CN110769530A - High-voltage-resistant graphene heating film for conductive fiber material electrode and preparation method thereof - Google Patents
High-voltage-resistant graphene heating film for conductive fiber material electrode and preparation method thereof Download PDFInfo
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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
- H05B3/20—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
-
- 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
- H05B3/02—Details
-
- 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
- H05B3/145—Carbon only, e.g. carbon black, graphite
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Abstract
The invention belongs to the field of graphene, and particularly relates to a high-voltage-resistant graphene heating film and a heating sheet for a conductive fiber material electrode and a preparation method of the high-voltage-resistant graphene heating film and the heating sheet. The graphene heating film comprises a high-voltage-resistant fiber conductive electrode layer, graphene conductive layers arranged on two sides of the high-voltage-resistant fiber conductive electrode layer and a supporting layer arranged on the outer side of the graphene conductive layer; insulating glue leakage-proof layers are arranged at the edges of two sides of the graphene conducting layer; the high-voltage-resistant fiber conductive electrode layer is connected with the bus bar. At present, the mainstream graphene heating film is loaded with a voltage below 12V and is used for heating clothes and physiotherapy products; the graphene electric heater unit or drying equipment is applied to the graphene electric heater unit or drying equipment with 220V or 380V alternating current and has high voltage resistance, ageing resistance and high insulating property.
Description
Technical Field
The invention belongs to the field of graphene, and particularly relates to a high-voltage-resistant graphene heating film and a heating sheet for a conductive fiber material electrode and a preparation method of the high-voltage-resistant graphene heating film and the heating sheet.
Background
The coal-fired heating in winter causes serious pollution, and in order to effectively improve the current situation of environmental pollution and realize sustainable development, the most effective method is to carry out coal-to-electricity engineering. Graphene is a quasi-two-dimensional material with the thickness of only one atomic layer, has the characteristics of high strength, super heat conductivity and super conductivity, and the special microstructure determines that the graphene material has the advantages of high heat generation speed, extremely high heat conversion rate, stable property and long service life. Therefore, the graphene material is the most ideal electric heating material at present. In order to meet the requirements of high-power heating and drying, 220V or 380V alternating current is adopted, so that the graphene heating film with high voltage resistance, ageing resistance and high insulation is required to be invented.
Disclosure of Invention
The invention aims to provide a high-voltage-resistant graphene heating film and a heating sheet for a conductive fiber material electrode and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-voltage-resistant graphene heating film of a conductive fiber material electrode comprises a high-voltage-resistant fiber conductive electrode layer, graphene conductive layers arranged on two sides of the high-voltage-resistant fiber conductive electrode layer and a supporting layer arranged on the outer side of the graphene conductive layers; insulating glue leakage-proof layers are arranged at the edges of two sides of the graphene conducting layer; the high-voltage-resistant fiber conductive electrode layer is connected with the bus bar.
The high-voltage resistant fiber conductive electrode layer comprises three high-voltage resistant fiber conductive electrodes which are sequentially arranged from top to bottom; the bus bars comprise a first bus bar and a second bus bar; the high-voltage-resistant fiber conductive electrode at the upper part and the high-voltage-resistant fiber conductive electrode at the lower part are communicated with the first bus bar; the middle high-voltage resistant fiber conductive electrode is communicated with the second bus bar.
The junction of the bus bar and the high-voltage resistant fiber conductive electrode is in a chamfer structure.
The left edge and the right edge of the supporting layer are respectively the inner sides of the first bus bar and the second bus bar; the upper edge and the lower edge are respectively the outer sides of the upper high-voltage resistant fiber conductive electrode and the lower high-voltage resistant fiber conductive electrode.
The supporting layer is made of polyester resin PET or polyethylene naphthalate PEN.
The invention also includes a method for preparing the heating film, which comprises the following steps:
1) coating the graphene heating slurry on a supporting layer, and coating insulating glue at the edge; respectively manufacturing an upper supporting layer and an upper graphene conducting layer; and a lower support layer and a lower graphene conductive layer;
2) placing a high-voltage-resistant fiber conductive electrode on the graphene heating slurry obtained in the step 1) to form a high-voltage-resistant fiber conductive electrode layer;
3) and combining the upper supporting layer and the upper graphene conducting layer, the lower supporting layer and the lower graphene conducting layer with the high-voltage-resistant fiber conducting electrode layer in the middle layer, extruding and drying to obtain the high-voltage-resistant graphene heating film of the conducting fiber material electrode.
The preparation method of the graphene heating slurry in the step 1) comprises the following steps: 1) dissolving graphene powder into an alcohol water solution, and ultrasonically stirring to prepare a colloidal solution; 2) adding a binder to prepare slurry.
Specifically, the volume ratio of the graphene powder to the alcohol water solution in the step 1) is 1-4mg/mL, and the graphene powder and the alcohol water solution are mixed and stirred for 10-13 hours and subjected to ultrasonic treatment for 4-6 hours to obtain graphene colloid; the stirring speed is 30-50r/min, and the concentration of the alcohol water solution is 62%.
The binder is 7-9% of sodium carboxymethylcellulose (CMC), 23-50% of Waterborne Polyurethane (WPU) or 30-40% of silicone-acrylic emulsion (Si-Acr).
The preparation method of the high-voltage resistant fiber conductive electrode comprises the following steps:
1) cleaning high-pressure resistant fibers, washing the high-pressure resistant fibers for 30min at the temperature of 60-80 ℃ by adopting a mixed solution of 20g/L NaOH and 6-10g/L deionized detergent, and removing oil stains on the surfaces of the fibers;
2) activating high-pressure resistant fiber, namely pretreating the oil stain removal high-pressure resistant fiber obtained in the step 1) by using 190-210g/L NaOH solution at the temperature of 60 ℃ for 40min to activate the hydroxyl on the surface of the fiber;
3) preparing sulfydryl modified coarsened high-pressure resistant fiber, taking out the high-pressure resistant fiber with activated surface hydroxyl prepared in the step 2), immersing the fiber into a solution of ethyl acetate and 3-mercaptopropyl triethoxysilane, wherein the 3-mercaptopropyl triethoxysilane accounts for 10% -15%, and reacting for 90min at room temperature to prepare the sulfydryl modified coarsened high-pressure resistant fiber;
4) taking out the sulfydryl modified coarsened high-pressure resistant fiber, washing with absolute ethyl alcohol, and drying for later use;
5) plating metal on the surface of the cleaned sulfydryl modified coarsened high-pressure resistant fiber obtained in the step 4); the metal plated in the step 5) is Au, Ag or Pt.
When the metal is Ag, the following steps are adopted: preparing electroplating solution A and electroplating solution B, and mixing the two solutions in the same volume;
solution A, AgNO3Dissolving in water to obtain 5-7% solution, and adding ammonia water while stirring until Ag is separated out2Dissolving the O precipitate completely, adding NaOH, blackening the solution again, keeping the pH at 11-12, and continuously dropwise adding ammonia water until the solution is completely clear;
dissolving glucose and tartaric acid in appropriate water, boiling, cooling, and adding ethanol water solution; glucose is dissolved in tartaric acid, and the mass ratio of ethanol to water is 11:1:20: 250.
Mixing the two solutions, putting into high pressure resistant fabric, and performing chemical silvering.
Compared with the prior art, the invention has the beneficial effects that:
1) at present, the mainstream graphene heating film is loaded with a voltage below 12V and is used for heating clothes and physiotherapy products; the graphene electric heater unit or drying equipment is applied to the graphene electric heater unit or drying equipment with 220V or 380V alternating current, and has high voltage resistance, ageing resistance and high insulating property;
2) traditional diaphragm that generates heat adopts electrically conductive silver thick liquid as electrode material, and under the loading high pressure condition, the diaphragm calorific capacity increases, and the deformation appears in diaphragm supporting material, because silver thick liquid drying condenses the back, has the silver thick liquid gathering condition, leads to electric conductive property unstable, and mechanical tensile properties is poor simultaneously, causes electrode and busbar junction to appear the crack, and then the fracture, causes the diaphragm to become invalid. According to the invention, the high-voltage resistant material fiber material such as PET, PEN or PI is plated with conductive metal such as silver and gold to manufacture the electrode, so that the traditional conductive silver paste is replaced, the material has good deformation performance, and the electrode fracture phenomenon is effectively solved;
3) improving the structure of the membrane, a, placing an electrifying terminal outside a membrane heating area; b. the graphene conductive slurry is adopted in the region (in the dotted line) enclosed by the electrodes and the bus bars, and the outside of the region is sealed by the insulating glue. The creepage effect of the diaphragm under the high-voltage condition is effectively solved; in the film pasting process, the terminal is burnt due to the warping of the electrode terminal, and the phenomenon is caused by the fact that the temperature of the terminal is too high and the terminal is damaged at the earliest because the graphene is directly contacted with the terminal;
4) high-pressure resistant materials such as PEN, PI and the like are used as supporting layers, so that the aging rate of the membrane under the conditions of high pressure and high heat is reduced.
Drawings
Fig. 1 is a schematic structural diagram of a high-voltage resistant graphene heating film of a conductive fiber material electrode according to the present invention;
FIG. 2 is a schematic structural diagram of a high-voltage resistant graphene heating film of a conductive fiber material electrode according to the present invention and a cross-sectional view of the heating film;
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
All materials used in this application are commercially available, and typical examples include carboxymethylcellulose sodium CMC (Shandong Weifang Strength composite Co., Ltd.), or waterborne polyurethane WPU (Anhui Dahuatai New Material Co., Ltd.), and silicone-acrylic emulsion Si-Acr (Shandong Baoda New Material Co., Ltd.). 3-mercaptopropyltriethoxysilane (morning light chemical).
Fig. 1-2 show a high voltage resistant graphene heating film of a conductive fiber material electrode, which includes a high voltage resistant fiber conductive electrode layer 4, graphene conductive layers 2 disposed on two sides of the high voltage resistant fiber conductive electrode layer, and a support layer 1 disposed on the outer side of the graphene conductive layers; the edges of two sides of the graphene conducting layer are provided with insulating glue anti-leakage layers 3; the high-voltage-resistant fiber conductive electrode layer is connected with the bus bar.
The high-voltage resistant fiber conductive electrode layer comprises three high-voltage resistant fiber conductive electrodes which are sequentially arranged from top to bottom; the bus bars comprise a first bus bar 11 and a second bus bar 12; wherein, the high-voltage resistant fiber conductive electrode at the upper part and the high-voltage resistant fiber conductive electrode at the lower part are communicated with the first bus bar 11; the middle high voltage resistant fiber conductive electrode is in communication with the second bus bar 12.
The junction of the bus bar and the high-voltage resistant fiber conductive electrode is in a chamfer structure.
The left edge and the right edge of the supporting layer are respectively the inner sides of the first bus bar and the second bus bar; the upper and lower edges are the outer sides of the upper and lower high voltage resistant fibre conductive electrodes, respectively (the positions of the squares given by the dotted lines in fig. 1-2).
The supporting layer is made of polyester resin PET or polyethylene naphthalate PEN.
The invention also includes a method for preparing the heating film, which comprises the following steps:
1) coating the graphene heating slurry on a supporting layer, and coating insulating glue at the edge; respectively manufacturing an upper supporting layer and an upper graphene conducting layer; and a lower support layer and a lower graphene conductive layer;
2) placing a high-voltage-resistant fiber conductive electrode on the graphene heating slurry obtained in the step 1) to form a high-voltage-resistant fiber conductive electrode layer;
3) and combining the upper supporting layer and the upper graphene conducting layer, the lower supporting layer and the lower graphene conducting layer with the high-voltage-resistant fiber conducting electrode layer in the middle layer, extruding and drying to obtain the high-voltage-resistant graphene heating film of the conducting fiber material electrode.
The preparation method of the graphene heating slurry in the step 1) comprises the following steps: 1) dissolving graphene powder into an alcohol water solution, and ultrasonically stirring to prepare a colloidal solution; preparing a mixed solution with the concentration of 1-4mg/mL by using graphene powder and an alcohol aqueous solution, mixing and stirring for 10-13 hours, and performing ultrasonic treatment for 4-6 hours to obtain a graphene colloid; the stirring speed is 30-50r/min, and the concentration of the alcohol water solution is 62%. 2) Adding a binder to prepare slurry. The adhesive is 7-9% of sodium carboxymethyl cellulose (CMC), 23-50% of Waterborne Polyurethane (WPU) or 30-40% of silicone-acrylic emulsion (Si-Acr).
The preparation method of the high-voltage resistant fiber conductive electrode comprises the following steps: 1) cleaning high-pressure resistant fibers, and washing the high-pressure resistant fibers for 30min at the temperature of 60-80 ℃ by adopting 20g/LNaOH and 6-10g/L deionized detergent mixed liquor to remove oil stains on the surfaces of the fibers; 2) activating high-pressure resistant fiber, namely pretreating the oil stain removal high-pressure resistant fiber obtained in the step 1) by using 190-210g/L NaOH solution at the temperature of 60 ℃ for 40min to activate the hydroxyl on the surface of the fiber;
3) preparing sulfydryl modified coarsened high-pressure resistant fiber, taking out the high-pressure resistant fiber with activated surface hydroxyl prepared in the step 2), immersing the fiber into a solution of ethyl acetate and 3-mercaptopropyl triethoxysilane, wherein the 3-mercaptopropyl triethoxysilane accounts for 10% -15%, and reacting for 90min at room temperature to prepare the sulfydryl modified coarsened high-pressure resistant fiber;
4) taking out the sulfydryl modified coarsened high-pressure resistant fiber, washing with absolute ethyl alcohol, and drying for later use;
5) plating metal on the surface of the cleaned sulfydryl modified coarsened high-pressure resistant fiber obtained in the step 4); the metal plated in the step 5) is Au, Ag or Pt.
When the metal is Ag, the following steps are adopted: preparing electroplating solution A and electroplating solution B, and mixing the two solutions in the same volume;
solution A, AgNO3Dissolving in water to obtain 5-7% solution, and adding ammonia water while stirring until Ag is separated out2Dissolving the O precipitate completely, adding NaOH, blackening the solution again, keeping the pH at 11-12, and continuously dropwise adding ammonia water until the solution is completely clear;
dissolving glucose and tartaric acid in appropriate water, boiling, cooling, and adding ethanol water solution; glucose is dissolved in tartaric acid, and the mass ratio of ethanol to water is 11:1:20: 250.
Mixing the two solutions, putting into high pressure resistant fabric, and performing chemical silvering.
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
Claims (9)
1. The high-voltage-resistant graphene heating film for the conductive fiber material electrode is characterized by comprising a high-voltage-resistant fiber conductive electrode layer, graphene conductive layers arranged on two sides of the high-voltage-resistant fiber conductive electrode layer and a supporting layer arranged on the outer side of the graphene conductive layer; insulating glue leakage-proof layers are arranged at the edges of two sides of the graphene conducting layer; the high-voltage-resistant fiber conductive electrode layer is connected with the bus bar.
2. The electrode high-voltage-resistant graphene heating film made of the conductive fiber material according to claim 1, wherein the high-voltage-resistant fiber conductive electrode layer comprises three high-voltage-resistant fiber conductive electrodes sequentially arranged from top to bottom; the bus bars comprise a first bus bar and a second bus bar; the high-voltage-resistant fiber conductive electrode at the upper part and the high-voltage-resistant fiber conductive electrode at the lower part are communicated with the first bus bar; the high-voltage resistant fiber conductive electrode in the middle is communicated with the second bus bar; the junction of the bus bar and the high-voltage resistant fiber conductive electrode is in a chamfer structure.
3. The electrode high voltage resistant graphene exothermic film according to claim 2, wherein the left and right edges of the supporting layer are respectively the inner sides of the first bus bar and the second bus bar; the upper edge and the lower edge are respectively the outer sides of the upper high-voltage resistant fiber conductive electrode and the lower high-voltage resistant fiber conductive electrode.
4. A method of producing a heat-generating film according to any one of claims 1 to 3, characterized by comprising the steps of:
1) coating the graphene heating slurry on a supporting layer, and coating insulating glue at the edge; respectively manufacturing an upper supporting layer and an upper graphene conducting layer; and a lower support layer and a lower graphene conductive layer;
2) placing a high-voltage-resistant fiber conductive electrode on the graphene heating slurry obtained in the step 1) to form a high-voltage-resistant fiber conductive electrode layer;
3) and combining the upper supporting layer and the upper graphene conducting layer, the lower supporting layer and the lower graphene conducting layer with the high-voltage-resistant fiber conducting electrode layer in the middle layer, extruding and drying to obtain the high-voltage-resistant graphene heating film of the conducting fiber material electrode.
5. The method for preparing a heat-generating film according to claim 4, wherein the method for preparing the graphene heat-generating paste in step 1) comprises:
1) dissolving graphene powder into an alcohol water solution, and ultrasonically stirring to prepare a colloidal solution;
2) adding a binder to prepare slurry.
6. The method for preparing a heating film according to claim 5, wherein the concentration of the graphene powder and the alcohol aqueous solution prepared in step 1) is 1-4mg/mL, and the graphene powder and the alcohol aqueous solution are mixed and stirred for 10-13 hours and subjected to ultrasonic treatment for 4-6 hours to obtain graphene colloid; the stirring speed is 30-50r/min, and the concentration of the alcohol water solution is 62%.
7. A method for producing a heat-generating film according to claim 6, wherein the method for producing the high-voltage resistant fiber conductive electrode comprises the steps of:
1) cleaning high-pressure resistant fibers, washing the high-pressure resistant fibers for 30min at the temperature of 60-80 ℃ by adopting a mixed solution of 20g/L NaOH and 6-10g/L deionized detergent, and removing oil stains on the surfaces of the fibers;
2) activating high-pressure resistant fiber, namely pretreating the oil stain removal high-pressure resistant fiber obtained in the step 1) by using 190-210g/L NaOH solution at the temperature of 60 ℃ for 40min to activate the hydroxyl on the surface of the fiber;
3) preparing sulfydryl modified coarsened high-pressure resistant fiber, taking out the high-pressure resistant fiber with activated surface hydroxyl prepared in the step 2), immersing the fiber into a solution of ethyl acetate and 3-mercaptopropyl triethoxysilane, wherein the 3-mercaptopropyl triethoxysilane accounts for 10% -15%, and reacting for 90min at room temperature to prepare the sulfydryl modified coarsened high-pressure resistant fiber;
4) taking out the sulfydryl modified coarsened high-pressure resistant fiber, washing with absolute ethyl alcohol, and drying for later use;
5) plating metal on the surface of the cleaned sulfhydryl modified coarsened high-pressure resistant fiber obtained in the step 4).
8. A method of producing a heat-generating film according to claim 7, wherein the metal plated in step 5) is Au, Ag or Pt.
9. A method of producing a heat-generating film according to claim 8, wherein when the metal is Ag, the following steps are employed: preparing electroplating solution A and electroplating solution B, and mixing the two solutions in the same volume;
solution A, AgNO3Dissolved in water to prepare 5 to 7 percentAnd ammonia water is dripped under continuous stirring until Ag is separated out2Dissolving the O precipitate completely, adding NaOH, blackening the solution again, keeping the pH at 11-12, and continuously dropwise adding ammonia water until the solution is completely clear;
dissolving glucose and tartaric acid in appropriate water, boiling, cooling, and adding ethanol water solution; glucose is dissolved in tartaric acid, and the mass ratio of ethanol to water is 11:1:20: 250.
Mixing the two solutions, putting into high pressure resistant fabric, and performing chemical silvering.
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CN113560144A (en) * | 2021-08-04 | 2021-10-29 | 德州宇航派蒙石墨烯科技有限责任公司 | Graphene three-dimensional curved surface heating body and preparation method thereof |
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CN107197549A (en) * | 2017-05-31 | 2017-09-22 | 北京绿能嘉业新能源有限公司 | Graphene nano far-infrared negative-ion composite fibre electric heating panel and manufacture craft |
CN211063803U (en) * | 2019-11-21 | 2020-07-21 | 天津北方石墨烯产业研究院 | High-voltage-resistant graphene heating film of conductive fiber material electrode |
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CN107197549A (en) * | 2017-05-31 | 2017-09-22 | 北京绿能嘉业新能源有限公司 | Graphene nano far-infrared negative-ion composite fibre electric heating panel and manufacture craft |
CN211063803U (en) * | 2019-11-21 | 2020-07-21 | 天津北方石墨烯产业研究院 | High-voltage-resistant graphene heating film of conductive fiber material electrode |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113560144A (en) * | 2021-08-04 | 2021-10-29 | 德州宇航派蒙石墨烯科技有限责任公司 | Graphene three-dimensional curved surface heating body and preparation method thereof |
CN113560144B (en) * | 2021-08-04 | 2023-08-18 | 德州宇航派蒙石墨烯科技有限责任公司 | Graphene three-dimensional curved surface heating body and preparation method thereof |
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