CN111918425A - Graphene polymerization nanometer energy heating sheet and preparation method thereof - Google Patents
Graphene polymerization nanometer energy heating sheet and preparation method thereof Download PDFInfo
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Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
- H05B3/36—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs heating conductor embedded in insulating material
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- Chemical Or Physical Treatment Of Fibers (AREA)
- Woven Fabrics (AREA)
Abstract
The graphene polymerization nanometer energy heating sheet comprises a first fiber composite fabric, a heating wire and a second fiber composite fabric from inside to outside, wherein the heating wire is embroidered on the first fiber composite fabric in a roundabout and winding shape in a computer embroidery mode, and the first fiber composite fabric is tightly connected with the second fiber composite fabric in a gluing mode and clamps the heating wire between the first fiber composite fabric and the second fiber composite fabric. The graphene polymerization nanometer energy heating sheet and the preparation method thereof have the advantages of reasonable structural design, good heating effect, high heat conduction speed, rapid temperature rise, non-conduction when electrified, long service life, water resistance, electric shock resistance, fire resistance, high safety, release of far infrared waves and negative oxygen ions, no radiation, contribution to human health, simple preparation method, high flexibility and wide application prospect.
Description
Technical Field
The invention belongs to the field of heating elements, and particularly relates to a graphene polymerization nanometer energy heating sheet and a preparation method thereof.
Background
With the progress of science and technology, the science and technology brings great changes to the traditional industries and traditional products, such as clothes, physiotherapy products, small household appliances and the like in the traditional industries. The modern people have abundant physical life, and the times of keeping warm and healthy simply depending on clothes, physiotherapy products and small household appliances have passed, the pursuit of natural comfort, health and personality becomes mainstream, and the potential requirements of the modern people on the clothes, the physiotherapy products and the small household appliances which generate heat are reflected.
At present, the clothes, the physiotherapy products and the small household appliances of the heating type can be divided into 3 types according to the types of the heat sources: electrical, chemical and solar heating. The chemistry generates heat and is exactly utilizing chemical reaction to produce heat, and the drawback is that the temperature that generates heat is too high, to clothing, physiotherapy product, can only place at the skin, places next to the shin and can scald skin, and glue also can remain and be difficult to wash on the clothing, can produce solid waste moreover. Solar heating utilizes sunlight to generate electric energy for heating, and has the defects that if the solar heating is worn in a winter and in a rainy season, the illumination intensity is not strong, the heating state is not realized for a certain time by the existing technology with low photoelectric conversion efficiency, and people are not always in the sunlight. The solar heating device is mostly indoors in the daytime, the time for receiving sunlight is short, and the electricity generated by solar energy is not enough to be consumed by the heating component.
Chemical heating and solar heating have great defects, and electric heating is better than other two heating modes in future development and has development potential. However, the heating clothes, physiotherapy products and small household appliances in the prior art have great defects, and particularly, the heating clothes, physiotherapy products and small household appliances are thick, have poor comfort, low heat conduction speed, cannot ensure the safety in a power-on state, have no radiation and the like, and also have no health care performance. Therefore, it is necessary to develop a graphene polymerization nano energy heating sheet to solve the above problems.
The Chinese patent application No. CN201320046173.8 discloses a multilayer composite carbon crystal heating body, which adopts a conventional weaving method, is easy to delaminate after being stressed, causes damage and short service life, and has no waterproof layer and potential safety hazard easily.
Chinese patent application No. CN201710336496.3 discloses a carbon fiber heating cable, which has serious heat attenuation, cannot ensure heating temperature, and consumes energy.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects, the invention aims to provide the graphene polymerization nanometer energy heating sheet and the preparation method thereof, and the graphene polymerization nanometer energy heating sheet has the advantages of reasonable structural design, good integrity, excellent flexibility, bending resistance, difficult fracture, long service life, good heating effect, high heat conduction speed, rapid temperature rise, electricity conduction and non-conduction, long service life, water resistance, oil pollution resistance, electric shock resistance, fire resistance, good moisture permeability, high safety, release of far infrared waves and negative oxygen ions, contribution to human health, simple preparation method, high flexibility and wide application prospect.
The purpose of the invention is realized by the following technical scheme:
a graphene polymerization nanometer energy heating sheet comprises a first fiber composite fabric, a heating wire and a second fiber composite fabric from inside to outside, wherein the heating wire is embroidered on the first fiber composite fabric in a roundabout and zigzag shape in a computer embroidery mode, and the first fiber composite fabric is tightly connected with the second fiber composite fabric in a gluing mode and clamps the heating wire between the first fiber composite fabric and the second fiber composite fabric; the fiber composite fabric I comprises a hydrophobic bottom layer, a fiber film layer and a hydrophobic top layer from inside to outside, and the hydrophobic bottom layer, the fiber film layer and the hydrophobic top layer are subjected to fiber stacking in an electrostatic spinning mode to form a three-dimensional net-shaped structure; the heating wire comprises a heating core body and a protective layer, wherein the heating core body is formed by three-dimensionally weaving a plurality of polymerization nanometer energy wires, and the protective layer comprises an insulating layer and a waterproof layer which are sequentially arranged from inside to outside and tightly covers the heating core body.
The graphene polymerization nanometer energy heating sheet is reasonable in structural design, the heating wire is embroidered on the first fiber composite fabric in a roundabout winding shape in a computer embroidery mode, the second fiber composite fabric and the second fiber composite fabric tightly clamp the heating wire in the middle, the heating effect of the graphene polymerization nanometer energy heating sheet is guaranteed, the heating efficiency is greatly improved, the service life of the graphene polymerization nanometer energy heating sheet is long, the heat conduction speed of the heating wire is high, the temperature is rapidly increased, the heating wire is not conductive when being electrified, the heating wire can be directly touched by hands when being electrified, the phenomenon is avoided, the heating wire is free of radiation, the graphene polymerization nanometer energy heating sheet can be used for heating clothes, heating physical therapy products, heating small household appliances and the like, the safety is high, and the application prospect is wide.
The first fiber composite fabric adopts a three-layer gradient structural design of a hydrophobic bottom layer, a fiber membrane layer and a hydrophobic top layer, is compounded together in an electrostatic spinning mode, has excellent waterproof performance and oil-water separation capacity, simultaneously has the function of a water vapor transmission carrier by placing the fiber membrane layer in the middle, improves the moisture permeability and the mechanical property, and has high integral structural strength; the heating wire comprises a heating core body and a protective layer, wherein the heating core body is formed by three-dimensionally weaving a plurality of polymeric nano energy wires, and the polymeric nano energy wire fibers extend along a plurality of spatial directions and are mutually crossed, so that the integrity is good, and the defects of low strength, easiness in layering, and need of sewing and machining in other weaving methods are overcome. The heating core body formed by three-dimensional weaving has the advantages of good integrity, strong continuity, excellent flexibility, bending resistance and difficult breakage, and the protective layer comprises an insulating layer and a waterproof layer, so that the heating wire is waterproof, anti-electric shock and fireproof.
Further, according to the graphene polymerization nanometer energy heating sheet, the structure and the material of the fiber composite fabric I and the fiber composite fabric II are the same; the heating core body is formed by weaving a plurality of polymerization nanometer energy wires by a1 x 1 four-step three-dimensional weaving method; the heating core body is of a three-dimensional four-way weaving structure, the weaving angle of a right-angle column section of the heating core body positioned on the outermost side is 20.7 degrees, and the maximum offset distance between a crankshaft line of the angle column section and a straight axis of an inner column section along the transverse direction of the heating core body and in a direction of 45 degrees with the surface of the heating core body is 0.29; the thickness of the first fiber composite fabric and the thickness of the second fiber composite fabric are both 0.02-0.04 mm; the diameter of the heating wire is 1.8-2.5 mm; 0.2-0.6 mm of the protective layer.
The 1 x 1 four-step three-dimensional knitting method is to divide a movement cycle of the polymerization nano energy filaments into four steps, wherein in the first step, the polymerization nano energy filaments in different rows alternately move to the left or the right in different directions by the position of one polymerization nano energy filament; in a second step, different columns of polymeric nano-energy filaments are alternately moved in different directions up or down to a polymeric nano-energy filament position; in the third step, the moving direction of the third step is the same as that of the first step; in the fourth step, the moving direction of the fourth step is opposite to that of the second step. And (4) continuously repeating the four steps by polymerizing the nano energy wire, and finishing the weaving process by tightening movement and core body output movement. In the movement process, the position of only one polymerization nano energy wire is moved when the polymerization nano energy wire moves transversely, and the position of only one polymerization nano energy wire is moved when the polymerization nano energy wire moves longitudinally, namely the three-dimensional weaving method adopting the 1 x 1 four-step method.
In order to meet the thickness requirement of the traditional heating wire material products, the traditional heating wire material products mostly adopt a laminated form, namely a plurality of layers of two-dimensional weaves are used for reinforcing or fiber winding is used for reinforcing. The pure matrix layer exists between the two-dimensional layered structure composite material product layers, and the two-dimensional layered structure composite material product layers are easy to be layered after being stressed, so that the product is damaged and has short service life. The heating core body is of a three-dimensional four-direction weaving structure, the weaving angle of the right-angle column section located on the outermost side is 20.7 degrees, the maximum offset distance between the crankshaft line of the angle column section and the straight axis line of the inner section in the direction of 45 degrees along the transverse direction of the heating core body and the surface of the heating core body is 0.29, and therefore the heating core body is enabled to have better flexibility, bending resistance and difficulty in breaking.
Further, in the graphene polymerization nanometer energy heating sheet, the hydrophobic bottom layer and the hydrophobic top layer have the same components and mainly comprise the following components: polyvinyl chloride, multi-walled carbon nanotubes, a mixed solvent and a flame retardant; the fiber film layer mainly comprises the following components: sodium chloride, polyurethane, fluorosilane, a solvent I and a solvent II; the mixed solvent is a mixed solution of DMF and acetone; the first solvent is DMF; and the second solvent is methanol.
The hydrophobic bottom layer and the hydrophobic top layer are mainly composed of polyvinyl chloride, multi-walled carbon nanotubes, a mixed solvent and a flame retardant, polyvinylidene fluoride has low surface energy, the multi-walled carbon nanotubes are used as a reinforcement body and have good strength, elasticity, fatigue resistance and isotropy, the water resistance and the oil-water separation capacity are greatly enhanced based on the surface wettability of the polyvinylidene fluoride and the synergistic effect of the porous structure of the multi-walled carbon nanotubes, and the hydrophobic bottom layer and the hydrophobic top layer have excellent flame retardant performance and are not prone to deformation when encountering fire due to the addition of the flame retardant. The fiber membrane layer mainly comprises sodium chloride, polyurethane, fluorosilane, a solvent I and a solvent II, wherein a hydrophilic group exists in a macromolecular chain of the polyurethane, a carrier is provided for water vapor diffusion, the sodium chloride is used for adjusting the conductivity of spinning solution, so that the fiber membrane layer has a porous structure, the fluorosilane is used for grafting modification, the problems of poor hydrophobicity and large aperture when the polyurethane is independently applied are solved, and the fiber membrane layer has excellent waterproof moisture-permeable performance and high tensile strength.
Further, the graphene polymerization nanometer energy heating sheet and the polymerization nanometer energy wire are mainly composed of the following components in parts by weight: 50-60 parts of polymeric fiber, 2-5 parts of graphene, 3-4 parts of kaolin, 0.5-1.5 parts of antimony, 1-2 parts of anion powder, 5-10 parts of tourmaline, 3-4 parts of shale, 5-6 parts of ceramic balls, 2-3 parts of flame retardant, 5-6 parts of polar solvent and 1-2 parts of cross-linking agent.
The polymerized nano energy wire is added with anion powder, tourmaline and ceramic ball materials, so that the polymerized nano energy wire has the effects of air purification and health preservation, wherein the anion powder can ionize the air to generate anions, the generated anions can be combined with dust and the like in the air to increase the weight of the dust and the like, and the dust and the like can fall to the ground, so that the polymerized nano energy wire has the effect of air purification, and can also improve sleep and prevent respiratory system diseases; the anion powder, the tourmaline and the ceramic ball are matched with each other, the oxygen content of the molecules can be increased, the far infrared wave energy emitted by the tourmaline can make the water molecules resonate, and the inert water molecules become independent water molecules, so that the oxygen content of the body is increased, the cell activity is increased, the aging is delayed, and the effect of improving the blood circulation of the body has the auxiliary treatment and recovery effects on cardiovascular diseases, body pain and the like. The addition of the flame retardant enables the heating wire to have excellent flame retardant performance, and the heating wire is non-combustible and non-deformable when meeting fire. And the protective layer comprises an insulating layer and a waterproof layer, so that the heating wire is waterproof, electric shock-proof and fireproof.
Further, in the graphene polymerization nanometer energy heating sheet, the polymer fiber is one or a mixture of polyethylene, polypropylene, polyvinylidene fluoride, polytetrafluoroethylene, polyperfluoroalkoxy ester, polyphenylene sulfide, nylon, polymethyl methacrylate, polycarbonate, polyimide or polyvinyl chloride; the flame retardant is one or a mixture of aluminum hydroxide, decabromodiphenylethane, brominated polystyrene and red phosphorus; the polar solvent is one or a mixture of N, N-dimethylacetamide, N-dimethylformamide, dimethyl sulfoxide and acetone; the cross-linking agent is one or a mixture of more of diaminodiphenyl ether and pyromellitic dianhydride.
Further, in the graphene polymerization nanometer energy heating sheet, the graphene is of a single-layer structure and has a thickness of 0.8-1.2 nanometers; the anion powder comprises the following components in parts by mass: 50 parts of rare earth oxide, 25 parts of kalium feldspar powder, 20 parts of rare earth composite salt, 15 parts of hexacyclic ring stone powder and 25 parts of nano TiO.
The graphene with the thickness of 0.8-1.2 nanometers and the single-layer structure can be better combined with other materials in the preparation process, and the performance of the graphene polymerization nanometer energy heating wire is further improved.
Further, in the graphene polymerization nanometer energy heating sheet, the insulating layer is made of silica gel, and an anti-oxidation layer is arranged on the surface of the insulating layer; the silica gel comprises the following components in parts by weight: 50 parts of vulcanized low-phenyl silicone rubber, 30 parts of reinforcing filler and oxidation-resistant additive Fe2O35 parts of silicon nitrogen cross-linking agent, 2 parts of silicon micro powder, 2 parts of talcum powder and 0.5 part of silane coupling agent; the anti-oxidation layer (211) comprises the following components in parts by weight: 60 parts of dioctyldiphenylamine, 30 parts of bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite and 10 parts of pentaerythritol tetrakis (3-laurylthiopropionate).
The insulating layer is made of silica gel, and the silica gel has characteristics such as acid and alkali resistance, waterproof, high temperature resistant, long-lived. In order to further improve the performance, a layer of antioxidant is coated on the surface of the glass to form an anti-oxidation layer. The insulating layer is coated on the heating core body, so that the heating wire has excellent flexibility, bending resistance, no expansion and contraction deformation, and difficult fracture, and the safety of the heating wire in use is fully ensured.
Furthermore, according to the graphene polymerization nanometer energy heating sheet, the waterproof layer is a polyacrylate waterproof coating, and a plurality of moisture-dispersing micropores are distributed on the surface of the polyacrylate waterproof coating.
The waterproof layer is a polyacrylate waterproof coating, so that the waterproof performance is further improved, and the safety of the heating wire in use is more fully ensured. Meanwhile, the surface of the polyacrylate waterproof coating is fully distributed with a plurality of micropores for dispersing moisture, so that heat transfer is not hindered, and the service life is prolonged.
The invention also relates to the graphene polymerization nanometer energy heating sheet and a preparation method thereof, which sequentially comprises the preparation of a fiber composite fabric I and a fiber composite fabric II, the preparation of a heating wire and the preparation of the graphene polymerization nanometer energy heating sheet; the preparation of the first fiber composite fabric and the second fiber composite fabric comprises the following steps:
(1) preparing spinning solutions of a hydrophobic bottom layer and a hydrophobic top layer: adding a multi-walled carbon nanotube into a mixed solvent, carrying out ultrasonic treatment for 3-5h, then adding polyvinylidene fluoride to dissolve, continuously stirring for 4-5h at room temperature, adding a flame retardant, and continuously stirring for 5-6h to obtain spinning solutions of a hydrophobic bottom layer and a hydrophobic top layer; the addition amount of the multi-wall carbon nano tube is 1.2-1.5 wt% of the mass fraction of the spinning solution of the hydrophobic bottom layer and the hydrophobic top layer, and the addition amount of the polyvinylidene fluoride solution is 18-20 wt% of the mass fraction of the mixed solvent; the addition amount of the flame retardant is 0.5-1.0 wt% of the mass fraction of the spinning solution of the hydrophobic bottom layer and the hydrophobic top layer;
(2) preparing a spinning solution of a fiber film layer: adding sodium chloride into the first solvent, stirring at room temperature for 0.5h, then adding polyurethane, and continuously stirring at room temperature for 18-10h to obtain a spinning solution of a fiber membrane layer; the addition amount of the sodium chloride is 0.01-0.02 wt% of the mass fraction of the spinning solution of the fiber membrane layer; the addition amount of the polyurethane is 20-22 wt% of the mass fraction of the first solvent;
(3) preparing a first fiber composite fabric and a second fiber composite fabric: and simultaneously putting the spinning solution of the hydrophobic bottom layer and the hydrophobic top layer and the spinning solution of the fiber film layer into an electrostatic spinning machine, preparing the hydrophobic bottom layer, the fiber film layer and the fibers of the hydrophobic top layer from inside to outside by a continuous electrostatic spinning method, stacking the fibers to form a three-dimensional reticular structure, wherein the spinning voltage is 20kV, and the solution flow rate is 0.8-1.0ml/h, so as to obtain a first fiber composite fabric and a second fiber composite fabric.
The invention adopts the electrostatic spinning technology, the preparation process is simple and easy to adjust, the fiber length-diameter ratio is large, the specific surface area is large, and the like, the hydrophobic bottom layer, the fiber film layer and the hydrophobic top layer are prepared from the fiber composite fabric I and the fiber composite fabric II, the fibers of the hydrophobic bottom layer, the fiber film layer and the hydrophobic top layer from inside to outside are stacked to form a three-dimensional net structure, a large number of pores are arranged in the middle of the three-dimensional net structure, the pores provide a large number of channels for the passage of water vapor and air flow, the moisture permeability is improved, and meanwhile, the hydrophobic bottom layer and the hydrophobic top layer on the two sides can prevent the passage of water.
Further, in the preparation method of the graphene polymerization nanometer energy heating sheet, the step (2) of preparing the first fiber composite fabric and the second fiber composite fabric further includes the following steps: and adding fluorosilane into a second solvent, performing ultrasonic treatment for 1-2 hours to obtain a mixed solution, adding the mixed solution into the spinning solution of the fiber film layer, and continuously stirring at room temperature for 8-10 hours to obtain the treated spinning solution of the fiber film layer.
Further, the preparation method of the graphene polymerization nanometer energy heating sheet comprises the following steps:
(1) ultrasonically dispersing graphene in a polar solvent, continuously stirring until the graphene is dissolved, adding a cross-linking agent for multiple times, introducing nitrogen into a container for protection, and then reacting at a low temperature to obtain a graphene mixed solution;
(2) mixing polymeric fibers, kaolin, anion powder, tourmaline, shale, ceramic balls and a flame retardant, melting at 600 ℃ under a vacuum condition, adding a graphene mixed solution, and uniformly stirring to obtain a spinning solution;
(3) standing the spinning solution, placing the spinning solution into drawing equipment after vacuum deaeration, introducing nitrogen into the drawing equipment, pressurizing the spinning solution by nitrogen, forming and drawing at a set specification, winding the spinning solution on a take-up roller after coagulating bath, taking the spinning solution off from the take-up roller, and drying the spinning solution in a vacuum drying oven to obtain a polymerized nano energy wire; the coagulating bath is a mixed solution of water and ethanol, wherein the volume ratio of the water to the ethanol is 2:1, the temperature of the coagulating bath is 40 ℃, the spinning pressure is 0.4-0.6 Mpa, and the drawing speed is 30-40 m/min;
(4) three-dimensional weaving is adopted for the polymerization nanometer energy wire, and a heating core body is obtained;
(5) and coating the protective layer on the heating core body, drying in a constant-temperature vacuum drying oven at 300 ℃, and cooling to room temperature to obtain the graphene polymerization nanometer energy heating sheet.
Further, the preparation method of the graphene polymerization nanometer energy heating sheet comprises the following steps: and embroidering the heating wire on the first fiber composite fabric in a roundabout and winding shape in a computer embroidery mode, wherein the first fiber composite fabric is tightly connected with the second fiber composite fabric in a gluing mode, and the heating wire is clamped between the first fiber composite fabric and the second fiber composite fabric.
Compared with the prior art, the invention has the following beneficial effects:
(1) the graphene polymerization nanometer energy heating sheet disclosed by the invention is reasonable in structural design, the heating wire is embroidered on the first fiber composite fabric in a roundabout and winding shape in a computer embroidery mode, and the first fiber composite fabric and the second fiber composite fabric tightly clamp the heating wire in the middle, so that the heating effect of the graphene polymerization nanometer energy heating sheet is ensured, the heating efficiency is greatly improved, the integrity of the graphene polymerization nanometer energy heating sheet is good, the graphene polymerization nanometer energy heating sheet has excellent flexibility, bending resistance and long service life, and is not easy to bend;
(2) according to the graphene polymerization nanometer energy heating sheet disclosed by the invention, the first fiber composite fabric adopts a three-layer gradient structure design of a hydrophobic bottom layer, a fiber film layer and a hydrophobic top layer, and is compounded together in an electrostatic spinning mode, so that the graphene polymerization nanometer energy heating sheet has excellent waterproof performance and oil-water separation capability, meanwhile, the fiber film layer is placed in the middle to play a role of a water vapor transmission carrier, the moisture permeability and mechanical properties are improved, the water resistance, the oil resistance, the electric shock resistance, the fire resistance and the moisture permeability are good, and the safety is improved;
(3) the graphene polymerization nanometer energy heating sheet and the preparation method thereof have the advantages that the preparation method is simple, the flexibility is high, and the requirements of different occasions are met;
(4) the heating core body is formed by three-dimensionally weaving a plurality of polymeric nano energy wires, and the polymeric nano energy wire fibers extend along a plurality of spatial directions and are mutually crossed, so that the integrity is good, and the defects of low strength, easiness in layering, and need of sewing and machining of other weaving methods are overcome;
(5) the hydrophobic bottom layer and the hydrophobic top layer are based on the synergistic effect of the surface wettability of polyvinylidene fluoride and the porous structure of the multi-walled carbon nanotube, the waterproofness and the oil-water separation capability are greatly enhanced, and the hydrophobic bottom layer and the hydrophobic top layer have excellent flame retardant performance and do not deform when encountering fire due to the addition of the flame retardant; the fiber film layer has excellent waterproof and moisture-permeable performances and high tensile strength;
(6) the polymerization nanometer energy silk fiber is safe and radiationless, has high heating speed and long duration, can basically have no failure, and improves the service life; the polymerized nanometer energy silk fiber can also emit light waves of 6-16 microns to a human body in a nanometer far infrared mode, and can stimulate acupuncture points, dredge channels, improve local blood circulation and promote metabolism when being applied to heating clothes and heating physical therapy products through reasonable and slow release of heat, so that the fiber has the characteristics of convenience in use, safety, environmental protection and the like; has physiotherapy effect, and can generate negative oxygen ion after heating, and the released negative oxygen ion can activate human body cell, enhance cell activity, purify air, and is beneficial to human health.
Drawings
Fig. 1 is a first structural schematic diagram of a graphene polymerization nanometer energy heating sheet according to the present invention;
FIG. 2 is a schematic structural diagram II of a graphene polymerization nanometer energy heating sheet according to the present invention;
fig. 3 is a third schematic structural diagram of a graphene polymerization nanometer energy heating sheet according to the present invention;
FIG. 4 is a schematic structural view of a fiber composite fabric of the graphene polymerization nanometer energy heating sheet according to the present invention;
FIG. 5 is a schematic structural view of a heater of the graphene polymerization nanometer energy heating sheet according to the present invention;
fig. 6 is a schematic structural diagram of a heating core body of the graphene polymerization nanometer energy heating sheet knitted by a1 × 1 four-step three-dimensional knitting method according to the present invention;
fig. 7 is a schematic diagram of a weaving angle of a right-angle column section of a heating core of the graphene polymerization nanometer energy heating sheet located at the outermost side according to the present invention;
FIG. 8 is a schematic view of the orientation of a coordinate system of a crankshaft line of a corner column section and a straight axis line of an internal section of a heating core of the graphene polymerization nanometer energy heating sheet according to the present invention;
in the figure: the heat-insulation composite heat-insulation material comprises a first fiber composite fabric 1, a heating wire 2, a heating core body 21, a polymerization nanometer energy wire 211, a protective layer 22, an insulating layer 221, a waterproof layer 222, an anti-oxidation layer 223, micropores 224, a second fiber composite fabric 3, a hydrophobic bottom layer 11, a fiber membrane layer 12, a hydrophobic top layer 13, a right-angle column section and a b inner column section; c weaving angle, d right angle column section crankshaft line and inner column section straight axis line maximum offset distance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to specific experimental data and accompanying drawings 1 to 8, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following embodiment provides a graphene polymerization nano energy heating sheet and a preparation method thereof, and the graphene polymerization nano energy heating sheet with the structure shown in fig. 1-3 comprises a fiber composite fabric I1, a heating wire 2 and a fiber composite fabric II 3 from inside to outside, wherein the heating wire 2 is embroidered on the fiber composite fabric I1 in a winding shape in a computer embroidery mode, the fiber composite fabric I1 is tightly connected with the fiber composite fabric II 3 in a gluing mode, and the heating wire 2 is clamped between the fiber composite fabric I1 and the fiber composite fabric II 3; as shown in fig. 4, the fiber composite fabric 1 comprises a hydrophobic bottom layer 11, a fiber membrane layer 12 and a hydrophobic top layer 13 from inside to outside, and the hydrophobic bottom layer 11, the fiber membrane layer 12 and the hydrophobic top layer 13 are stacked by fibers in an electrostatic spinning manner to form a three-dimensional mesh structure; as shown in fig. 5, the heating wire 2 includes a heating core 21 and a protective layer 22, the heating core 21 is formed by three-dimensionally weaving a plurality of polymeric nano-energy wires 211, and the protective layer 22 includes an insulating layer 221 and a waterproof layer 222 which are sequentially arranged from inside to outside and tightly covers the heating core 21.
As shown in fig. 6, 7 and 8, the structure and the material of the fiber composite fabric one 1 and the fiber composite fabric two 3 are the same; the heating core body 21 is formed by weaving a plurality of polymerization nanometer energy wires 211 by a1 x 1 four-step three-dimensional weaving method. The heating core body 21 has a three-dimensional four-way weaving structure, the weaving angle c of the right-angle column section a of the heating core body 21 positioned at the outermost side is 20.7 degrees, and the maximum offset distance d between the crankshaft line of the right-angle column section a and the straight axis line of the inner column section b along the transverse direction of the heating core body 21 and in the direction of 45 degrees with the surface of the heating core body 21 is 0.29. The thicknesses of the first fiber composite fabric 1 and the second fiber composite fabric 3 are both 0.02-0.04 mm. The diameter of the heating wire 2 is 1.8-2.5 mm. 0.2-0.6 mm of the protective layer 22.
Further, the hydrophobic bottom layer 11 and the hydrophobic top layer 13 have the same composition and mainly consist of the following components: polyvinyl chloride, multi-walled carbon nanotubes, a mixed solvent and a flame retardant; the fiber membrane layer 12 is mainly composed of the following components: sodium chloride, polyurethane, fluorosilane, a solvent I and a solvent II; the mixed solvent is a mixed solution of DMF and acetone; the first solvent is DMF; and the second solvent is methanol.
Further, the polymeric nano energy filament 211 is mainly composed of the following components in parts by weight: 50-60 parts of polymeric fiber, 2-5 parts of graphene, 3-4 parts of kaolin, 0.5-1.5 parts of antimony, 1-2 parts of anion powder, 5-10 parts of tourmaline, 3-4 parts of shale, 5-6 parts of ceramic balls, 2-3 parts of flame retardant, 5-6 parts of polar solvent and 1-2 parts of cross-linking agent.
Further, the polymeric fiber is one or a mixture of polyethylene, polypropylene, polyvinylidene fluoride, polytetrafluoroethylene, polyperfluoroalkoxy ester, polyphenylene sulfide, nylon, polymethyl methacrylate, polycarbonate, polyimide or polyvinyl chloride; the flame retardant is one or a mixture of aluminum hydroxide, decabromodiphenylethane, brominated polystyrene and red phosphorus; the polar solvent is one or a mixture of N, N-dimethylacetamide, N-dimethylformamide, dimethyl sulfoxide and acetone; the cross-linking agent is one or a mixture of more of diaminodiphenyl ether and pyromellitic dianhydride.
Furthermore, the graphene is of a single-layer structure, and the thickness of the graphene is 0.8-1.2 nanometers. The anion powder comprises the following components in parts by mass: 50 parts of rare earth oxide, 25 parts of kalite powder, 20 parts of rare earth composite salt, 15 parts of hexacyclic ring stone powder and nano TiO25 parts of the raw materials.
Further, as shown in fig. 1, the insulating layer 221 is made of silica gel, and an anti-oxidation layer 223 is disposed on the surface of the insulating layer 221; the silica gel comprises the following components in parts by weight: 50 parts of vulcanized low-phenyl silicone rubber, 30 parts of reinforcing filler, 35 parts of oxidation-resistant additive Fe2O, 2 parts of silicon nitrogen cross-linking agent, 1 part of silicon micropowder, 2 parts of talcum powder and 0.5 part of silane coupling agent; the anti-oxidation layer (211) comprises the following components in parts by weight: 60 parts of dioctyldiphenylamine, 30 parts of bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite and 10 parts of pentaerythritol tetrakis (3-laurylthiopropionate). The waterproof layer 222 is a polyacrylate waterproof coating, and a plurality of moisture-permeable micropores 224 are distributed on the surface of the waterproof layer 222.
Example 1
The preparation method of the graphene polymerization nanometer energy heating sheet is characterized by sequentially comprising the steps of preparing a fiber composite fabric I1 and a fiber composite fabric II 3, preparing a heating wire 2 and preparing the graphene polymerization nanometer energy heating sheet.
The preparation of the first fiber composite fabric 1 and the second fiber composite fabric 3 comprises the following steps:
(1) preparation of the spinning dope for the hydrophobic bottom layer 11 and the hydrophobic top layer 13: adding a multi-walled carbon nanotube into a mixed solvent, carrying out ultrasonic treatment for 3-5h, then adding polyvinylidene fluoride to dissolve, continuously stirring for 4-5h at room temperature, adding a flame retardant, and continuously stirring for 5-6h to obtain spinning solutions of a hydrophobic bottom layer 11 and a hydrophobic top layer 13; the addition amount of the multi-wall carbon nano tube is 1.2-1.5 wt% of the mass fraction of the spinning solution of the hydrophobic bottom layer 11 and the hydrophobic top layer 13, and the addition amount of the polyvinylidene fluoride solution is 18-20 wt% of the mass fraction of the mixed solvent; the addition amount of the flame retardant is 0.5-1.0 wt% of the mass fraction of the spinning solution of the hydrophobic bottom layer 11 and the hydrophobic top layer 13;
(2) preparation of spinning solution of the fiber membrane layer 12: adding sodium chloride into the first solvent, stirring for 0.5h at room temperature, then adding polyurethane, and continuously stirring for 18-10h at room temperature to obtain a spinning solution of the fiber membrane layer 12; the addition amount of the sodium chloride is 0.01-0.02 wt% of the mass fraction of the spinning solution of the fiber membrane layer 12; the addition amount of the polyurethane is 20-22 wt% of the mass fraction of the first solvent;
(3) preparing a first fiber composite fabric 1 and a second fiber composite fabric 3: and simultaneously putting the spinning solutions of the hydrophobic bottom layer 11 and the hydrophobic top layer 13 and the spinning solution of the fiber film layer 12 into an electrostatic spinning machine, preparing the hydrophobic bottom layer 11, the fiber film layer 12 and the hydrophobic top layer 13 by a continuous electrostatic spinning method, stacking the fibers from inside to outside to form a three-dimensional net-shaped structure, wherein the spinning voltage is 20kV, and the solution flow rate is 0.8-1.0ml/h, so as to obtain a fiber composite fabric I1 and a fiber composite fabric II 3.
The preparation of the heating wire (2) comprises the following steps:
(1) ultrasonically dispersing graphene in a polar solvent, continuously stirring until the graphene is dissolved, adding a cross-linking agent for multiple times, introducing nitrogen into a container for protection, and then reacting at a low temperature to obtain a graphene mixed solution;
(2) mixing polymeric fibers, kaolin, anion powder, tourmaline, shale, ceramic balls and a flame retardant, melting at 600 ℃ under a vacuum condition, adding a graphene mixed solution, and uniformly stirring to obtain a spinning solution;
(3) standing the spinning solution, placing the spinning solution into a drawing device after vacuum deaeration, introducing nitrogen into the drawing device, pressurizing the spinning solution with nitrogen, forming and drawing at a set specification, winding the spinning solution on a take-up roller after coagulating bath, taking the spinning solution off from the take-up roller, and drying the spinning solution in a vacuum drying oven to obtain a polymerized nano energy wire 211; the coagulating bath is a mixed solution of water and ethanol, wherein the volume ratio of the water to the ethanol is 2:1, the temperature of the coagulating bath is 40 ℃, the spinning pressure is 0.4-0.6 Mpa, and the drawing speed is 30-40 m/min;
(4) three-dimensional weaving is adopted for the polymerization nanometer energy wire 211, and a heating core body 21 is obtained;
(5) and coating the protective layer 22 on the heating core body 21, drying in a constant-temperature vacuum drying oven at 300 ℃, and cooling to room temperature to obtain the graphene polymerization nanometer energy heating sheet.
The preparation method of the graphene polymerization nanometer energy heating sheet comprises the following steps: the heating wire 2 is embroidered on the first fiber composite fabric 1 in a roundabout and winding shape in a computer embroidery mode, the second fiber composite fabric 3 is tightly connected with the second fiber composite fabric 3 in a gluing mode, and the heating wire 2 is clamped between the first fiber composite fabric 1 and the second fiber composite fabric 3.
Example 2
The preparation method of the graphene polymerization nanometer energy heating sheet is characterized by sequentially comprising the steps of preparing a fiber composite fabric I1 and a fiber composite fabric II 3, preparing a heating wire 2 and preparing the graphene polymerization nanometer energy heating sheet.
The preparation of the first fiber composite fabric 1 and the second fiber composite fabric 3 comprises the following steps:
(1) preparation of the spinning dope for the hydrophobic bottom layer 11 and the hydrophobic top layer 13: adding a multi-walled carbon nanotube into a mixed solvent, carrying out ultrasonic treatment for 3-5h, then adding polyvinylidene fluoride to dissolve, continuously stirring for 4-5h at room temperature, adding a flame retardant, and continuously stirring for 5-6h to obtain spinning solutions of a hydrophobic bottom layer 11 and a hydrophobic top layer 13; the addition amount of the multi-wall carbon nano tube is 1.2-1.5 wt% of the mass fraction of the spinning solution of the hydrophobic bottom layer 11 and the hydrophobic top layer 13, and the addition amount of the polyvinylidene fluoride solution is 18-20 wt% of the mass fraction of the mixed solvent; the addition amount of the flame retardant is 0.5-1.0 wt% of the mass fraction of the spinning solution of the hydrophobic bottom layer 11 and the hydrophobic top layer 13;
(2) preparation of spinning solution of the fiber membrane layer 12: adding sodium chloride into the first solvent, stirring for 0.5h at room temperature, then adding polyurethane, and continuously stirring for 18-10h at room temperature to obtain a spinning solution of the fiber membrane layer 12; the addition amount of the sodium chloride is 0.01-0.02 wt% of the mass fraction of the spinning solution of the fiber membrane layer 12; the addition amount of the polyurethane is 20-22 wt% of the mass fraction of the first solvent; adding fluorosilane into a second solvent, carrying out ultrasonic treatment for 1-2 hours to obtain a mixed solution, adding the mixed solution into the spinning solution of the fiber film layer 12, and continuously stirring at room temperature for 8-10 hours to obtain the treated spinning solution of the fiber film layer 12;
(3) preparing a first fiber composite fabric 1 and a second fiber composite fabric 3: and simultaneously putting the spinning solutions of the hydrophobic bottom layer 11 and the hydrophobic top layer 13 and the spinning solution of the fiber film layer 12 into an electrostatic spinning machine, preparing the hydrophobic bottom layer 11, the fiber film layer 12 and the hydrophobic top layer 13 by a continuous electrostatic spinning method, stacking the fibers from inside to outside to form a three-dimensional net-shaped structure, wherein the spinning voltage is 20kV, and the solution flow rate is 0.8-1.0ml/h, so as to obtain a fiber composite fabric I1 and a fiber composite fabric II 3.
The preparation of the heating wire 2 comprises the following steps:
(1) ultrasonically dispersing graphene in a polar solvent, continuously stirring until the graphene is dissolved, adding a cross-linking agent for multiple times, introducing nitrogen into a container for protection, and then reacting at a low temperature to obtain a graphene mixed solution;
(2) mixing polymeric fibers, kaolin, anion powder, tourmaline, shale, ceramic balls and a flame retardant, melting at 600 ℃ under a vacuum condition, adding a graphene mixed solution, and uniformly stirring to obtain a spinning solution;
(3) standing the spinning solution, placing the spinning solution into a drawing device after vacuum deaeration, introducing nitrogen into the drawing device, pressurizing the spinning solution with nitrogen, forming and drawing at a set specification, winding the spinning solution on a take-up roller after coagulating bath, taking the spinning solution off from the take-up roller, and drying the spinning solution in a vacuum drying oven to obtain a polymerized nano energy wire 211; the coagulating bath is a mixed solution of water and ethanol, wherein the volume ratio of the water to the ethanol is 2:1, the temperature of the coagulating bath is 40 ℃, the spinning pressure is 0.4-0.6 Mpa, and the drawing speed is 30-40 m/min;
(4) three-dimensional weaving is adopted for the polymerization nanometer energy wire 211, and a heating core body 21 is obtained;
(5) and coating the protective layer 22 on the heating core body 21, drying in a constant-temperature vacuum drying oven at 300 ℃, and cooling to room temperature to obtain the graphene polymerization nanometer energy heating sheet.
The preparation method of the graphene polymerization nanometer energy heating sheet comprises the following steps: the heating wire 2 is embroidered on the first fiber composite fabric 1 in a roundabout and winding shape in a computer embroidery mode, the second fiber composite fabric 3 is tightly connected with the second fiber composite fabric 3 in a gluing mode, and the heating wire 2 is clamped between the first fiber composite fabric 1 and the second fiber composite fabric 3.
Effect verification:
the graphene polymerization nanometer energy heating sheet obtained in the above embodiment 1 and embodiment 2 passes RoHS (content of 10 kinds of limiting substances), and the test method comprises IEC 62321-5:2013 and IEC 62321-4: 2013+ A1:2017, IEC 62321-7-1:2015, IEC 62321-7-2:2017, IEC 62321-6:2015 and IEC 62321-8:2017, and ICP-OES and UV & GC-MS are used for analysis.
The performance of the heating wire of the graphene polymerization nanometer energy heating sheet obtained in the above example 1 and example 2 was tested according to the following criteria, and the test results are shown in table 1. Reference is made to GB/T2951-2008 general test method-mechanical property test for insulation and sheathing materials of cables and optical cables;
reference is made to GB/T3048.5-2007 electric property test method for electric wires and cables part 5: insulation resistance test ";
testing the flame retardant performance by referring to GB/T8625, GB/T14402 and GB/T14403, and evaluating the flame retardant grade of the flame retardant performance;
TABLE 1 heater Performance test results
The performance of the first fiber composite fabric (the second fiber composite fabric) of the graphene polymerization nano energy heating sheet obtained in the above examples 1 and 2 was measured according to the following criteria, and the measurement results are shown in table 2.
Waterproof performance: the waterproof performance (hydrostatic pressure) of the fiber composite fabric I (fiber composite fabric II) is measured by a hydrostatic pressure tester according to the AATCC 127 standard measurement method.
Moisture permeability: fiber composite face one (fiber composite face two) was measured according to ASTM E96-CaCl 2 standard desiccant method using a water vapor transmission tester.
Oil-water separation performance: (1) oil absorption capacity: immersing a first fiber composite fabric (a second fiber composite fabric) sample with the same area and thickness into oil, taking the sample out of the oil after 1min, wiping the sample by using filter paper to remove redundant oil on the surface, and calculating the oil absorption capacity K according to the formula K ═ mt-mi)/mi, wherein mi and mt are the weight of the sample before and after oil absorption respectively; (2) oil flux: calculating by measuring the time a volume of oil permeates through the sample; (3) oil-water separation capacity: the test was performed by an oil-water separation test in which an oil/water mixture consisting of 10ml of oil and 10ml of water was directly poured into a separation apparatus to separate the oil-water mixture by the sample, and the separated liquid was collected to determine the separation efficiency. The calculation formula of the sample separation efficiency is q ═ Vl/Vo, wherein Vo and V1 are the volumes of oil before and after oil-water separation.
Flame retardant property: the Limit Oxygen Index (LOI) test was carried out using an FTT0002 type oxygen index measuring instrument from Fire Testing Technology, according to the GB/T5455-2008 standard.
Table 2 fiber composite fabric one (fiber composite fabric two) test results
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (10)
1. The graphene polymerization nanometer energy heating sheet is characterized by comprising a first fiber composite fabric (1), a heating wire (2) and a second fiber composite fabric (3) from inside to outside, wherein the heating wire (2) is embroidered on the first fiber composite fabric (1) in a winding shape in a computer embroidery mode, the first fiber composite fabric (1) is tightly connected with the second fiber composite fabric (3) in a gluing mode, and the heating wire (2) is clamped between the first fiber composite fabric (1) and the second fiber composite fabric (3); the first fiber composite fabric (1) comprises a hydrophobic bottom layer (11), a fiber membrane layer (12) and a hydrophobic top layer (13), wherein the hydrophobic bottom layer (11), the fiber membrane layer (12) and the hydrophobic top layer (13) are stacked from inside to outside in an electrostatic spinning mode to form a three-dimensional net-shaped structure; the heating wire (2) comprises a heating core body (21) and a protective layer (22), the heating core body (21) is formed by three-dimensionally weaving a plurality of polymerization nanometer energy wires (211), and the protective layer (22) comprises an insulating layer (221) and a waterproof layer (222) which are sequentially arranged from inside to outside and tightly covers the heating core body (21).
2. The graphene polymerization nanometer energy heating sheet according to claim 1, wherein the structure and the material of the fiber composite fabric I (1) and the fiber composite fabric II (3) are the same; the heating core body (21) is formed by weaving a plurality of polymerization nanometer energy wires (211) by a1 x 1 four-step three-dimensional weaving method; the heating core body (21) has a three-dimensional four-way weaving structure, the weaving angle of a right-angle column section of the heating core body (21) positioned at the outermost side is 20.7 degrees, and the maximum offset distance between a crankshaft line of the angle column section and a straight axis of an inner column section along the transverse direction of the heating core body (21) and in a direction forming an angle of 45 degrees with the surface of the heating core body (21) is 0.29; the thicknesses of the first fiber composite fabric (1) and the second fiber composite fabric (3) are both 0.02-0.04 mm; the diameter of the heating wire (2) is 1.8-2.5 mm; 0.2-0.6 mm of the protective layer (22).
3. The graphene polymeric nano energy heating sheet according to claim 1, wherein the hydrophobic bottom layer (11) and the hydrophobic top layer (13) have the same composition and mainly consist of the following components: polyvinyl chloride, multi-walled carbon nanotubes, a mixed solvent and a flame retardant; the fiber film layer (12) is mainly composed of the following components: sodium chloride, polyurethane, fluorosilane, a solvent I and a solvent II; the mixed solvent is a mixed solution of DMF and acetone; the first solvent is DMF; the second solvent is methanol; the polymerization nanometer energy wire (211) mainly comprises the following components in parts by weight: 50-60 parts of polymeric fiber, 2-5 parts of graphene, 3-4 parts of kaolin, 0.5-1.5 parts of antimony, 1-2 parts of anion powder, 5-10 parts of tourmaline, 3-4 parts of shale, 5-6 parts of ceramic balls, 2-3 parts of flame retardant, 5-6 parts of polar solvent and 1-2 parts of cross-linking agent.
4. The graphene polymerization nanometer energy heating sheet according to claim 3, wherein the polymer fiber is one or a mixture of polyethylene, polypropylene, polyvinylidene fluoride, polytetrafluoroethylene, polyperfluoroalkoxy ester, polyphenylene sulfide, nylon, polymethyl methacrylate, polycarbonate, polyimide or polyvinyl chloride; the flame retardant is one or a mixture of aluminum hydroxide, decabromodiphenylethane, brominated polystyrene and red phosphorus; the polar solvent is one or a mixture of N, N-dimethylacetamide, N-dimethylformamide, dimethyl sulfoxide and acetone; the cross-linking agent is one or a mixture of more of diaminodiphenyl ether and pyromellitic dianhydride.
5. The graphene polymerization nanometer energy heating sheet according to claim 4, wherein the graphene is of a single-layer structure and has a thickness of 0.8-1.2 nm; the anion powder comprises the following components in parts by mass: 50 parts of rare earth oxide, 25 parts of kalium feldspar powder, 20 parts of rare earth composite salt, 15 parts of hexacyclic ring stone powder and 25 parts of nano TiO.
6. The graphene polymerization nanometer energy heating sheet according to claim 1, wherein the insulating layer (221) is made of silica gel, and an anti-oxidation layer (223) is arranged on the surface of the insulating layer (221); the silica gel comprises the following components in parts by weight: 50 parts of vulcanized low-phenyl silicone rubber, 30 parts of reinforcing filler, 35 parts of oxidation-resistant additive Fe2O, 2 parts of silicon nitrogen cross-linking agent, 1 part of silicon micropowder, 2 parts of talcum powder and 0.5 part of silane coupling agent; the anti-oxidation layer (211) comprises the following components in parts by weight: 60 parts of dioctyldiphenylamine, 30 parts of bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite and 10 parts of pentaerythritol tetrakis (3-laurylthiopropionate); the waterproof layer (222) is a polyacrylate waterproof coating, and a plurality of moisture-permeable micropores (224) are distributed on the surface of the waterproof layer (222).
7. The preparation method of the graphene polymerization nano energy heating sheet according to any one of claims 1 to 6, which comprises the steps of preparing a fiber composite fabric I (1) and a fiber composite fabric II (2), preparing a heating wire (2), and preparing the graphene polymerization nano energy heating sheet in sequence; the preparation of the fiber composite fabric I (1) and the fiber composite fabric II (2) comprises the following steps:
(1) preparing spinning solutions of a hydrophobic bottom layer (11) and a hydrophobic top layer (13): adding a multi-walled carbon nanotube into a mixed solvent, carrying out ultrasonic treatment for 3-5h, then adding polyvinylidene fluoride to dissolve, continuously stirring for 4-5h at room temperature, adding a flame retardant, and continuously stirring for 5-6h to obtain spinning solutions of a hydrophobic bottom layer (11) and a hydrophobic top layer (13); the addition amount of the multi-wall carbon nano tube is 1.2-1.5 wt% of the mass fraction of the spinning solution of the hydrophobic bottom layer (11) and the hydrophobic top layer (13), and the addition amount of the polyvinylidene fluoride solution is 18-20 wt% of the mass fraction of the mixed solvent; the addition amount of the flame retardant is 0.5-1.0 wt% of the mass fraction of the spinning solution of the hydrophobic bottom layer (11) and the hydrophobic top layer (13);
(2) preparing a spinning solution of the fiber film layer (12): adding sodium chloride into the first solvent, stirring for 0.5h at room temperature, then adding polyurethane, and continuously stirring for 18-10h at room temperature to obtain a spinning solution of a fiber membrane layer (12); the addition amount of the sodium chloride is 0.01-0.02 wt% of the mass fraction of the spinning solution of the fiber membrane layer (12); the addition amount of the polyurethane is 20-22 wt% of the mass fraction of the first solvent;
(3) preparing a first fiber composite fabric (1) and a second fiber composite fabric (2): and (2) simultaneously putting the spinning solution of the hydrophobic bottom layer (11), the spinning solution of the hydrophobic top layer (13) and the spinning solution of the fiber membrane layer (12) into an electrostatic spinning machine, preparing the hydrophobic bottom layer (11), the fiber membrane layer (12) and the fibers of the hydrophobic top layer (13) from inside to outside by a continuous electrostatic spinning method, stacking the fibers to form a three-dimensional reticular structure, wherein the spinning voltage is 20kV, and the solution flow rate is 0.8-1.0ml/h, so as to obtain a fiber composite fabric I (1) and a fiber composite fabric II (2).
8. The preparation method of the graphene polymerization nano energy heating sheet according to claim 7, wherein the step (2) of preparing the first fiber composite fabric (1) and the second fiber composite fabric (2) further comprises the following steps: and adding fluorosilane into a second solvent, carrying out ultrasonic treatment for 1-2h to obtain a mixed solution, adding the mixed solution into the spinning solution of the fiber film layer (12), and continuously stirring for 8-10h at room temperature to obtain the treated spinning solution of the fiber film layer (12).
9. The preparation method of the graphene polymerization nanometer energy heating sheet according to claim 7, wherein the preparation of the heating wire (2) comprises the following steps:
(1) ultrasonically dispersing graphene in a polar solvent, continuously stirring until the graphene is dissolved, adding a cross-linking agent for multiple times, introducing nitrogen into a container for protection, and then reacting at a low temperature to obtain a graphene mixed solution;
(2) mixing polymeric fibers, kaolin, anion powder, tourmaline, shale, ceramic balls and a flame retardant, melting at 600 ℃ under a vacuum condition, adding a graphene mixed solution, and uniformly stirring to obtain a spinning solution;
(3) standing the spinning solution, placing the spinning solution into a drawing device after vacuum deaeration, introducing nitrogen into the drawing device, pressurizing the spinning solution by nitrogen, forming and drawing at a set specification, winding the spinning solution on a take-up roller after coagulating bath, taking the spinning solution off from the take-up roller, and drying the spinning solution in a vacuum drying oven to obtain a polymerized nano energy wire (211); the coagulating bath is a mixed solution of water and ethanol, wherein the volume ratio of the water to the ethanol is 2:1, the temperature of the coagulating bath is 40 ℃, the spinning pressure is 0.4-0.6 Mpa, and the drawing speed is 30-40 m/min;
(4) three-dimensional weaving is adopted for the polymerization nanometer energy wire (211) to obtain a heating core body (21);
(5) and coating the protective layer (22) on the heating core body (21), drying in a constant-temperature vacuum drying oven at 300 ℃, and cooling to room temperature to obtain the graphene polymerization nanometer energy heating sheet.
10. The preparation method of the graphene polymerization nanometer energy heating sheet according to claim 9, wherein the preparation method of the graphene polymerization nanometer energy heating sheet comprises the following steps: the heating wire (2) is embroidered on the first fiber composite fabric (1) in a roundabout and winding shape in a computer embroidery mode, the second fiber composite fabric (3) is tightly connected with the second fiber composite fabric (3) in a gluing mode, and the heating wire (2) is clamped between the first fiber composite fabric (1) and the second fiber composite fabric (3).
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| CN114989529B (en) * | 2022-04-23 | 2023-08-11 | 星空男孩(杭州)科技有限公司 | Environment-friendly composite surface sheet layer and preparation method and application method thereof |
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