CN109576823B - Phase change energy storage material with skin-core fiber structure and preparation method thereof - Google Patents
Phase change energy storage material with skin-core fiber structure and preparation method thereof Download PDFInfo
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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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
- D01F1/08—Addition of substances to the spinning solution or to the melt for forming hollow filaments
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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 belongs to the field of phase change energy storage materials, and discloses a phase change energy storage material with a skin-core fiber structure and a preparation method thereof. Dissolving polyacrylonitrile in an organic solvent, adding phase change energy storage particles, stirring and mixing uniformly to obtain an oil phase solution; dissolving a water-soluble phase-change material in deionized water or directly using the deionized water as an aqueous phase solution; adding the water phase solution into the oil phase solution, adding an emulsifier for homogeneous dispersion to obtain a water-in-oil type emulsion, and then performing electrostatic spinning to obtain a composite fiber material with a skin-core structure; freezing and drying to obtain a hollow fiber material; and finally, carrying out pre-oxidation and carbonization treatment in an inert atmosphere to obtain the phase change energy storage material with the skin-core fiber structure. According to the invention, a fiber preparation technology is organically combined with a high-performance phase-change material, and the obtained phase-change energy storage material has higher phase-change enthalpy and reversible capacity, so that the multi-scene application of the phase-change energy storage material is realized.
Description
Technical Field
The invention belongs to the field of phase change energy storage materials, and particularly relates to a phase change energy storage material with a skin-core fiber structure and a preparation method thereof.
Background
Because the traditional fossil energy frequently used at present such as coal, petroleum and the like is not inexhaustible, and the global greenhouse effect is intensified and the energy price is increased, how to improve the utilization rate of energy and accelerate the use of novel green and environment-friendly energy is an urgent need for solving the global energy problem. In addition, energy conservation and emission reduction are also necessary means for dealing with climate change caused by energy problems, the development and manufacture of a more efficient and cheaper energy storage technology is a very important choice for solving the energy crisis, and the existing energy storage technology is mainly divided into a mechanical energy storage system, an electrical energy storage system and a thermal energy storage system, wherein the thermal energy storage technology can be divided into three types, namely sensible heat energy storage, latent heat energy storage and chemical energy storage.
Latent heat storage (latent heat storage) is a way of storing energy by using materials in the phase change process, and achieves the purpose of storing heat by absorbing or releasing phase change latent heat. The melting process (solid-liquid state transition), the gasification process (liquid-gas state transition), and the sublimation process (solid-gas state transition) all absorb heat from the environment. The reverse process will release the phase change heat. One can use this effectively by using latent heat materials. Therefore, once the latent heat energy storage material is widely applied in life, the latent heat energy storage material is an optimal energy-saving environment-friendly green carrier, and can utilize waste intermittent energy sources such as solar energy, industrial waste heat, geothermal energy, waste heat and the like. The energy storage and temperature regulation functions can be realized by utilizing the characteristics of Phase Change Materials (PCM).
Since PAN (polyacrylonitrile) and pitch are common raw materials for industrial carbon fibers, PAN is often used as a carbon source for carbon materials in research. In addition, polymers such as polyvinyl alcohol (PVA), Polyimide (PI), Polybenzimidazole (PBI), polyvinylidene fluoride (PVDF), phenol resin, and lignin are also used as a carbon source. High temperatures of around 1000 ℃ are generally required for the conversion of electrospun polymer fibers into carbon fibers. In principle, any polymer having a carbon skeleton can be used as a precursor of the carbon material. When PAN and pitch are used as carbon fiber precursors, a pre-oxidation treatment is required before carbonization in order to maintain the structure of the fiber. During the pre-oxidation and carbonization processes, the fiber mass is reduced and the diameter is reduced.
The emulsion electrostatic spinning is a technical method capable of preparing the nano fiber with the core-shell structure in one step. Generally, emulsion electrospinning is mainly characterized in that a water-in-oil two-phase dispersion system is utilized to form an external polymer organic solution continuous phase and an internal aqueous solution dispersed phase in an emulsion, and an amphiphilic emulsifier is used to promote the interaction between the external phase and the internal phase so as to form a stable emulsion. Compared with coaxial electrostatic spinning, the emulsion electrostatic spinning has better controllability and wider application field, and has special significance in the aspect of preparing functional fibers.
The existing energy storage fiber material has the problems of low phase change enthalpy, relatively low mechanical property and poor thermal stability and thermal conductivity of the material.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a preparation method of a phase change energy storage material with a sheath-core fiber structure. The method organically combines the preparation technology of the novel emulsion electrostatic spinning fiber with the traditional phase-change material, exerts respective advantages and prepares the phase-change energy storage material with the skin-core fiber structure.
The invention also aims to provide the phase change energy storage material with the sheath-core fiber structure prepared by the method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a phase change energy storage material with a skin-core fiber structure comprises the following steps:
(1) preparation of oil phase solution: dissolving polyacrylonitrile in an organic solvent, adding phase change energy storage particles, stirring and mixing uniformly to obtain an oil phase solution;
(2) preparation of aqueous phase solution: dissolving a water-soluble phase-change material in deionized water to obtain an aqueous phase solution, or directly using the deionized water as the aqueous phase solution;
(3) adding the water phase solution into the oil phase solution, adding an emulsifier for homogeneous dispersion to obtain a water-in-oil emulsion, and then performing electrostatic spinning on the water-in-oil emulsion to obtain a composite fiber material with a skin-core structure;
(4) carrying out freeze drying treatment on the composite fiber material with the skin-core structure to remove the core layer moisture of the composite fiber material with the skin-core structure, so as to obtain a hollow fiber material;
(5) and carrying out pre-oxidation and carbonization treatment on the hollow fiber material in an inert atmosphere to obtain the phase change energy storage material with a skin-core fiber structure.
Preferably, the organic solvent in step (1) is N, N dimethylformamide.
Preferably, the phase change energy storage particles in the step (1) are ZnO and SnO2、Fe3O4、Co3O4And TiO2At least one of particles; the diameter of the phase change energy storage particles is 50-500 nm. The particles are too large to obtain good coating, and the obtained spinning fiber is in a bead-like shape; if the particles are too small, the phase change energy storage particles can be seriously agglomerated and cannot be well dispersed.
Preferably, the mass ratio of the polyacrylonitrile to the phase change energy storage particles in the step (1) is (0.5-0.8): (0.05-0.1).
Preferably, the water-soluble phase change material in the step (2) is CaCl2·6H2O、SrCl2·6H2O and SnCl2At least one of (1).
Preferably, the emulsifier in step (3) is at least one of span, tween, sodium dodecyl sulfate and sodium dodecyl sulfate; the more preferable emulsifier is span 80, the span 80 is a nonionic surfactant, the HLB value (hydrophilic-hydrophobic balance value) of the surfactant is 4.3, the surfactant is suitable for being used as a emulsifier of water-in-oil system emulsion, the stability of the emulsion can be effectively ensured, the maintenance of the state of the emulsion in the electrostatic spinning process of the emulsion is facilitated, and the generation of a layering phenomenon is avoided.
Preferably, the freeze-drying time in the step (4) is 12-24 h, and the freeze-drying can remove moisture on the basis of not damaging the original morphology of the fiber, so that the preparation of the hollow fiber is realized.
Preferably, the pre-oxidation temperature in the step (5) is 200-400 ℃, and the heat preservation time is 0.5-10 h; the carbonization temperature is 550-1100 ℃, the heat preservation time is 1-24 h, the heating rate is 0.1-10 ℃/min, the gas flow rate is 5-500 ml/min, and the inert atmosphere is argon or nitrogen.
More preferably, the pre-oxidation temperature in the step (5) is 250-280 ℃, the heat preservation time is 2-2.5 h, and the temperature rise rate is 2-3 ℃/min. If the temperature rise rate is less than 2 ℃/min, the pre-oxidation time is too long; if the temperature increase rate is more than 3 ℃/min, side reactions may occur first. The pre-oxidation temperature is less than 200 ℃, and the pre-oxidation reaction cannot be completed; if the pre-oxidation temperature is greater than 400 ℃, the fibers may melt or burn due to overheating. The temperature of the carbonization treatment is 600-650 ℃, and the carbonization time is 3-6 h. If the carbonization temperature is less than 600 ℃ and the time is less than 3h, H, N and other non-carbon elements cannot be completely removed from the fiber; if the carbonization temperature is higher than 650 ℃ and the time is longer than 6 hours, the strength of the carbon fiber is reduced.
A phase change energy storage material with a skin-core fiber structure is prepared by the method.
Furthermore, the reversible capacity of the phase change energy storage material with the sheath-core fiber structure is 50-250 mAh/g, and the enthalpy value is 100-300J/g.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) compared with coaxial electrostatic spinning, the method realizes the one-step preparation of the skin-core structure fiber through emulsion electrostatic spinning, avoids the use of complex equipment and instruments, reduces the inconvenience brought by a complex liquid inlet propelling device, and improves the preparation efficiency of the skin-core composite fiber.
(2) The phase change energy storage material with the sheath-core fiber structure is obtained through freeze drying, pre-oxidation and carbonization, the structure and the appearance of the material are controlled by means of various post-processing means, meanwhile, the hollow porous fiber structure can provide a certain phase change space for the phase change material, and the energy storage efficiency is improved.
(3) The novel fiber preparation technology is organically combined with the high-performance phase-change material, the respective advantages are exerted, and the novel phase-change material with higher phase-change enthalpy, thermal stability, higher heat conductivity coefficient and better mechanical property is prepared; and according to different use scenes, the multi-scene application of the phase change energy storage material is realized through the regulation and control of components and parameters.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
Adding 0.5g of polyacrylonitrile into 5ml of N, N-dimethylformamide, adding 0.05g of ZnO particles after completely dissolving, and fully mixing and stirring uniformly to obtain an oil phase solution; 0.1g of CaCl.6H2Adding O into 1ml of deionized water to obtain an aqueous phase solution; adding the water phase solution into the oil phase solution, adding 0.01g of span 80, passing through a high-speed homogenizing dispersion machine emulsion for 10min to obtain a water-in-oil type emulsion, and then performing electrostatic spinning on the water-in-oil type emulsion to obtain a composite fiber material with a skin-core structure; freeze-drying the composite fiber material with the skin-core structure for 12h, and removing the core layer moisture of the composite fiber material with the skin-core structure to obtain a hollow fiber material; and subjecting the obtained hollow fiber material to pre-oxidation (200 ℃, 10h) and carbonization (550 ℃, 24h) in a tube furnace under the nitrogen atmosphere to obtain the phase change energy storage material with the sheath-core fiber structure.
The reversible capacity of the phase change energy storage material with the sheath-core fiber structure obtained in the embodiment is 50mAh/g, the enthalpy value is 100J/g, the weight retention rate under a TG test is 91.26%, the heat conductivity coefficient is 1.03W/(m.DEG C), and the compressive strength is 20.8 MPa; the phase change energy storage material has good conductivity, stable electrochemical performance, excellent mechanical flexibility and very good cycling stability.
Example 2
0.8g of polyacrylonitrile was added to 10ml of N, N-dimethylformamide, and after complete dissolution, 0.1g of TiO was added2Fully mixing and uniformly stirring the particles to obtain an oil phase solution; 1g of SrCl2·6H2Adding O into 5ml of deionized water to obtainTo an aqueous phase solution; adding the water phase solution into the oil phase solution, adding 0.1g of alkyl sodium sulfate, passing through a high-speed homogenizing dispersion machine emulsion for 10min to obtain a water-in-oil type emulsion, and then performing electrostatic spinning on the water-in-oil type emulsion to obtain a composite fiber material with a skin-core structure; freeze-drying the composite fiber material with the skin-core structure for 24 hours to remove the core layer moisture of the composite fiber material with the skin-core structure, thereby obtaining a hollow fiber material; and subjecting the obtained hollow fiber material to pre-oxidation (400 ℃, 0.5h) and carbonization (1100 ℃, 1h) in a tubular furnace under the nitrogen atmosphere to obtain the phase change energy storage material with the sheath-core fiber structure.
The reversible capacity of the phase change energy storage material with the sheath-core fiber structure obtained in the embodiment is 250mAh/g, the enthalpy value is 300J/g, the weight retention rate under a TG test is 93.02%, the heat conductivity coefficient is 1.17W/(m.DEG C), and the compressive strength is 22.4 MPa; the phase change energy storage material has good conductivity, stable electrochemical performance, excellent mechanical flexibility and very good cycling stability.
Example 3
0.7g of polyacrylonitrile was added to 7ml of N, N-dimethylformamide, and after complete dissolution, 0.3g of SnO was added2Fully mixing and uniformly stirring the particles to obtain an oil phase solution; 2ml of deionized water is used as an aqueous phase solution; adding the water phase solution into the oil phase solution, adding 0.05g of Tween 80, passing through a high-speed homogenizing dispersion machine emulsion for 10min to obtain a water-in-oil type emulsion, and then performing electrostatic spinning on the water-in-oil type emulsion to obtain a composite fiber material with a skin-core structure; freeze-drying the composite fiber material with the skin-core structure for 20h, and removing the core layer moisture of the composite fiber material with the skin-core structure to obtain a hollow fiber material; and subjecting the obtained hollow fiber material to pre-oxidation (300 ℃, 5h) and carbonization (800 ℃, 8h) in a tube furnace under the nitrogen atmosphere to obtain the phase change energy storage material with the skin-core fiber structure.
The reversible capacity of the phase change energy storage material with the sheath-core fiber structure obtained in the embodiment is 150mAh/g, the enthalpy value is 220J/g, the weight retention rate under a TG test is 92.02%, the heat conductivity coefficient is 1.09W/(m.DEG C), and the compressive strength is 21.9 MPa; the phase change energy storage material has good conductivity, stable electrochemical performance, excellent mechanical flexibility and very good cycling stability.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A preparation method of a phase change energy storage material with a skin-core fiber structure is characterized by comprising the following steps:
(1) preparation of oil phase solution: dissolving polyacrylonitrile in an organic solvent, adding phase change energy storage particles, stirring and mixing uniformly to obtain an oil phase solution;
(2) preparation of aqueous phase solution: dissolving a water-soluble phase-change material in deionized water to obtain an aqueous phase solution, or directly using the deionized water as the aqueous phase solution;
(3) adding the water phase solution into the oil phase solution, adding an emulsifier for homogeneous dispersion to obtain a water-in-oil emulsion, and then performing electrostatic spinning on the water-in-oil emulsion to obtain a composite fiber material with a skin-core structure;
(4) carrying out freeze drying treatment on the composite fiber material with the skin-core structure to remove the core layer moisture of the composite fiber material with the skin-core structure, so as to obtain a hollow fiber material;
(5) pre-oxidizing and carbonizing a hollow fiber material in an inert atmosphere to obtain a phase change energy storage material with a skin-core fiber structure;
in the step (1), the phase change energy storage particles are ZnO and SnO2、Fe3O4、Co3O4And TiO2At least one of particles; the diameter of the phase change energy storage particles is 50-500 nm;
the water-soluble phase-change material in the step (2) is CaCl2·6H2O、SrCl2·6H2O and SnCl2At least one of;
the freeze drying time in the step (4) is 12-24 hours;
the pre-oxidation temperature of the step (5) is 200-400 ℃, and the heat preservation time is 0.5-10 h; the carbonization temperature is 550-1100 ℃, the heat preservation time is 1-24 h, the heating rate is 0.1-10 ℃/min, the gas flow rate is 5-500 ml/min, and the inert atmosphere is argon or nitrogen.
2. The method for preparing a phase change energy storage material with a sheath-core fiber structure according to claim 1, wherein the method comprises the following steps: in the step (1), the organic solvent is N, N-dimethylformamide.
3. The method for preparing a phase change energy storage material with a sheath-core fiber structure according to claim 1, wherein the method comprises the following steps: in the step (1), the mass ratio of the polyacrylonitrile to the phase change energy storage particles is (0.5-0.8) to (0.05-0.1).
4. The method for preparing a phase change energy storage material with a sheath-core fiber structure according to claim 1, wherein the method comprises the following steps: in the step (3), the emulsifier is at least one of span, tween, sodium dodecyl sulfate and sodium dodecyl sulfate.
5. A phase change energy storage material with a sheath-core fiber structure is characterized in that: prepared by the method of any one of claims 1 to 4.
6. A phase change energy storage material having a sheath-core fiber structure according to claim 5, wherein: the reversible capacity of the phase change energy storage material with the sheath-core fiber structure is 50-250 mAh/g, and the enthalpy value is 100-300J/g.
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