanotube-polyvinyl alcohol composite fiber having high thermal conductivity according to claim 1, wherein: the mass ratio of the carboxylated carbon nanotubes, the polyvinyl alcohol, the dicyclohexylcarbodiimide and the 4-dimethylaminopyridine in the step (2) is 0.3-1.5:100:20-35: 3-6.
5. The carbon nanotube-polyvinyl alcohol composite fiber having high thermal conductivity according to claim 1, wherein: the electrostatic spinning device in the step (3) comprises a receiving plate, the receiving plate is movably connected with a rotating guide wheel, the rotating guide wheel is movably connected with a screw, a supporting block is fixedly connected to the upper portion of the electrostatic spinning device, an injector is fixedly connected to the upper portion of the supporting block, dispersion liquid is arranged in the injector, a piston is movably connected to the injector, and a spinning needle head is fixedly connected to the lower portion of the injector.
6. The carbon nanotube-polyvinyl alcohol composite fiber having high thermal conductivity according to claim 1, wherein: and (3) controlling the spinning voltage to be 18-22Kv, the distance between the spinning needle head and the receiving plate to be 15-20cm, and the spinning flow rate to be 0.4-0.8mL/h in the electrostatic spinning process.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116478577A (en) * | 2023-04-28 | 2023-07-25 | 陕西科技大学 | Direct-writing conductive ink stabilized by polymer and preparation and application methods thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116478577A (en) * | 2023-04-28 | 2023-07-25 | 陕西科技大学 | Direct-writing conductive ink stabilized by polymer and preparation and application methods thereof |
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