CN113174755B - Elastic phase change energy storage fiber with temperature induction and electric heating and preparation method thereof - Google Patents
Elastic phase change energy storage fiber with temperature induction and electric heating and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of phase change fibers, and discloses an elastic phase change energy storage fiber with temperature induction and electroheating and a preparation method thereof. The method comprises the following steps: 1) dissolving polyurethane in an organic solvent or a mixed solution of the organic solvent and an ionic liquid to obtain a spinning solution; carrying out wet spinning on the spinning solution, freezing and drying to obtain porous polyurethane fibers; 2) loading the phase change material in the pore structure of the porous polyurethane fiber by adopting a vacuum impregnation method to obtain the porous polyurethane fiber containing the phase change material; 3) and coating the conductive liquid consisting of the conductive material and the polymer on the surface of the porous polyurethane fiber containing the phase-change material, and drying to obtain the elastic phase-change energy storage fiber. The fiber of the invention can load a large amount of phase change materials and has the functions of electroheating and temperature induction. The volume of the phase-change material can expand or contract in the phase-change process, so that the conductive layer stretches or contracts, and the electrical conductivity of the fiber can change along with the change of the external temperature.
Description
Technical Field
The invention belongs to the technical field of intelligent materials, and particularly relates to an elastic phase change energy storage fiber with temperature induction and electroheating and a preparation method thereof.
Background
When the external environment temperature changes rapidly, the phase change material inside the phase change energy storage fiber is subjected to phase transition, and heat is absorbed/released in the process, so that the influence of the temperature change on the microclimate environment of a human body can be effectively buffered, and the wearing comfort of people is improved. With the development of smart wearing products, phase change energy storage fibers need to be endowed with more functions.
The phase change energy storage material can absorb/release latent heat in the phase change process, and the temperature in the process is kept constant, so that the phase change energy storage material is widely applied to the fields of spaceflight, buildings, clothes and the like. The phase change energy storage materials are classified according to phase state conversion modes and are divided into solid-liquid phase change materials, solid-gas phase change materials and liquid-gas phase change materials, wherein the volume change of the materials before and after the phase change of the solid-liquid phase change materials is small, and the materials are easy to package in a carrier, so the phase change energy storage materials are widely used. The phase-change material packaged by the metal and carbon porous support can endow the composite material with excellent heat conduction/electric capacity and has the functions of electric heating and photo-thermal conversion.
The polyurethane is also called polyurethane, the main chain contains repeated urethane groups, and the chain segments of the polyurethane fiber have a structure in which soft and hard segments are embedded, so that the polyurethane fiber has excellent elasticity, the elongation at break can reach 700%, the elastic recovery rate and the fatigue resistance performance are excellent, and the polyurethane fiber is widely applied to the field of clothes.
The existing phase change energy storage fiber adopts a conductive carrier support or adds a conductive component in the carrier support, so that the phase change energy storage material can prolong the heat preservation effect of the phase change composite material through electric heating in the use process, but because the phase change composite material has no temperature sensing function, an external temperature sensing probe is required in practical application, so that the fabric structure becomes complicated; meanwhile, the mechanical properties of the fiber are reduced by adding a conductive component into the porous carrier or adopting the conductive porous carrier.
Disclosure of Invention
In view of the above disadvantages and shortcomings of the prior art, the present invention provides an elastic phase change energy storage fiber with temperature sensing and electro-heating functions and a method for preparing the same. The elastic phase change energy storage fiber with temperature induction and electroheating is obtained by loading a phase change material in porous elastic polyurethane fiber and then coating an elastic conductive layer on the surface of the fiber. The porous polyurethane fiber with high porosity can load a large amount of phase change materials, and meanwhile, the conductive layer on the surface can endow the composite phase change fiber with the functions of photothermal conversion and electrothermal conversion. And the volume of the phase-change material in the fiber can expand or contract in the phase-change process, so that the conductive layer on the surface of the elastic polyurethane fiber is stretched or contracted, and the electrical conductivity of the fiber can change along with the change of the external temperature.
In order to realize the purpose of the invention, the technical scheme of the invention is as follows:
an elastic phase-change energy storage fiber with temperature induction and electric heating comprises an elastic polyurethane fiber, a phase-change material and a conductive coating, wherein the elastic polyurethane fiber has a three-dimensional porous network structure; the phase-change material is filled in the three-dimensional porous network structure of the elastic polyurethane fiber; the film layer is coated on the surface of the elastic polyurethane fiber; the conductive coating is composed of a conductive material and an elastic polymer; the elastic polymer is waterborne polyurethane and/or waterborne acrylate;
the internal pore structure in the elastic polyurethane fiber is communicated with the external pore structure, namely the internal pore is communicated with the pore on the surface of the fiber.
A preparation method of elastic phase change energy storage fiber with temperature induction and electroheating comprises the following steps:
1) dissolving polyurethane in an organic solvent to obtain a spinning solution; preparing polyurethane fiber from the spinning solution by wet spinning, and then freezing and drying to obtain porous polyurethane fiber;
2) loading the phase change material in the pore structure of the porous polyurethane fiber by adopting a vacuum impregnation method to obtain the porous polyurethane fiber containing the phase change material;
3) mixing a conductive material with a polymer solution or a polymer emulsion to obtain a conductive liquid; and coating the conductive liquid on the surface of the porous polyurethane fiber containing the phase-change material, and drying to obtain the elastic phase-change energy storage fiber with temperature induction and electroheating.
The polyurethane in step 1) comprises polyether and/or polyester thermoplastic polyurethane. The polyurethane is linear polyurethane; preferably a thermoplastic polyurethane;
the organic solvent in the step 1) is more than one of N, N-dimethylformamide, N-dimethylacetamide, methyl pyrrolidone, dichloroethane, butanone, acetone and toluene.
The concentration of the polyurethane in the spinning solution in the step 1) is 1-50 wt%, preferably 10-30 wt%.
The wet spinning in the step 1) is to form spinning solution trickle through a spinning device, and the spinning solution trickle enters a coagulating bath to be solidified to obtain the polyurethane fiber.
The inner diameter of the spinning device is 1-1000 mu m.
The curing time is 1-20 min; the flow rate of the spinning solution is 0.01-100 m/min.
The coagulating bath is water or a mixed solution of an organic solvent and water, the organic solvent is more than one of N, N-dimethylformamide, cyclohexanone, butanone, acetone, ethyl acetate and toluene, and N, N-dimethylformamide is preferred; the mass concentration of the organic solvent in the mixed solution is 0-70 wt%.
The freezing temperature of the freezing in the step 1) is-10 to-200 ℃, and the freezing time is 15min to 16 h; the absolute pressure of drying is 1-100 pa, the temperature of drying is 30-50 ℃, and the time of drying is 6-48 h.
The drying is carried out in a freeze drying device, the temperature of a plate layer for placing the object to be dried is 30-50 ℃, and the drying time is 6-48 h.
The phase-change material in the step 2) is more than one of alkane, polyethylene glycol, higher fatty acid, higher fatty alcohol and ionic liquid. The alkane is alkane with 15-35 carbon atoms, the relative molecular weight of the polyethylene glycol is 600-20000 g/mol, the higher fatty acid is higher fatty acid with 15-30 carbon atoms, and the higher fatty alcohol is higher fatty alcohol with 15-30 carbon atoms. The ionic liquid is more than one of 1-ethyl-3-methylimidazole tetrafluoroborate, 1-ethyl-3-methylimidazole chloride, 1-ethyl-3-methylimidazole nitrate, 1-ethyl-3-methylimidazole tetrachloroaluminate, 1-butyl-3-methylimidazole chloride, 1-butyl-3-methylimidazole hexafluorophosphate and 1-decyl-3-methylimidazole bromide.
The vacuum impregnation conditions in step 2): in a vacuum environment, the temperature of vacuum impregnation is 50-100 ℃, and the time of vacuum impregnation is 0.5-24 h.
The phase-change material in the step 2) is in a liquid state before vacuum impregnation, such as: heating to make it in molten state;
after vacuum impregnation in the step 2), removing the phase change material on the surface of the porous polyurethane fiber, namely standing for 5-8 h at 50-100 ℃ in an air environment.
The polymer in the step 3) is one or more of waterborne polyurethane and waterborne acrylate;
in the step 3), the solid content (namely the total weight of the conductive material and the polymer in the conductive liquid) in the conductive liquid is 0.01-10 wt%.
The mass of the polymer/the mass of the total solid in the conductive liquid in the step 3) is 10-80%, and preferably 30-60%; the total solid mass is the total mass of the polymer and the conductive material.
The conductive material in the step 3) is more than one of graphene, multi-walled carbon nanotubes, expanded graphite, carbon black, nano silver wires, nano gold rods, nano silver rods and nano copper wires.
In the step 3), water can be added into the conductive liquid for dilution, and the solid content is 0.01-10 wt%.
In the step 3), the conductive liquid is coated for 1-100 times, and the thickness of the coating is 0.1-50 μm.
The coating in the step 3) comprises spray coating and/or dipping, wherein the dipping refers to soaking the fibers in a conductive liquid for 0.5-1.5 min, and drying; drying is here air drying.
According to the invention, the conductive coating provides a layer of coated protective layer on the surface of the porous structure fiber, and the capillary force provided by the internal pore structure is combined, so that the load of the phase change material can be well realized.
An elastic phase change energy storage fiber with temperature induction and electrogenerated heat is prepared by the method; the elastic phase-change energy storage fiber with temperature induction and electric heating comprises a porous elastic polyurethane fiber, a phase-change energy storage material and a conductive coating layer, wherein the elastic polyurethane fiber is prepared by wet spinning and freeze drying processes, the interior of the elastic polyurethane fiber is of a porous structure, holes are communicated with one another and can realize size control and quantity distribution of the holes, and an internal hole support is elastic; the energy storage material is loaded in the porous elastic polyurethane fiber; the conductive coating layer is made of a conductive material and an elastic polymer, is uniformly coated on the surface of the fiber, and is tightly attached to the surface of the fiber.
The size of the internal pores of the fiber is 0.5-100 mu m, the diameter of the fiber is 1-5000 mu m, and the specific surface area is 1-700 m 2 (ii)/g; the enthalpy value of the fiber is 50-350J/g, the elongation at break is 50-500%, the conductivity is good, and the fiber has the functions of electrothermal conversion, photothermal conversion, phase change energy storage and temperature induction.
In the invention, the porous polyurethane fiber with high porosity can load a large amount of phase-change materials, and meanwhile, the conductive layer on the surface can endow the composite phase-change fiber with the functions of photothermal conversion and electrothermal conversion. Meanwhile, the volume of the phase-change material in the fiber can expand or contract in the phase-change process, so that the conductive layer on the surface of the elastic polyurethane fiber is stretched or contracted, and the electrical conductivity of the fiber can change along with the change of the external temperature.
Compared with the prior art, the invention has the following advantages:
(1) the internal porosity of the porous polyurethane fiber prepared by wet spinning and freeze drying is very high, a large amount of phase change materials can be packaged, so that the composite phase change fiber has very high phase change enthalpy, and meanwhile, because the porous polyurethane fiber has excellent elasticity, the volume change of the phase change materials in the phase change process also influences the volume change of the porous polyurethane fiber, the conductive layer on the surface of the fiber is stretched or shrunk, the conductivity is changed, and the composite phase change fiber has the temperature sensing function.
(2) The elastic phase change energy storage fiber with temperature induction and electroheating provided by the invention has the advantages of simple preparation process and mild preparation conditions, and is suitable for large-scale production.
(3) The elastic phase change energy storage fiber with temperature induction and electroheating can be used in electric-thermal conversion, photo-thermal conversion, phase change energy storage, intelligent induction and flexible wearable devices.
Drawings
FIG. 1 is a schematic structural diagram of an elastic phase change energy storage fiber.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto. The structural schematic diagram of the elastic phase change energy storage fiber is shown in fig. 1, and the elastic phase change energy storage fiber comprises an elastic polyurethane fiber (namely porous polyurethane), a phase change material and a conductive coating, wherein the elastic polyurethane fiber has a three-dimensional porous network structure; the phase-change material is filled in the three-dimensional porous network structure of the elastic polyurethane fiber; the film layer is coated on the surface of the elastic polyurethane fiber; the conductive coating is composed of a conductive material and an elastic polymer; the elastic polymer is waterborne polyurethane and/or waterborne acrylate;
the internal pore structure in the elastic polyurethane fiber is communicated with the external pore structure, namely the internal pore is communicated with the pore on the surface of the fiber.
Example 1
10g of thermoplastic polyurethane with the Pasteur type number of 1185A is dissolved in 30ml of butanone to be used as spinning solution; taking deionized water as a coagulating bath, carrying out wet spinning at 25 ℃, solidifying for 10min, freezing the fiber at-40 ℃ for 8h, and freeze-drying in a freeze-drying device at 30 ℃ for 16h to obtain porous polyurethane fiber; completely immersing the porous polyurethane fiber in the melted octadecane, carrying out vacuum treatment for 5h at the temperature of 60 ℃, taking out the fiber, placing the fiber on filter paper, standing for 3h at the temperature of 60 ℃, and removing the redundant octadecane; dispersing 1.5g of waterborne polyurethane emulsion with polymer mass fraction of 38% and Jitian chemical model 1624 and 0.5g of graphene in 50mL of deionized water, uniformly mixing to obtain a conductive liquid, spraying the prepared conductive liquid on the surface of the fiber, drying at normal temperature, and repeating the spraying and drying process for 25 times to obtain the elastic phase-change energy storage fiber with temperature induction and electroheating.
The elastic phase change energy storage fiber with temperature induction and electroheating obtained in the embodiment has the enthalpy value of 180.5J/g, the phase change temperature of 28 ℃, and the temperature of the fiber can reach 50 ℃ after the two ends of the fiber are electrified with 10V voltage. The temperature is raised from 15 ℃ to 28 ℃ and the resistance is raised 1.35 times as high.
Example 2
8g of thermoplastic polyurethane with a basf type number of 685A is dissolved in 30ml of toluene to obtain a spinning solution; taking deionized water as a coagulating bath, carrying out wet spinning at 25 ℃, solidifying for 5min, freezing the fiber at-20 ℃ for 12h, and freeze-drying in a freeze dryer for 24h to obtain porous polyurethane fiber; completely immersing the porous polyurethane fiber in the molten tetracosan, carrying out vacuum treatment for 3h at 100 ℃, taking out the fiber, placing the fiber on filter paper, standing for 5h at 100 ℃, and removing the redundant tetracosan; adding 0.135g of nano silver wire and 0.5g of water-based acrylic resin emulsion with polymer mass fraction of 48% and Korean type RX-20 into 75ml of deionized water, soaking the fiber in a conductive coating for 1min, taking out, drying at normal temperature, and repeating the soaking and drying process for 20 times to obtain the elastic phase change energy storage fiber with temperature induction and electroheating.
The enthalpy value of the elastic phase change energy storage fiber which is obtained by the example, has temperature induction and can generate heat electrically is 187J/g, the phase change temperature is 51 ℃, and after the voltage of 10V is applied to the two ends of the fiber, the temperature of the fiber can reach 37 ℃. The temperature was raised from 20 ℃ to 50 ℃ and the resistance was raised 1.5 times as high.
Example 3
10g of thermoplastic polyurethane with the Pasteur type number of 685A is dissolved in 30ml of N, N-dimethylformamide to prepare spinning solution; taking a 5% N, N-dimethylformamide aqueous solution as a coagulating bath, carrying out wet spinning at 40 ℃, solidifying for 15min, freezing the fiber by using liquid nitrogen for 15min (-196 ℃), and carrying out freeze drying in a freeze dryer for 18h to obtain the porous polyurethane fiber; completely immersing the porous polyurethane fiber in molten hexadecanol, carrying out vacuum treatment for 5h at 90 ℃, taking out the fiber, placing the fiber on filter paper, standing for 7h at 90 ℃, and removing the redundant hexadecanol; 0.4g of waterborne polyurethane emulsion with polymer mass fraction of 38% and Jitian chemical model 1526 and 0.3g of nano gold rod are dispersed in 50mL of deionized water to prepare a conductive solution, the fiber is placed in the conductive solution to be soaked for 1min, taken out and dried at normal temperature, and the soaking and drying process is repeated for 30 times to obtain the elastic phase-change energy storage fiber with temperature induction and electroheating.
The enthalpy value of the elastic phase change energy storage fiber which has temperature induction and can generate heat electrically is 164J/g, the phase change temperature is 46 ℃, and the temperature of the fiber can reach 68 ℃ after the two ends of the fiber are electrified with 10V voltage. The temperature was raised from 20 ℃ to 50 ℃ and the resistance was raised 1.7 times as high.
Example 4 (reduction of the content of the conductive component in the conductive coating)
Dissolving 12g of thermoplastic polyurethane with a Basff model number of b95a in 30ml of N, N-dimethylformamide to prepare spinning solution, taking 10% of N, N-dimethylformamide aqueous solution as a coagulating bath, carrying out wet spinning at 40 ℃, solidifying for 10min, freezing the fiber with liquid nitrogen for 15min (-196 ℃), and carrying out freeze drying in a freeze dryer for 18h to obtain porous polyurethane fiber; completely immersing the porous polyurethane fiber in molten hexadecanol, carrying out vacuum treatment for 5h at 90 ℃, taking out the fiber, placing the fiber on filter paper, standing for 7h at 90 ℃, and removing the redundant hexadecanol; 2g of Jitian chemical model 1526 aqueous polyurethane emulsion with the polymer mass fraction of 38% and 0.1g of carbon black are dispersed in 50mL of deionized water to prepare a conductive liquid, the fiber is placed in the conductive liquid to be soaked for 1min, the fiber is taken out and dried at normal temperature, and the soaking and drying processes are repeated for 10 times to obtain the elastic phase-change energy storage fiber with temperature induction and electroheating.
The enthalpy value of the elastic phase change energy storage fiber which is obtained by the embodiment and can generate heat electrically is 176J/g, the phase change temperature is 46 ℃, and after the voltage of 10V is applied to two ends of the fiber, the temperature of the fiber is still maintained at room temperature (because the content of the conductive component in the conductive coating is low, the fiber is not heated enough under the voltage of 10V, but the resistance of the material can still be changed due to the expansion caused by heat and the contraction caused by cold of the phase change material). The temperature was raised from 20 ℃ to 50 ℃ and the resistance was raised 1.45 times as high.
Example 5 (No load phase Change Material)
10g of thermoplastic polyurethane with a Basff model number of b95a is dissolved in 30ml of N, N-dimethylformamide to prepare spinning solution; taking a 5% N, N-dimethylformamide aqueous solution as a coagulating bath, carrying out wet spinning at normal temperature, solidifying for 8min, freezing the fiber at-60 ℃ for 4h, and freeze-drying in a freeze dryer for 18h to obtain porous polyurethane fiber; dispersing 0.4g of waterborne polyurethane emulsion with polymer mass fraction of 38% and Jitian chemical model number of 1526 and 0.5g of carbon black in 50mL of deionized water to prepare a conductive liquid; and (3) soaking the porous polyurethane fiber in the conductive liquid for 1min, taking out, drying at normal temperature, and repeating the soaking and drying process for 10 times.
After the voltage of 10V is applied to the two ends of the conductive fiber obtained in the example, the temperature of the fiber can reach 60 ℃. The temperature was increased from 20 c to 50 c and no change in resistance occurred. Meanwhile, as the phase-change material is not loaded, the fiber has no phase-change enthalpy and corresponding phase-change temperature.
The above embodiments are only some embodiments with better effects, but the embodiments of the present invention are not limited by the above embodiments, and all the equivalent substitutions, variations, modifications, etc. of some technical features within the inventive concept and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. An elastic phase change energy storage fiber with temperature sensing and electroheating functions is characterized in that: the elastic polyurethane fiber comprises an elastic polyurethane fiber, a phase change material and a conductive coating, wherein the elastic polyurethane fiber has a three-dimensional porous network structure; the phase-change material is filled in the three-dimensional porous network structure of the elastic polyurethane fiber; the conductive coating is coated on the surface of the elastic polyurethane fiber; the conductive coating is composed of a conductive material and an elastic polymer; the elastic polymer is waterborne polyurethane and/or waterborne acrylate;
the internal pore structure and the external pore structure in the elastic polyurethane fiber are communicated;
the preparation method of the elastic phase change energy storage fiber with temperature induction and electroheating comprises the following steps:
1) dissolving polyurethane in an organic solvent to obtain a spinning solution; preparing polyurethane fiber from the spinning solution by wet spinning, and then freezing and drying to obtain porous polyurethane fiber;
2) loading the phase change material in the pore structure of the porous polyurethane fiber by adopting a vacuum impregnation method to obtain the porous polyurethane fiber containing the phase change material;
3) mixing a conductive material with a polymer solution or a polymer emulsion to obtain a conductive liquid; coating the conductive liquid on the surface of porous polyurethane fiber containing phase-change material, and drying to obtain elastic phase-change energy-storage fiber with temperature induction and electroheating;
the polymer in the step 3) is one or more of waterborne polyurethane and waterborne acrylate;
in the step 3), the solid content in the conductive liquid is 0.01-10 wt%, and the solid content is the total weight of the conductive material and the polymer in the conductive liquid;
the mass of the polymer/the mass of the total solid in the conductive liquid in the step 3) is 30-60%; the total solid mass is the total mass of the polymer and the conductive material;
the conductive material in the step 3) is more than one of graphene, multi-walled carbon nanotubes, expanded graphite, carbon black, nano silver wires, nano gold rods, nano silver rods and nano copper wires;
the polyurethane in the step 1) comprises polyether type and/or polyester type thermoplastic polyurethane;
the organic solvent in the step 1) is more than one of N, N-dimethylformamide, N-dimethylacetamide, methyl pyrrolidone, dichloroethane, butanone, acetone and toluene;
the phase-change material in the step 2) is more than one of alkane, polyethylene glycol, higher fatty acid, higher fatty alcohol and ionic liquid; the alkane is alkane with 15-35 carbon atoms, the relative molecular weight of the polyethylene glycol is 600-20000, the higher fatty acid is higher fatty acid with 15-30 carbon atoms, and the higher fatty alcohol is higher fatty alcohol with 15-30 carbon atoms;
the ionic liquid is more than one of 1-ethyl-3-methylimidazole tetrafluoroborate, 1-ethyl-3-methylimidazole chloride, 1-ethyl-3-methylimidazole nitrate, 1-ethyl-3-methylimidazole tetrachloroaluminate, 1-butyl-3-methylimidazole chloride, 1-butyl-3-methylimidazole hexafluorophosphate and 1-decyl-3-methylimidazole bromide.
2. The elastic phase-change energy storage fiber with temperature induction and electric heating functions as claimed in claim 1, wherein:
the concentration of the polyurethane in the spinning solution in the step 1) is 1-50 wt%; the wet spinning in the step 1) is that the spinning solution forms spinning solution trickles through a spinning device, and the spinning solution trickles enter a coagulating bath to be solidified to obtain the polyurethane fiber.
3. The elastic phase-change energy storage fiber with temperature induction and electric heating functions as claimed in claim 2, wherein: the coagulating bath is water or a mixed solution of an organic solvent and water, and the organic solvent is more than one of N, N-dimethylformamide, cyclohexanone, butanone, acetone, ethyl acetate and toluene; the mass concentration of the organic solvent in the mixed solution is 0-70 wt%;
the curing time is 1-20 min.
4. The elastic phase-change energy storage fiber with temperature induction and electric heating functions as claimed in claim 1, wherein:
the freezing temperature of the freezing in the step 1) is-10 to-200 ℃, and the freezing time is 15min to 16 h;
the vacuum impregnation conditions in step 2): in a vacuum environment, the temperature of vacuum impregnation is 50-100 ℃, and the time of vacuum impregnation is 0.5-24 h;
after vacuum impregnation in the step 2), removing the phase change material on the surface of the porous polyurethane fiber, namely standing for 5-8 h at 50-100 ℃ in an air environment;
the conductive liquid is coated for 1-100 times in the step 3), and the thickness of the coating is 0.1-50 mu m;
the coating in step 3) comprises spray coating and/or dipping.
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