CN109576823A - A kind of phase-changing energy storage material and preparation method thereof with core-skin fibre structure - Google Patents
A kind of phase-changing energy storage material and preparation method thereof with core-skin fibre structure Download PDFInfo
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- CN109576823A CN109576823A CN201811324958.0A CN201811324958A CN109576823A CN 109576823 A CN109576823 A CN 109576823A CN 201811324958 A CN201811324958 A CN 201811324958A CN 109576823 A CN109576823 A CN 109576823A
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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
-
- 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
Abstract
The invention belongs to phase-changing energy storage material fields, disclose a kind of phase-changing energy storage material and preparation method thereof with core-skin fibre structure.Polyacrylonitrile is dissolved in organic solvent, phase-change accumulation energy particle is then added and is uniformly mixed, obtains oil-phase solution；Water-soluble phase-change material is dissolved in deionized water or directly uses deionized water as aqueous phase solution；Aqueous phase solution is added in oil-phase solution, emulsifier homogenous disperse is added, obtains water-in-oil emulsion, then electrostatic spinning is obtained with skin-core structure complex fiber material；Freeze-drying process obtains hollow fiber material；Finally the phase-changing energy storage material with core-skin fibre structure is obtained by pre-oxidation and carbonization treatment under an inert atmosphere.The present invention organically combines fiber technology of preparing and high performance phase-change material, and gained phase-changing energy storage material has higher enthalpy of phase change and reversible capacity, realizes more scene applications of phase-changing energy storage material.
Description
Technical field
The invention belongs to phase-changing energy storage material fields, and in particular to a kind of phase-changing energy storage material with core-skin fibre structure
And preparation method thereof.
Background technique
Due to the traditional fossil energy that coal, petroleum etc. frequently use at present be not it is inexhaustible, add
How the aggravation of upper Global Greenhouse Effect and the rising of energy prices improve the utilization rate of the energy while accelerating using novel green
Eco-friendly power source be solve the whole world about energy problem there is an urgent need to.In addition to this, energy-saving and emission-reduction are also to cope with energy problem
The necessary means of caused climate change, it is solve energy crisis one that exploitation, which manufactures more efficient, more cheap energy storage technology,
A highly important selection, energy storage technology now are broadly divided into mechanical energy energy storage system, electric energy storage system and thermal energy storage bodies
System, wherein heat storage technology can be divided into sensible heat energy storage, hidden heat energy storage and three kinds of chemical energy energy storage.
Hidden heat energy storage (latent heat storage) carries out the side of energy storage using material in phase transition process
Formula, it is to achieve the purpose that accumulation of heat using absorption or release latent heat of phase change.Melting process (mushy stage transformation), gasification (liquid
Gaseous state transformation) and sublimation process (transformation of solid gas state) heat can be all absorbed from environment.When carrying out inverse process, phase transformation will be discharged
Heat.People can effectively be used it by latent heat materials.Therefore, once latent heat storage material is extensive in life
Using, it by be maximum energy-saving environmental protection green carriers, can will be between the wastes such as solar energy, industrial exhaust heat, geothermal energy, waste heat
Performance of having a rest source uses.It may be implemented to store up using this characteristic of phase-change material (phase change material, PCM)
It can temperature adjustment function.
Since PAN (polyacrylonitrile) and pitch are the common raw materials of industrial carbon fiber, thus under study for action often using PAN as
The carbon source of carbon material.In addition to this, polyvinyl alcohol (PVA), polyimides (PI), polybenzimidazoles (PBI), Kynoar
(PVDF), the polymer such as phenolic resin and lignin are used also as carbon source.In order to convert carbon for electrospun polymer fibers
Fiber usually needs 1000 DEG C or so of high temperature cabonization.Theoretically, any to all can serve as carbon material by the polymer of skeleton of carbon
Presoma.When PAN and pitch are as carbon fiber precursor, in order to maintain the structure of fiber, need to carry out before carbonization pre-
Oxidation processes.During pre-oxidation and carbonization treatment, Mass lost, the diameter of fiber reduce.
Emulsion electrostatic spinning be it is a kind of can a step prepare the technical method with nuclear shell structure nano fiber.General feelings
Under condition, emulsion electrostatic spinning liquid is mainly the two-phase dispersion for utilizing water-in-oil type, and external polymer is formed in lotion
Organic solution continuous phase and internal aqueous dispersion phase, while being promoted between foreign minister and interior phase using the emulsifier of amphipathic characteristic
Interaction so that form stable lotion.Emulsion electrostatic spinning is more preferable relative to coaxial electrostatic spinning controllability, using neck
Domain is more extensive, there is special meaning in terms of preparing functional fibre.
That there are enthalpy of phase change is not high for existing energy-storage fibre material, mechanical property is relatively low, the thermal stability of material and leads
Hot bad problem.
Summary of the invention
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing one kind has
The preparation method of the phase-changing energy storage material of core-skin fibre structure.The method of the present invention is by New Emulsion electrospun fibers technology of preparing
It is organically combined, is displayed one's respective advantages with conventional phase change material, prepare a kind of phase-change accumulation energy material with core-skin fibre structure
Material.
Another object of the present invention is to provide it is a kind of by the above method be prepared with core-skin fibre structure
Phase-changing energy storage material.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of the phase-changing energy storage material with core-skin fibre structure, includes the following steps:
(1) preparation of oil-phase solution: polyacrylonitrile is dissolved in organic solvent, and the stirring of phase-change accumulation energy particle is then added
It is uniformly mixed, obtains oil-phase solution；
(2) preparation of aqueous phase solution: water-soluble phase-change material is dissolved in deionized water, obtains aqueous phase solution, Huo Zhezhi
It connects and uses deionized water as aqueous phase solution；
(3) aqueous phase solution is added in oil-phase solution, emulsifier homogenous disperse is added, obtains water-in-oil emulsion, so
Water-in-oil emulsion is obtained by electrostatic spinning with skin-core structure complex fiber material afterwards；
(4) there will be skin-core structure complex fiber material by freeze-drying process, and remove skin-core structure composite fibre material
The sandwich layer moisture of material, obtains hollow fiber material；
(5) hollow fiber material is obtained under an inert atmosphere by pre-oxidation and carbonization treatment with core-skin fibre knot
The phase-changing energy storage material of structure.
Preferably, organic solvent described in step (1) is n,N dimethylformamide.
Preferably, phase-change accumulation energy particle described in step (1) is ZnO, SnO2、Fe3O4、Co3O4And TiO2In particle extremely
Few one kind；Phase-change accumulation energy particle diameter is 50~500nm.Particle is excessive, cannot be coated well, obtained spinning fibre
It is beading pattern；Particle is too small, and serious agglomeration can occur for phase-change accumulation energy grains, cannot be able to divide well
It dissipates.
Preferably, the mass ratio of polyacrylonitrile described in step (1) and phase-change accumulation energy particle is (0.5~0.8): (0.05
~0.1).
Preferably, water solubility phase-change material described in step (2) is CaCl2·6H2O、SrCl2·6H2O and SnCl2In
It is at least one.
Preferably, emulsifier described in step (3) is sapn, tween, lauryl sodium sulfate and dodecyl sodium sulfate
At least one of；Preferred emulsifier is sorbester p17, and sorbester p17 is a kind of non-ionic surfactant, its HLB
Value (hydrophilic thin equilibrium valve) is 4.3, is suitable as the agent of water-in-oil system lotion, can effectively ensure that emulsion intercalation method,
The maintenance for being conducive to emulsion state during emulsion electrostatic spinning, avoids the generation of lamination.
Preferably, the time of freeze-drying described in step (4) be 12~for 24 hours, by freeze-drying can not destroy
Moisture is removed on the basis of fiber primary morphology, realizes the preparation of doughnut.
Preferably, step (5) Pre oxidation is 200~400 DEG C, 0.5~10h of soaking time；The carburizing temperature is
550~1100 DEG C, soaking time 1~for 24 hours, heating rate is 0.1~10 DEG C/min, and specific gas flow rate is 5~500ml/min, lazy
Property atmosphere be argon gas or nitrogen.
It is highly preferred that the temperature of pre-oxidation described in step (5) is 250~280 DEG C, soaking time is 2~2.5h, heating
Rate is 2~3 DEG C/min.If heating rate, less than 2 DEG C/min, the time pre-oxidized is too long；If heating rate be greater than 3 DEG C/
Side reaction then may first occur for min.The temperature of pre-oxidation cannot then complete pre-oxidation less than 200 DEG C；If pre-oxidation
Temperature be greater than 400 DEG C, then fiber may be melted or be burnt because of overheat.The temperature of the carbonization treatment is 600~650
DEG C, carbonization time is 3~6h.If carburizing temperature, less than 600 DEG C, the time is less than 3h, then the non-carbon elements such as H, N can not be from fiber
Abjection is clean；If carburizing temperature is greater than 650 DEG C, the time is greater than 6h, then the intensity of carbon fiber can decline.
A kind of phase-changing energy storage material with core-skin fibre structure, is prepared by the above method.
Further, the reversible capacity of the phase-changing energy storage material with core-skin fibre structure is 50~250mAh/g,
Heat enthalpy value is 100~300J/g.
Compared with prior art, the invention has the following advantages and beneficial effects:
(1) compared to coaxial electrostatic spinning, the present invention realizes that one-step method prepares skin-core structure fibre by emulsion electrostatic spinning
Dimension avoids being reduced complicated feed liquor propulsion device bring inconvenience using complicated equipment and instrument, being improved the system of core-skin composite fiber
Standby efficiency.
(2) phase-changing energy storage material with core-skin fibre structure is obtained by freeze-drying, pre-oxidation and carbonization, by more
The structure and pattern of kind post-processing means control material, while hollow porous fiber structure can give phase-change material certain phase
Emptying, improve energy-storing efficiency.
(3) novel fiber technology of preparing organically combined with high performance phase-change material, displayed one's respective advantages, made
It is standby with higher enthalpy of phase change, thermal stability, more high thermal conductivity coefficient, more preferable mechanical property novel phase-change material；And according to not
Same usage scenario realizes more scene applications of phase-changing energy storage material by the regulation of ingredient and parameter.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
The polyacrylonitrile of 0.5g is added in the n,N dimethylformamide of 5ml, wait be added after being completely dissolved
0.05gZnO particle, is sufficiently mixed and stirs evenly, and obtains oil-phase solution；By the CaCl6H of 0.1g2O be added to 1ml go from
In sub- water, aqueous phase solution is obtained；Aqueous phase solution is added in oil-phase solution, and 0.01g sorbester p17 is added, passes through high speed
Homogenous disperse machine lotion 10min, obtains water-in-oil emulsion, then obtains water-in-oil emulsion with skin by electrostatic spinning
Cored structure complex fiber material；There to be skin-core structure complex fiber material by freeze-drying 12h, it is compound to remove skin-core structure
The sandwich layer moisture of fibrous material, obtains hollow fiber material；By obtained hollow fiber material in tube furnace under nitrogen atmosphere
Experience pre-oxidation (200 DEG C, 10h) and (the 550 DEG C, for 24 hours) process that is carbonized, obtain the phase-change accumulation energy material with core-skin fibre structure
Material.
The phase-changing energy storage material reversible capacity with core-skin fibre structure that the present embodiment obtains is 50mAh/g, heat enthalpy value
For 100J/g, the rate of taking care of yourself under TG test is 91.26%, and thermal coefficient is 1.03W/ (m DEG C), compression strength 20.8MPa；Phase
Change energy-storage material good conductivity, stable electrochemical property, and also mechanical flexibility is excellent, and has extraordinary stable circulation
Property.
Embodiment 2
The polyacrylonitrile of 0.8g is added in the n,N dimethylformamide of 10ml, wait be added after being completely dissolved
0.1g TiO2Particle is sufficiently mixed and stirs evenly, and obtains oil-phase solution；By the SrCl of 1g2·6H2O is added to the deionization of 5ml
In water, aqueous phase solution is obtained；Aqueous phase solution is added in oil-phase solution, and 0.1g sodium alkyl sulfate is added, passes through height
Fast homogenous disperse machine lotion 10min, obtains water-in-oil emulsion, is then had water-in-oil emulsion by electrostatic spinning
Skin-core structure complex fiber material；There to be skin-core structure complex fiber material for 24 hours, it is multiple to remove skin-core structure by freeze-drying
The sandwich layer moisture of condensating fiber material, obtains hollow fiber material；By obtained hollow fiber material in tube furnace nitrogen atmosphere
Lower experience pre-oxidation (400 DEG C, 0.5h) and carbonization (1100 DEG C, 1h) process, obtain the phase-change accumulation energy with core-skin fibre structure
Material.
The phase-changing energy storage material reversible capacity with core-skin fibre structure that the present embodiment obtains is 250mAh/g, heat enthalpy value
For 300J/g, the rate of taking care of yourself under TG test is 93.02%, and thermal coefficient is 1.17W/ (m DEG C), compression strength 22.4MPa；Phase
Change energy-storage material good conductivity, stable electrochemical property, and also mechanical flexibility is excellent, and has extraordinary stable circulation
Property.
Embodiment 3
The polyacrylonitrile of 0.7g is added in the n,N dimethylformamide of 7ml, wait add 0.3g after being completely dissolved
SnO2Particle is sufficiently mixed and stirs evenly, and obtains oil-phase solution；Using the deionized water of 2ml as aqueous phase solution；By aqueous phase solution
It is added in oil-phase solution, and 0.05g Tween 80 is added, by high speed homogenization dispersion machine lotion 10min, obtain water-in-oil type
Then lotion is obtained water-in-oil emulsion with skin-core structure complex fiber material by electrostatic spinning；There to be core-skin knot
Structure complex fiber material removes the sandwich layer moisture of skin-core structure complex fiber material, obtains doughnut by freeze-drying 20h
Material；Experience pre-oxidation (300 DEG C, 5h) and carbonization (800 under nitrogen atmosphere in tube furnace by obtained hollow fiber material
DEG C, 8h) process, obtain the phase-changing energy storage material with core-skin fibre structure.
The phase-changing energy storage material reversible capacity with core-skin fibre structure that the present embodiment obtains is 150mAh/g, heat enthalpy value
For 220J/g, the rate of taking care of yourself under TG test is 92.02%, and thermal coefficient is 1.09W/ (m DEG C), compression strength 21.9MPa；Phase
Change energy-storage material good conductivity, stable electrochemical property, and also mechanical flexibility is excellent, and has extraordinary stable circulation
Property.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the phase-changing energy storage material with core-skin fibre structure, it is characterised in that include the following steps:
(1) preparation of oil-phase solution: polyacrylonitrile is dissolved in organic solvent, and phase-change accumulation energy particle is then added and is stirred
Uniformly, oil-phase solution is obtained；
(2) preparation of aqueous phase solution: water-soluble phase-change material is dissolved in deionized water, obtains aqueous phase solution, or directly make
Use deionized water as aqueous phase solution；
(3) aqueous phase solution is added in oil-phase solution, emulsifier homogenous disperse is added, obtains water-in-oil emulsion, then will
Water-in-oil emulsion is obtained by electrostatic spinning with skin-core structure complex fiber material；
(4) there will be skin-core structure complex fiber material by freeze-drying process, and remove skin-core structure complex fiber material
Sandwich layer moisture, obtains hollow fiber material；
(5) hollow fiber material is obtained having core-skin fibre structure under an inert atmosphere by pre-oxidation and carbonization treatment
Phase-changing energy storage material.
2. a kind of preparation method of phase-changing energy storage material with core-skin fibre structure according to claim 1, feature
Be: organic solvent described in step (1) is n,N dimethylformamide.
3. a kind of preparation method of phase-changing energy storage material with core-skin fibre structure according to claim 1, feature
Be: phase-change accumulation energy particle described in step (1) is ZnO, SnO2、Fe3O4、Co3O4And TiO2At least one of particle；Phase transformation
Energy storage particle diameter is 50~500nm.
4. a kind of preparation method of phase-changing energy storage material with core-skin fibre structure according to claim 1, feature
Be: the mass ratio of polyacrylonitrile described in step (1) and phase-change accumulation energy particle is (0.5~0.8): (0.05~0.1).
5. a kind of preparation method of phase-changing energy storage material with core-skin fibre structure according to claim 1, feature
Be: water solubility phase-change material described in step (2) is CaCl2·6H2O、SrCl2·6H2O and SnCl2At least one of.
6. a kind of preparation method of phase-changing energy storage material with core-skin fibre structure according to claim 1, feature
Be: emulsifier described in step (3) is at least one in sapn, tween, lauryl sodium sulfate and dodecyl sodium sulfate
Kind.
7. a kind of preparation method of phase-changing energy storage material with core-skin fibre structure according to claim 1, feature
Be: the time of freeze-drying described in step (4) be 12~for 24 hours.
8. a kind of preparation method of phase-changing energy storage material with core-skin fibre structure according to claim 1, feature
Be: step (5) Pre oxidation is 200~400 DEG C, 0.5~10h of soaking time；The carburizing temperature is 550~1100
DEG C, soaking time 1~for 24 hours, heating rate is 0.1~10 DEG C/min, and specific gas flow rate is 5~500ml/min, and inert atmosphere is argon
Gas or nitrogen.
9. a kind of phase-changing energy storage material with core-skin fibre structure, it is characterised in that: pass through any one of claim 1~8 institute
The method stated is prepared.
10. a kind of phase-changing energy storage material with core-skin fibre structure according to claim 9, it is characterised in that: described
The reversible capacity of phase-changing energy storage material with core-skin fibre structure is 50~250mAh/g, and heat enthalpy value is 100~300J/g.
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| CN110129916A (en) * | 2019-04-17 | 2019-08-16 | 浙江理工大学 | A kind of paraffin/polyacrylonitrile intelligent thermoregulating nanofiber |
| CN110747551A (en) * | 2019-11-01 | 2020-02-04 | 南开大学 | Hydrogel fiber of artificial spider silk and preparation method thereof |
| CN111005092A (en) * | 2019-11-25 | 2020-04-14 | 东北林业大学 | Preparation method of alkali lignin-based porous carbon fiber and tin oxide composite nano material |
| CN112160073A (en) * | 2020-08-31 | 2021-01-01 | 江苏大学 | Citronellal/gelatin antibacterial nanofiber membrane and preparation method and application thereof |
| CN113652769A (en) * | 2021-08-30 | 2021-11-16 | 中国工程物理研究院激光聚变研究中心 | Core-shell type Fe3Preparation of C/C fiber composite wave absorbing agent and application thereof in microwave absorption |
| CN114808192A (en) * | 2022-04-14 | 2022-07-29 | 苏州大学 | Emulsion-based heat storage fiber and preparation method thereof |
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