CN104178845A - Multifunctional high-performance carbon-based nanoparticle/sodium alginate composite fibers and preparation method thereof - Google Patents
Multifunctional high-performance carbon-based nanoparticle/sodium alginate composite fibers and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of carbon-based nanoparticle/sodium alginate composite fibers. The method comprises the steps of firstly, preparing a sodium alginate water solution with a certain concentration; then, feeding graphene oxide into the solution, fully mixing, and carrying out ultrasonic dispersion to obtain a graphene oxide/sodium alginate water solution; feeding a certain quantity of carbon nano tubes into the solution, fully mixing, and carrying out the ultrasonic dispersion to obtain a carbon nano tube/graphene oxide/sodium alginate spinning solution with the good dispersion; filtering the spinning solution, defoaming, and carrying out solution spinning at the room temperature to prepare the carbon-based nanoparticle/sodium alginate composite fibers. According to the carbon-based nanoparticle/sodium alginate composite fibers prepared by adopting the method, the uniform dispersion and the formation of a network structure of carbon-based nanoparticles in the fibers can be realized, the effective orientation of the carbon-based nanoparticles in the fibers can be realized, and the tensile strength, the electrical conductivity and the degradability resistance of the fibers are improved; furthermore, the adsorbability of the fibers is effectively improved, so that the carbon-based nanoparticle/sodium alginate composite fibers can be used for absorbing heavy metal ions and dye in water solutions.
Description
Technical field
The invention belongs to the preparation field of marine biomass composite fibre, specifically by the cooperative effect between sodium alginate, CNT, redox graphene three, prepare multifunctional high-performance carbon-based nano particle/sodium alginate composite fiber.
Background technology
Alginate fibre is that to take the sodium alginate that brown alga (as sea-tangle, bulk kelp) extracts be the proprietary spining technology of prepared using and equipment, produces and has tencel material property and function, that can be used for weaving health care, military project and medical treatment.Alginate fibre has following premium properties: superpower fire resistance; Good hemostatic and antibacterial effect; Green production process.But due to the molecular structure of natural polymer uniqueness, the characteristic such as molecular weight distribution is wide, the mechanical strength of alginate fibre is lower, and the electric conductivity of fiber is low, and Application Areas is restricted.Build the high performance marine alga composite fibre of Multifunction, will greatly open up the Application Areas of alginate fibre, for industries such as China's weaving, fire-fighting, military project, space flight, contribute, promote the added value of marine alga simultaneously, drive blue economic development.One dimension CNT has excellent mechanical property, thereby existing a large amount of report of the research about CNT fortifying fibre.The preparation method of a patent CN101768798A(sodium alginate/carbon nano tube composite fibre) utilize the dispersiveness that sodium alginate is good to CNT, prepared sodium alginate/CNT and strengthened composite fibre.Yet research shows, although CNT add the TENSILE STRENGTH that can significantly improve fiber, the elongation at break of fiber declines to some extent, causes the toughness of fiber poor.And the toughness of fiber is mainly to be determined by the microstructure of fiber, so the design of microstructure fiber is vital with controlling for obtaining strong and tough fiber.Two dimensional oxidation Graphene is the same with one dimension CNT has excellent mechanical property, even there are some researches show that graphene oxide has better mechanical property, thereby become the focus of recent people research, and graphene oxide surface has the functional groups such as hydroxyl, can react with the carboxyl of sodium alginate, thereby improve better the interface bond strength of matrix and fiber.More worth proposition, up-to-date research shows, because CNT is one dimension material with carbon element, and Graphene is Two-dimensional Carbon material, both use simultaneously and can form network structure, and can produce synergy, and this microstructure improves a lot for the toughness of fiber.Have at present the report of graphene/carbon nanotube modified synergic glass fiber reinforcement epoxy composite, also have the report of graphene/carbon nanotube modified synergic polyvinyl alcohol composite fiber.But, also do not utilize the Synergistic effect modified alginate fibre between sodium alginate, CNT, redox Graphene three at present, give alginate fibre high-performance and multi-functional report simultaneously.This fiber not only has the toughness of high strength, excellence, also has good electric conductivity, anti-degradability, radiation resistance, absorption property, can be widely used in the fields such as high performance fibre material, medicine and environment.
Summary of the invention
Task of the present invention is for providing a kind of carbon-based nano particle/sodium alginate multifunctional high-performance composite fibre and preparation method thereof.
A kind of carbon-based nano particle/sodium alginate multifunctional high-performance composite fibre and preparation method thereof, comprises the following steps:
A. sodium alginate is added to the water, at room temperature stirs 0.5-5 hour, then at 35-60 ℃, stir 2-5 hour, the sodium alginate aqueous solution that configuration quality percent concentration is 3-20%;
B. will in the sodium alginate aqueous solution obtaining in step a, add graphene oxide, the mass percent concentration that makes its graphene oxide is 0.01-3%, then adopts ultrasonic processing 0.5-5 hours, obtains graphene oxide/sodium alginate aqueous solution;
C. by obtaining in step b, in graphene oxide/sodium alginate aqueous solution, add CNT, the mass percent concentration that makes its CNT is 0.01-3%, then adopt ultrasonic processing 0.5-5 hours, obtain CNT/graphene oxide/sodium alginate spinning solution;
D. CNT/graphene oxide step c being obtained/sodium alginate spinning solution is placed on 6-24 hour in vacuum drying oven, carries out deaeration, to mixed solution without bubble till;
E. CNT/graphene oxide steps d being obtained/sodium alginate spinning solution, by certain spinning process, through coagulating bath, obtains sodium alginate/CNT/graphene oxide as-spun fibre;
F. by CNT/graphene oxide of producing in step e/sodium alginate as-spun fibre through after preheating bath, drawing-off and bathing
Carry out drafting forming and oiling treatment, obtain CNT/graphene oxide/sodium alginate composite fiber.
In described step a, sodium alginate used is for to be extracted and Bacteria Culture by brown alga.
In described step b, graphene oxide used is Brodie method, and Staudenmaier method and Hummers method prepare.
In described step c, CNT used is Single Walled Carbon Nanotube, double-walled carbon nano-tube and multi-walled carbon nano-tubes.
In described step e, described spinning process comprises wet spinning, dry spinning, dry-wet spinning, electrostatic spinning.
In described step e, spinning solution temperature is 35 ℃ 60 ℃; Coagulating bath is that mass percent concentration is 2% 7% calcium chloride and other divalent salts aqueous solution, comprises calcium chloride, zinc chloride, barium chloride; Coagulation bath temperature is 25 ℃ 65 ℃.
CNT/graphene oxide/sodium alginate composite fiber that above-mentioned steps is prepared, has excellent TENSILE STRENGTH, toughness, electric conductivity, anti-degradability, absorption property.
CNT/graphene oxide/the sodium alginate composite fiber of the prepared described preparation of above-mentioned steps, its electric conductivity has humidity controllability and invertibity.
useful technique effect of the present invention is:
The present invention adopts two-dimentional carbon nanomaterial (graphene oxide) and carbon nanomaterial (CNT) the modified synergic alginate fibre of one dimension to strengthen toughness reinforcing alginate fibre, utilize sodium alginate, CNT, in the time of excellent properties separately of graphene oxide, also use the cooperative effect between their threes, realized CNT, the formation of the dispersed and network structure of graphene oxide in fiber, and CNT and the effective orientation of graphene oxide in fiber, therefore make the composite fibre of preparation there is excellent TENSILE STRENGTH, toughness, electric conductivity, anti-degradability, absorption property.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
A. sodium alginate is added to the water, at room temperature stirs 0.5 hour, then at 35 ℃, stir 2 hours the sodium alginate aqueous solution that configuration quality percent concentration is 3%;
B. will in the sodium alginate aqueous solution obtaining in step a, add graphene oxide, the mass percent concentration that makes its graphene oxide is 1%, then adopts ultrasonic processing 2 hours, obtains graphene oxide/sodium alginate aqueous solution;
C. will in step b, obtain adding CNT in graphene oxide/sodium alginate aqueous solution, the mass percent concentration that makes its CNT is 0.01%, then adopts ultrasonic processing 0.5 hour, obtains CNT/graphene oxide/sodium alginate spinning solution;
D. CNT/graphene oxide step c being obtained/sodium alginate spinning solution is placed in vacuum drying oven 6 hours, carries out deaeration, to mixed solution without bubble till;
E. it is 55 ℃ that CNT/graphene oxide steps d being obtained/sodium alginate spinning solution is adjusted to temperature, utilize the spinnerets in 75 microns, 70 hole to carry out wet spinning to spinning solution, spinning speed is 30 ms/min, then it is 25 ℃ that the thread that makes spinning solution form by spinnerets enters temperature, in the calcium chloride water of mass percent concentration 7%, solidify, obtain CNT/graphene oxide/sodium alginate as-spun fibre;
F. by CNT/graphene oxide of producing in step e/sodium alginate as-spun fibre through after preheating bath, drawing-off and bathing
Carry out drafting forming and oiling treatment, obtain CNT/graphene oxide/sodium alginate composite fiber.
Embodiment 2
A. sodium alginate is added to the water, at room temperature stirs 5 hours, then at 50 ℃, stir 5 hours the sodium alginate aqueous solution that configuration quality percent concentration is 15%;
B. will in the sodium alginate aqueous solution obtaining in step a, add graphene oxide, the mass percent concentration that makes its graphene oxide is 0.01%, then adopts ultrasonic processing 2 hours, obtains graphene oxide/sodium alginate aqueous solution;
C. will in step b, obtain adding CNT in graphene oxide/sodium alginate aqueous solution, the mass percent concentration that makes its CNT is 1%, then adopts ultrasonic processing 0.5 hour, obtains CNT/graphene oxide/sodium alginate spinning solution;
D. CNT/graphene oxide step c being obtained/sodium alginate spinning solution is placed in vacuum drying oven 24 hours, carries out deaeration, to mixed solution without bubble till;
E. it is 65 ℃ that CNT/graphene oxide steps d being obtained/sodium alginate spinning solution is adjusted to temperature, utilize the spinnerets in 75 microns, 70 hole to carry out wet spinning to spinning solution, spinning speed is 30 ms/min, then it is 60 ℃ that the thread that makes spinning solution form by spinnerets enters temperature, in the calcium chloride water of mass percent concentration 5%, solidify, obtain CNT/graphene oxide/sodium alginate as-spun fibre;
F. CNT/graphene oxide of producing in step e/sodium alginate as-spun fibre is carried out to drafting forming and oiling treatment after preheating bath, drawing-off bath, obtain CNT/graphene oxide/sodium alginate composite fiber.
Embodiment 3
A. sodium alginate is added to the water, at room temperature stirs 5 hours, then at 60 ℃, stir 5 hours the sodium alginate aqueous solution that configuration quality percent concentration is 20%;
B. will in the sodium alginate aqueous solution obtaining in step a, add graphene oxide, the mass percent concentration that makes its graphene oxide is 1%, then adopts ultrasonic processing 2 hours, obtains graphene oxide/sodium alginate aqueous solution;
C. will in step b, obtain adding CNT in graphene oxide/sodium alginate aqueous solution, the mass percent concentration that makes its CNT is 0.01%, then adopts ultrasonic processing 0.5 hour, obtains CNT/graphene oxide/sodium alginate spinning solution;
D. CNT/graphene oxide step c being obtained/sodium alginate spinning solution is placed in vacuum drying oven 24 hours, carries out deaeration, to mixed solution without bubble till;
E. it is 65 ℃ that CNT/graphene oxide steps d being obtained/sodium alginate spinning solution is adjusted to temperature, utilize the spinnerets in 75 microns, 70 hole to carry out wet spinning to spinning solution, spinning speed is 30 ms/min, then it is 65 ℃ that the thread that makes spinning solution form by spinnerets enters temperature, in the barium chloride solution of mass percent concentration 2%, solidify, obtain CNT/graphene oxide/sodium alginate as-spun fibre;
F. by CNT/graphene oxide of producing in step e/sodium alginate as-spun fibre through after preheating bath, drawing-off and bathing
Carry out drafting forming and oiling treatment, obtain CNT/graphene oxide/sodium alginate composite fiber.
Embodiment 4
A. sodium alginate is added to the water, at room temperature stirs 0.5 hour, then at 50 ℃, stir 5 hours the sodium alginate aqueous solution that configuration quality percent concentration is 3%;
B. will in the sodium alginate aqueous solution obtaining in step a, add graphene oxide, the mass percent concentration that makes its graphene oxide is 0.1%, then adopts ultrasonic processing 0.5 hour, obtains graphene oxide/sodium alginate aqueous solution;
C. will in step b, obtain adding CNT in graphene oxide/sodium alginate aqueous solution, the mass percent concentration that makes its CNT is 3%, then adopts ultrasonic processing 5 hours, obtains CNT/graphene oxide/sodium alginate spinning solution;
D. CNT/graphene oxide step c being obtained/sodium alginate spinning solution is placed in vacuum drying oven 6 hours, carries out deaeration, to mixed solution without bubble till;
E. it is 55 ℃ that CNT/graphene oxide steps d being obtained/sodium alginate spinning solution is adjusted to temperature, utilize the spinnerets in 75 microns, 70 hole to carry out wet spinning to spinning solution, spinning speed is 30 ms/min, then it is 40 ℃ that the thread that makes spinning solution form by spinnerets enters temperature, in the calcium chloride water of mass percent concentration 5%, solidify, obtain CNT/graphene oxide/sodium alginate as-spun fibre;
F. by CNT/graphene oxide of producing in step e/sodium alginate as-spun fibre through after preheating bath, drawing-off and bathing
Carry out drafting forming and oiling treatment, obtain CNT/graphene oxide/sodium alginate composite fiber.
Embodiment 5
A. sodium alginate is added to the water, at room temperature stirs 0.5 hour, then at 50 ℃, stir 5 hours the sodium alginate aqueous solution that configuration quality percent concentration is 3%;
B. will in the sodium alginate aqueous solution obtaining in step a, add graphene oxide, the mass percent concentration that makes its graphene oxide is 3%, then adopts ultrasonic processing 5 hours, obtains graphene oxide/sodium alginate aqueous solution;
C. will in step b, obtain adding CNT in graphene oxide/sodium alginate aqueous solution, the mass percent concentration that makes its CNT is 1%, then adopts ultrasonic processing 3 hours, obtains CNT/graphene oxide/sodium alginate spinning solution;
D. CNT/graphene oxide step c being obtained/sodium alginate spinning solution is placed in vacuum drying oven 24 hours, carries out deaeration, to mixed solution without bubble till;
E. it is 50 ℃ that CNT/graphene oxide steps d being obtained/sodium alginate spinning solution is adjusted to temperature, utilize the spinnerets in 75 microns, 70 hole to carry out wet spinning to spinning solution, spinning speed is 30 ms/min, then it is 40 ℃ that the thread that makes spinning solution form by spinnerets enters temperature, in the calcium chloride water of mass percent concentration 5%, solidify, obtain CNT/graphene oxide/sodium alginate as-spun fibre;
F. CNT/graphene oxide of producing in step e/sodium alginate as-spun fibre is carried out to drafting forming and oiling treatment after preheating bath, drawing-off bath, obtain CNT/graphene oxide/sodium alginate composite fiber.
Claims (8)
1. carbon-based nano particle sodium alginate multifunctional high-performance composite fibre and preparation method thereof, its step is as follows:
A. sodium alginate is added to the water, at room temperature stirs 0.5-5 hour, then at 35-60 ℃, stir 2-5 hour, the sodium alginate aqueous solution that configuration quality percent concentration is 3-20%;
B. will in the sodium alginate aqueous solution obtaining in step a, add graphene oxide, the mass percent concentration that makes its graphene oxide is 0.01-3%, then adopts ultrasonic processing 0.5-5 hours, obtains graphene oxide/sodium alginate aqueous solution;
C. by obtaining in step b, in graphene oxide/sodium alginate aqueous solution, add CNT, the mass percent concentration that makes its CNT is 0.01-3%, then adopt ultrasonic processing 0.5-5 hours, obtain CNT/graphene oxide/sodium alginate spinning solution;
D. CNT/graphene oxide step c being obtained/sodium alginate spinning solution is placed on 6-24 hour in vacuum drying oven, carries out deaeration, to mixed solution without bubble till;
E. CNT/graphene oxide steps d being obtained/sodium alginate spinning solution, by certain spinning process, through coagulating bath, obtains sodium alginate/CNT/graphene oxide as-spun fibre;
F. by CNT/graphene oxide of producing in step e/sodium alginate as-spun fibre through after preheating bath, drawing-off and bathing
Carry out drafting forming and oiling treatment, obtain CNT/graphene oxide/sodium alginate composite fiber.
2. in step a according to claim 1, it is characterized in that: sodium alginate used is for to be extracted and Bacteria Culture by brown alga.
3. in step b according to claim 1, it is characterized in that: graphene oxide used is Brodie method, Staudenmaier method and Hummers method prepare.
4. in step c according to claim 1, it is characterized in that: CNT used is Single Walled Carbon Nanotube, double-walled carbon nano-tube and multi-walled carbon nano-tubes.
5. in step e according to claim 1, it is characterized in that: described spinning process comprises wet spinning, dry spinning, dry-wet spinning, electrostatic spinning.
6. in step e according to claim 1, it is characterized in that: spinning solution temperature is 25 ℃ 60 ℃; Coagulating bath is that mass percent concentration is 2% 7% calcium chloride and other divalent salts aqueous solution, comprises calcium chloride, zinc chloride, barium chloride; Coagulation bath temperature is 25 ℃ 65 ℃.
7. CNT/graphene oxide/sodium alginate composite fiber of preparing according to claim 1, has excellent TENSILE STRENGTH, toughness, electric conductivity, anti-degradability, absorption property.
8. CNT/graphene oxide/sodium alginate composite fiber of preparing according to claim 1, its electric conductivity has humidity controllability and invertibity.
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