CN110958725A - Preparation method of flexible low-voltage composite polymer heating film - Google Patents
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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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
- H05B3/02—Details
- H05B3/03—Electrodes
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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
- H05B3/145—Carbon only, e.g. carbon black, graphite
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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
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Abstract
The invention provides a preparation method of a flexible low-voltage composite polymer heating film, which comprises the following steps: plasticating the thermoplastic elastomer on an open mill to a transparent state; putting the plasticated thermoplastic elastomer, half of the uniformly mixed solid powder, the high-fluidity agent and the anti-aging agent into an internal mixer for uniform mixing, and continuously adding the other half of the uniformly mixed solid powder and the base oil for internal mixing; crushing the mixed materials by an internal mixer, and putting the crushed materials into an extruder for extrusion; putting the extruded material into a four-roll calender to extrude a composite film with the thickness of 0.1-0.3 mm; printing a conductive coating on the graphene composite film by using screen printing equipment, and heating and drying; placing the graphene composite film printed with the conductive coating in an oven for baking; and attaching the resin soft film to the graphene composite film and between the graphene composite film and the resin soft film. The invention has the advantages of low pressure, rapid heating, uniform heat, low manufacturing cost, safe use, convenience, reliable quality and the like.
Description
Technical Field
The invention belongs to the technical field of heating films, and particularly relates to a preparation method of a low-voltage heating flexible film printed by silver paste.
Background
At present, most of common heating materials in the market are traditional heating wires, silicon carbide and advanced PTC ceramic heating elements, recently, carbon fiber heating materials appear in the market, most of the heating materials are hard and brittle in texture and uneven in heating density, and the phenomena of dry skin, thirst and the like of a human body can be caused after long-time use of the heating materials, so that the pursuit of people for high-quality life in the current social and economic level is not met. Meanwhile, most common heating materials in the market can meet the heating requirement only by using higher power supply voltage, and the safety and portability using requirements of the heating film are not facilitated.
Disclosure of Invention
The invention aims to provide a preparation method of a flexible low-voltage composite polymer heating film with the voltage within 5V.
According to one aspect of the invention, a preparation method of a flexible low-voltage composite polymer heating film is provided, which comprises the following steps:
adjusting the temperature of the open mill to 160 ℃, and plasticating the thermoplastic elastomer on the open mill to be in a transparent state;
adjusting the temperature of an internal mixer to 160-180 ℃, putting the plasticated thermoplastic elastomer, one half of the uniformly mixed solid powder, the high-fluidity agent and the anti-aging agent into the internal mixer to be uniformly mixed, and continuously adding the other half of the uniformly mixed solid powder and the base oil to be internally mixed, wherein the solid powder comprises conductive carbon black, graphene and natural graphite;
crushing the mixed materials by an internal mixer, and putting the crushed materials into an extruder for extrusion;
putting the extruded material into a four-roll calender to extrude a composite film with the thickness of 0.1-0.3 mm;
printing a conductive coating on the graphene composite film by using screen printing equipment, and heating and drying, wherein the thickness of the conductive coating is 8-20 microns;
placing the graphene composite film printed with the conductive coating in an oven for baking, wherein the baking temperature is 120 ℃, and the baking time is 20 min;
and attaching the resin soft film to the graphene composite film, and positioning the resin soft film on the graphene composite film and the conductive coating.
In some embodiments, the conductive coating serves as an electrode, the electrode includes two parallel bus bars and a plurality of internal electrodes, adjacent internal electrodes are respectively connected to different bus bars, the bus bars are connected to the positive electrode or the negative electrode of the power supply, so that the polarities of the adjacent internal electrodes are opposite, when the power supply is powered on, current flows into the corresponding negative internal electrode through the positive bus bar, and finally all the internal electrodes are converged into the negative bus bar, the distances between the internal electrodes are equal, and the distances between the internal electrodes and the bus bars which are not in contact with the internal electrodes are equal.
In some embodiments, two first holes are formed in the resin soft film, a second hole is formed in the bus bar, the diameter of the second hole is smaller than the width of the bus bar, after the resin soft film is covered on the conductive coating and attached to the composite film, the first holes correspond to the second holes, and the diameter of the first holes is larger than that of the second holes.
In some embodiments, the preparation raw materials comprise, in weight percent: 65% of thermoplastic elastomer, 10-15% of conductive carbon black, 6-10% of graphene, 5-8% of natural graphite, 3% of anti-aging agent, 3% of base oil and 3% of high-fluidity agent.
In some embodiments, the thermoplastic elastomer is polypropylene, polystyrene plastic modified styrene or polyurethane block copolymer selected from, but not limited to, TPE or TPU or TPV, with a shore a hardness between 45 and 50.
In some embodiments, the conductive carbon black has a nano-scale particle size, the graphene has a platelet size of less than 5 microns, and the graphene is prepared by a mechanical exfoliation method or a chemical method.
In some embodiments, the antioxidant is one or more compounds of environment-friendly phenolic antioxidants, and is selected from but not limited to one or more of N-cyclohexyl-N' -phenyl-p-phenylenediamine, N- (1, 3-dimethylbutyl-N-phenyl-phenylenediamine, tris (2, 4-di-tert-butyl) phenyl phosphite, β - (3, 5-di-tert-butyl-4-hydroxyphenyl) N-octadecyl propionate, and β - (3, 5-di-tert-butyl-4-hydroxyphenyl) isooctyl propionate.
In some embodiments, the base oil is selected from, but not limited to, industrial white oils, environmentally friendly aromatic oils, naphthenic oils.
In some embodiments, the conductive coating includes, but is not limited to, silver paste, copper paste, and the solid content of the conductive coating is not less than 50%.
In some embodiments, the flexible resin film is flexible and can be attached to the composite film by lamination after heating, and the flexible resin film is selected from polyurethane and polyethylene.
The beneficial effects are as follows: the invention comprises a composite film prepared from a thermoplastic elastomer, graphene, conductive carbon black and natural graphite, a conductive silver coating layer and a resin soft film, wherein the composite film comprises the following components in parts by weight: the composite film has high temperature resistance of 160 deg.c and the conducting silver paint layer is ladder-shaped non-closed loop.
The graphene in the composite film has good conductive and heat dissipation functions and has a physical therapy effect on a body; the conductive coating has reasonable size and pattern, uniform heating, soft material, better contact with human body, better body feeling effect, comfortable use, convenient carrying when going out of a door and no influence on the beauty of wearing and use; the heating film prepared by the invention has the use condition that the voltage is lower than 5V, can be used only by common charging treasures in the market, is safe and convenient, and can meet the use requirements of different places, different seasons and different crowds.
The invention is suitable for the technical occasions of heating physiotherapy, precise electronic instruments, new energy field and the like, the conductive heating film layer and lines of the heating film are uniformly distributed, the heat density is large after the heating film is electrified, the integral heating is uniform, and the base material is flexible and foldable. The thickness of the film can be used between 0.1 and 0.2mm, the thermoplastic elastomer composite film has no obvious performance change after being aged in hot air for 200 hours at 100 ℃, the printed conductive film does not fall off after being soaked in water for 24 hours, the flexible resin film is covered on the film, the film can be completely waterproof, and the conductive coating is continuously twisted for 2 ten thousand times after a plurality of light kneading experiments, so that the film has the advantages of low-pressure rapid heating, uniform heat, low manufacturing cost, safe use, convenience, reliable texture and the like.
Drawings
Fig. 1 is a schematic structural diagram of a conductive coating in a method for manufacturing a flexible low-voltage composite polymer heating film according to an embodiment of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
Example one
A preparation method of a flexible low-voltage composite high-molecular heating film comprises the steps of adjusting the temperature of an open mill to 160 ℃, adjusting the roll distance of the open mill to 0.5mm, plasticating a thermoplastic elastomer to a transparent state on the open mill, adjusting the temperature of an internal mixer to 160 ℃, uniformly mixing the plasticated thermoplastic elastomer, half of uniformly mixed solid powder, a high-fluidity agent and an anti-aging agent through the internal mixer, adding the other half of the uniformly mixed solid powder and base oil after 5min, and internally mixing for 10min, crushing the well-mixed materials through the internal mixer, adding the mixture into an extruder to extrude the solid powder comprising conductive carbon black, graphene and natural graphite, wherein the reaction components comprise 65% of the thermoplastic elastomer, 10% of the conductive carbon black, 10% of the graphene, 6% of the natural graphene, 3% of the conductive agent, 3% of the base oil and 3% of the high-fluidity agent according to weight percentage, wherein the high-fluidity agent is a flowing modifier, the thermoplastic elastomer is V, the graphene is 6%, the natural graphene, 3% of the base oil and 3% of the high-fluidity agent are respectively placed on a conductive resin, the conductive film is prepared by a conductive film, the first conductive film, the conductive film is placed on a conductive bar, the conductive film is placed on a conductive film, the second conductive bar, the conductive bar is placed on the first conductive bar, the bar.
In this example, the area of the heat-generating film was 50 to 150cm2The voltage is 3.5-5V, and the temperature of the heating film is 50-55 ℃; in practical application, the connection can be carried out in series or in parallel; the thickness of the composite film can be used between 0.1mm and 0.3mm, the thermoplastic elastomer composite film has no obvious performance change after being aged in hot air for 200 hours at 100 ℃, the printed conductive film does not fall off after being soaked in water for 24 hours, the flexible resin film is covered on the composite film, the composite film can be completely waterproof, and the composite film is subjected to a plurality of light kneading experiments, and is continuously kneaded and folded for 2 ten thousand times, so that the composite film has the advantages of low-pressure rapid heating, uniform heat, low manufacturing cost, safe use, convenience, reliable texture and the like.
Example two
A preparation method of a flexible low-voltage composite polymer heating film comprises the following steps: the temperature of the open mill is adjusted to 160 ℃, the roller spacing of the open mill is adjusted to 0.5mm, and the thermoplastic elastomer is plasticated on the open mill to a transparent state. And (3) adjusting the temperature of the internal mixer to 180 ℃, uniformly mixing the plasticated thermoplastic elastomer, half of the uniformly mixed solid powder, the high-fluidity agent and the anti-aging agent by the internal mixer, and after 5min, adding the other half of the uniformly mixed solid powder and the base oil for internal mixing for 10 min. And crushing the mixed materials by an internal mixer, and putting the crushed materials into an extruder for extrusion. The solid powder includes conductive carbon black, graphene and natural graphite. The reaction components comprise the following components in percentage by weight: 65% of thermoplastic elastomer, 15% of conductive carbon black, 6% of graphene, 8% of natural graphite, 3% of anti-aging agent, 3% of base oil and 3% of high-fluidity agent. In this embodiment, the high flow agent is a flow modifier. The thermoplastic elastomer is TPE, and the hardness Shore A is 45-50. The particle size of the conductive carbon black is nano-scale, the sheet diameter of the graphene is less than 5 microns, and the graphene is prepared by a mechanical stripping method or a chemical method. The anti-aging agent is compounded by N-cyclohexyl-N' -phenyl-p-phenylenediamine and N- (1, 3-dimethylbutyl-N-phenyl-phenylenediamine, the base oil is environment-friendly aromatic oil, the particle size of the conductive carbon black is nano-grade, the sheet diameter of the graphene is less than 5 micrometers, the extruded material is put into a four-roll calender to be extruded into a graphene composite film with the thickness of 0.3mm, a screen printing device is used for printing a conductive coating on the graphene composite film with the thickness of 0.3mm and heating and drying the conductive coating, the thickness of the conductive coating is 15 micrometers, the conductive coating comprises but is not limited to copper paste, the solid content of the conductive coating is not less than 50 percent, in the embodiment, a silver paste electrode pattern shown in figure 1 is printed on the graphene composite film, the thickness of the silver paste is 15 micrometers, the conductive coating is used as an electrode of a heating film and consists of a bus bar, the bus bar 11 is straight and the inner electrode 12 is wavy. The bus bar 11 is connected to the positive or negative electrode of the power supply so that the polarities of the adjacent internal electrodes 12 are opposite. When the current is applied, the current flows into the corresponding negative internal electrode 12 through the positive bus bar 11, and finally all the current is collected into the negative bus bar 11. Two bus bars 11 are arranged in parallel, two adjacent internal electrodes 12 are respectively connected to different bus bars 11, the distance between each bus bar 11 and the bus bar 11 which is not in contact with the bus bar is the same, and the distance between the internal electrodes 12 is the same. And (3) placing the graphene composite film printed with the electrode pattern in an oven for baking, wherein the baking temperature is 120 ℃, and the baking time is 20 min. Two first holes are opened in the resin soft film using a laser device. The bus bar 11 is provided with a second hole 111, and the diameter of the second hole 111 is smaller than the width of the frame of the bus bar 11. When the resin soft film is attached to the graphene composite film, the two first holes correspond to the second holes 111 of the bus bar 11 on the conductive coating respectively, and the diameter of each first hole is larger than that of the corresponding second hole 111. And attaching the resin soft film with the holes to the graphene composite film, so that the silver-copper paste electrode pattern is positioned between the graphene composite film and the resin soft film. The resin soft film is flexible and can be jointed and connected with the composite film after being heated, and the resin soft film is polyethylene.
The area of the prepared heating film is 50-150cm2The voltage is 3.5-5V, and the temperature of the heating film is 50-55 ℃; in practical application, the series connection or the parallel connection can be carried outConnecting; the thickness of the composite film can be used between 0.1mm and 0.3mm, the thermoplastic elastomer composite film has no obvious performance change after being aged in hot air for 200 hours at 100 ℃, the printed conductive film does not fall off after being soaked in water for 24 hours, the flexible resin film is covered on the composite film, the composite film can be completely waterproof, and the composite film is subjected to a plurality of light kneading experiments, and is continuously kneaded and folded for 2 ten thousand times, so that the composite film has the advantages of low-pressure rapid heating, uniform heat, low manufacturing cost, safe use, convenience, reliable texture and the like.
EXAMPLE III
A preparation method of a flexible low-voltage composite high-molecular heating film comprises the steps of adjusting the temperature of an open mill to 160 ℃, adjusting the roller distance of the open mill to 0.5mm, plasticating a thermoplastic elastomer to be in a transparent state on the open mill, adjusting the temperature of an internal mixer to 170 ℃, uniformly mixing the plasticated thermoplastic elastomer, half of uniformly mixed solid powder, a high flow agent and an anti-aging agent through the internal mixer, after 5min, adding the other half of the uniformly mixed solid powder and base oil to be internally mixed for 10min, crushing the mixed materials through the internal mixer, putting the crushed materials into an extruder, extruding the solid powder comprising conductive carbon black, graphene and natural graphite, wherein the reaction components comprise, by weight, 65% of the thermoplastic elastomer, 12% of conductive carbon black, 8% of the graphene, 5% of the natural graphite, 3% of the anti-aging agent, 3% of the base oil and 3% of the high flow agent, wherein the high flow agent is a flow modifier, the thermoplastic elastomer is TPV, the hardness A is 45-50%, the conductive carbon black is 3% of the conductive carbon black, the conductive carbon black is not less than 2, the conductive carbon black is not less than the conductive carbon black, the conductive carbon black is placed on the conductive carbon black of a conductive carbon black conductive film, the second conductive carbon black conductive film, the conductive carbon black carbon.
The area of the prepared heating film is 50-150cm2The voltage is 3.5-5V, and the temperature of the heating film is 50-55 ℃; in practical application, the connection can be carried out in series or in parallel; the thickness of the composite film can be used between 0.1mm and 0.3mm, the thermoplastic elastomer composite film has no obvious performance change after being aged in hot air for 200 hours at 100 ℃, the printed conductive film does not fall off after being soaked in water for 24 hours, the flexible resin film is covered on the composite film, the composite film can be completely waterproof, and the composite film is subjected to a plurality of light kneading experiments, and is continuously kneaded and folded for 2 ten thousand times, so that the composite film has the advantages of low-pressure rapid heating, uniform heat, low manufacturing cost, safe use, convenience, reliable texture and the like.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a flexible low-voltage composite polymer heating film is characterized by comprising the following steps:
adjusting the temperature of the open mill to 160 ℃, and plasticating the thermoplastic elastomer on the open mill to be in a transparent state;
adjusting the temperature of an internal mixer to 160-180 ℃, putting the plasticated thermoplastic elastomer, one half of the uniformly mixed solid powder, the high-fluidity agent and the anti-aging agent into the internal mixer to be uniformly mixed, and continuously adding the other half of the uniformly mixed solid powder and the base oil to be internally mixed, wherein the solid powder comprises conductive carbon black, graphene and natural graphite;
crushing the mixed materials by an internal mixer, and putting the crushed materials into an extruder for extrusion;
putting the extruded material into a four-roll calender to extrude a composite film with the thickness of 0.1-0.3 mm;
printing a conductive coating on the graphene composite film by using screen printing equipment, and heating and drying, wherein the thickness of the conductive coating is 8-20 microns;
placing the graphene composite film printed with the conductive coating in an oven for baking, wherein the baking temperature is 120 ℃, and the baking time is 20 min;
and attaching the resin soft film to the graphene composite film, and positioning the resin soft film on the graphene composite film and the conductive coating.
2. The method according to claim 1, wherein the conductive coating is used as an electrode, the electrode comprises two parallel bus bars and a plurality of inner electrodes, the adjacent inner electrodes are respectively connected to different bus bars, the bus bars are connected to the positive electrode or the negative electrode of the power supply, so that the polarities of the adjacent inner electrodes are opposite, when the power is supplied, the current flows into the corresponding negative inner electrode through the positive bus bar and finally flows into the negative bus bar, the distances between the inner electrodes are equal, and the distances between the inner electrodes and the bus bars which are not in contact with the inner electrodes are equal.
3. The method according to claim 1, wherein two first holes are formed in the resin soft film, a second hole is formed in the bus bar, the diameter of the second hole is smaller than the width of the bus bar, the first hole corresponds to the second hole after the resin soft film is covered on the conductive coating and attached to the composite film, and the diameter of the first hole is larger than the diameter of the second hole.
4. The preparation method of the flexible low-voltage composite polymer heating film according to claim 1, wherein the preparation raw materials comprise, by weight: 65% of thermoplastic elastomer, 10-15% of conductive carbon black, 6-10% of graphene, 5-8% of natural graphite, 3% of anti-aging agent, 3% of base oil and 3% of high-fluidity agent.
5. The method for preparing a flexible low-voltage composite polymer heating film according to claim 4, wherein the thermoplastic elastomer is a block copolymer of styrene or polyurethane modified from polypropylene or polystyrene plastic, selected from but not limited to TPE or TPU or TPV, and has a Shore A hardness of 45-50.
6. The method for preparing the flexible low-voltage composite polymer heating film according to claim 4, wherein the particle size of the conductive carbon black is nano-scale, the sheet diameter of the graphene is less than 5 microns, and the graphene is prepared by a mechanical stripping method or a chemical method.
7. The method for preparing the flexible low-voltage composite polymer heating film according to claim 4, wherein the anti-aging agent is one or more of environment-friendly phenol anti-aging agents, and is selected from but not limited to one or more of N-cyclohexyl-N' -phenyl-p-phenylenediamine, N- (1, 3-dimethylbutyl-N-phenyl-phenylenediamine), tris (2, 4-di-tert-butyl) phenyl phosphite, β - (3, 5-di-tert-butyl-4-hydroxyphenyl) N-octadecyl propionate, and β - (3, 5-di-tert-butyl-4-hydroxyphenyl) isooctyl propionate.
8. The method for preparing the flexible low-voltage composite polymer heating film according to claim 4, wherein the base oil is selected from but not limited to industrial white oil, environment-friendly aromatic oil and naphthenic oil.
9. The preparation method of the flexible low-voltage composite polymer heating film according to claim 1, wherein the conductive coating comprises but is not limited to silver paste and copper paste, and the solid content of the conductive coating is not less than 50%.
10. The method for preparing a flexible low-voltage composite polymer heating film according to claim 1, wherein the flexible resin film is flexible and can be attached to the composite film after being heated, and the flexible resin film is selected from polyurethane and polyethylene.
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