CN114205937A - Manufacturing process of graphene electric heating PI (polyimide) membrane - Google Patents
Manufacturing process of graphene electric heating PI (polyimide) membrane Download PDFInfo
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- CN114205937A CN114205937A CN202210051140.6A CN202210051140A CN114205937A CN 114205937 A CN114205937 A CN 114205937A CN 202210051140 A CN202210051140 A CN 202210051140A CN 114205937 A CN114205937 A CN 114205937A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 66
- 238000005485 electric heating Methods 0.000 title claims abstract description 54
- 239000012528 membrane Substances 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 229920001721 polyimide Polymers 0.000 title description 3
- 239000004642 Polyimide Substances 0.000 title description 2
- 229920002050 silicone resin Polymers 0.000 claims abstract description 31
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000006258 conductive agent Substances 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 239000000080 wetting agent Substances 0.000 claims abstract description 13
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920005989 resin Polymers 0.000 claims abstract description 4
- 239000011347 resin Substances 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- -1 polydimethylsiloxane Polymers 0.000 claims description 25
- 229920002678 cellulose Polymers 0.000 claims description 6
- 239000001913 cellulose Substances 0.000 claims description 6
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims description 6
- 238000007650 screen-printing Methods 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000006230 acetylene black Substances 0.000 claims description 3
- 150000003973 alkyl amines Chemical class 0.000 claims description 3
- UDHMTPILEWBIQI-UHFFFAOYSA-N butyl naphthalene-1-sulfonate;sodium Chemical compound [Na].C1=CC=C2C(S(=O)(=O)OCCCC)=CC=CC2=C1 UDHMTPILEWBIQI-UHFFFAOYSA-N 0.000 claims description 3
- 239000002134 carbon nanofiber Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 150000004665 fatty acids Chemical class 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 3
- 239000003273 ketjen black Substances 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 239000010408 film Substances 0.000 description 21
- 229910002804 graphite Inorganic materials 0.000 description 14
- 239000010439 graphite Substances 0.000 description 14
- 229920000642 polymer Polymers 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 238000000554 physical therapy Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 description 2
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- H05B3/145—Carbon only, e.g. carbon black, graphite
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The embodiment of the invention discloses a manufacturing process of a graphene electric heating PI membrane, which is used for solving the technical problems of poor conductivity and unstable conductivity of the existing graphene electric heating product. The embodiment of the invention comprises the following steps: s1, mixing a conductive agent, a dispersing agent, a leveling agent, a wetting agent, a defoaming agent and conductive carbon black, and performing high-speed dispersion and grinding treatment to obtain conductive slurry; s2, adding a catalyst into the silicone resin, heating for reaction for a preset time, and then cooling to room temperature of 25 ℃; s3, stirring and mixing the graphene, the silicon resin and the conductive paste according to a preset mixing proportion, and dispersing at a high speed to obtain electrothermal paste; s4, preparing a PI membrane, coating the electric heating slurry on the surface of the PI membrane, and then heating and drying the electric heating slurry to form a graphene electric heating film on the surface of the PI membrane, so that the graphene electric heating PI membrane is obtained.
Description
Technical Field
The invention relates to the technical field of graphene electric heating, in particular to a manufacturing process of a graphene electric heating PI membrane.
Background
Graphene is a honeycomb-shaped planar thin film formed by carbon atoms in an sp2 hybridization mode, has a unique two-dimensional nano structure, has the advantages of high electron transmission rate, good electrical conductivity, high thermal conductivity and the like, is the thinnest, most rigid and best conductive and heat-conducting nano material at present, and has good application prospects in the fields of physics, materials science, electronic information, computers, aerospace and the like.
In recent years, researchers have gradually moved their development direction toward graphene exothermic materials. The graphene heating material is high in electricity-heat conversion rate, energy-saving and safe, and heat generated by the graphene electric heating film is emitted in a far infrared mode to play a role in physical therapy and health care for a human body. A plurality of existing physiotherapy health-care products are provided with a graphene electric heating film, such as knee pads and physiotherapy mattresses, but due to the defects of poor conductivity, unstable conductivity and the like of the existing products with the graphene electric heating film on the market, when a user uses the product, the temperature often drops or the temperature fluctuates, and the normal use of the product by the user is seriously affected.
Therefore, finding a manufacturing process of a graphene electrothermal PI film capable of solving the above technical problems is an important issue to be studied by those skilled in the art.
Disclosure of Invention
The embodiment of the invention discloses a manufacturing process of a graphene electric heating PI membrane, which is used for solving the technical problems of poor conductivity and unstable conductivity of the existing graphene electric heating product.
The embodiment of the invention provides a manufacturing process of a graphene electric heating PI membrane, which comprises the following steps:
s1, mixing a conductive agent, a dispersing agent, a leveling agent, a wetting agent, a defoaming agent and conductive carbon black, and performing high-speed dispersion and grinding treatment to obtain conductive slurry;
s2, adding a catalyst into the silicone resin, heating for reaction for a preset time, and then cooling to room temperature of 25 ℃;
s3, stirring and mixing the graphene, the silicon resin and the conductive paste according to a preset mixing proportion, and dispersing at a high speed to obtain electrothermal paste;
s4, preparing a PI membrane, coating the electrothermal slurry on the surface of the PI membrane, and drying the electrothermal slurry to form a membrane to obtain the graphene electrothermal PI membrane.
Optionally, the conductive slurry comprises, by mass, 5-55% of conductive carbon black, 5-20% of a conductive agent, 1-15% of a dispersing agent, 0.11-5% of a leveling agent, 0.11-5% of a wetting agent, and 0.11-5% of an antifoaming agent.
Optionally, the step S4 specifically includes:
preparing a PI membrane, coating the electric heating slurry on the surface of the PI membrane in a screen printing or blade coating or spraying manner, and drying the electric heating slurry through a baking oven, so that a graphene electric heating film is formed on the surface of the PI membrane, and the graphene electric heating PI membrane is obtained, wherein the baking temperature is 200-250 ℃, and the baking time is 30-40 min.
Optionally, the step S3 specifically includes:
according to the graphene: silicone resin: and (3) stirring and mixing the graphene, the silicone resin and the conductive paste according to the proportion of 2:7:1, and dispersing at a high speed to obtain the electrothermal paste.
Optionally, the step S2 specifically includes:
adding a catalyst into the silicone resin, carrying out heating reaction at the temperature of 100-150 ℃ for 30-60 min, and then cooling to room temperature of 25 ℃.
Optionally, the catalyst is hydrogen chloride.
Optionally, the dispersant comprises one or more of carboxylic acid based cellulose, polyethylene glycol, acetate based cellulose.
Optionally, the leveling agent comprises one or more of diethylene glycol ethyl ether acetate, isophorone, polydimethylsiloxane, and polymethylphenylsiloxane.
Optionally, the conductive agent comprises one or more of conductive graphite powder, acetylene black, carbon nanotubes, carbon nanofibers, ketjen black.
Optionally, the wetting agent comprises one or more of polyoxyethylene alkylamine, sodium butylnaphthalene sulfonate and sodium alkyl sulfate;
the defoaming agent comprises one or more of a fatty acid defoaming agent, a polyurethane defoaming agent and an organic fluorine defoaming agent.
According to the technical scheme, the embodiment of the invention has the following advantages:
in the embodiment, the silicone resin is a siloxane polymer with a branched structure, and is heated to react under the action of a catalyst to further generate a high polymer in a shape, and the silicon-oxygen bond in the silicone resin has high bonding performance and specificity on a molecular structure, so that the silicone resin has high heat resistance and excellent electrical performance. Through mixing silicone resin with conductive paste and graphite alkene, make graphite alkene can alternate in the three-dimensional structure that forms when the silicone resin cross-linking polymerization, when the silicone resin takes place deformation, the electrically conductive path that graphite alkene formed also changes thereupon, can not form the short circuit or open circuit, the electrically conductive stability of graphite alkene electric heating film has been ensured, and utilize graphite alkene and electrically conductive thick liquids collocation use, make the electrically conductive path internal resistance that graphite alkene electric heating film formed lower, electrically conductive performance is better, the electric conductivity is higher, then make the better more stable of the heating performance of graphite alkene electric heating PI diaphragm, satisfy user's demand.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
Fig. 1 is a schematic flow chart of a manufacturing process of a graphene electrothermal PI membrane provided in an embodiment of the present invention.
Detailed Description
The embodiment of the invention discloses a manufacturing process of a graphene electric heating PI membrane, which is used for solving the technical problems of poor conductivity and unstable conductivity of the existing graphene electric heating product.
In order that those skilled in the art will better understand the disclosure, the invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
Referring to fig. 1, a process for manufacturing a graphene electrothermal PI film provided in this embodiment includes the following steps:
s1, mixing a conductive agent, a dispersing agent, a leveling agent, a wetting agent, a defoaming agent and conductive carbon black, and performing high-speed dispersion and grinding treatment to obtain conductive slurry;
s2, adding a catalyst into the silicone resin, heating for reaction for a preset time, and then cooling to room temperature of 25 ℃;
s3, stirring and mixing the graphene, the silicon resin and the conductive paste according to a preset mixing proportion, and dispersing at a high speed to obtain electrothermal paste;
s4, preparing a PI membrane, coating the electric heating slurry on the surface of the PI membrane, and then heating and drying the electric heating slurry to form a graphene electric heating film on the surface of the PI membrane, so that the graphene electric heating PI membrane is obtained.
The PI film (polyimide film) is formed by polycondensing pyromellitic dianhydride (PMDA) and diaminodiphenyl ether (DDE) in a strongly polar solvent, casting the resulting film, and imidizing the resulting film, and has good insulating properties.
In the embodiment, the silicone resin is a siloxane polymer with a branched structure, and is heated to react under the action of a catalyst to further generate a high polymer in a shape, and the silicon-oxygen bond in the silicone resin has high bonding performance and specificity on a molecular structure, so that the silicone resin has high heat resistance and excellent electrical performance. Through mixing silicone resin with conductive paste and graphite alkene, make graphite alkene can alternate in the three-dimensional structure that forms when the silicone resin cross-linking polymerization, when the silicone resin takes place deformation, the electrically conductive path that graphite alkene formed also changes thereupon, can not form the short circuit or open circuit, the electrically conductive stability of graphite alkene electric heating film has been ensured, and utilize graphite alkene and the built-up use of electrically conductive thick liquids, make the electrically conductive path internal resistance that graphite alkene electric heating film formed lower, electrically conductive performance is better, the conductivity is higher, then make the better more stable of the heating performance of graphite alkene electric heating PI diaphragm, satisfy user's demand.
Further, the step S1 specifically includes:
mixing a conductive agent, a dispersing agent, a leveling agent, a wetting agent, a defoaming agent and conductive carbon black, and performing high-speed dispersion by a high-speed dispersion machine and grinding by a grinding machine to obtain conductive slurry;
the speed of the high-speed dispersion machine is 1000-2000 r/min, and the processing time is 30-40 min; the speed of the mill was 2500r/min and the treatment time was 20min to 30 min.
Further, the conductive slurry comprises, by mass, 5-55% of conductive carbon black, 5-20% of a conductive agent, 1-15% of a dispersing agent, 0.11-5% of a leveling agent, 0.11-5% of a wetting agent, and 0.11-5% of a defoaming agent.
Further, the step S4 specifically includes:
preparing a PI membrane, coating the electric heating slurry on the surface of the PI membrane in a screen printing or blade coating or spraying manner, and drying the electric heating slurry through a baking oven, so that a graphene electric heating film is formed on the surface of the PI membrane, and the graphene electric heating PI membrane is obtained, wherein the baking temperature is 200-250 ℃, and the baking time is 30-40 min.
Specifically, the thickness of the graphene electric heating film in the graphene electric heating PI membrane formed by the above process is 0.2 to 0.3mm, and the thickness of the PI membrane is 0.2 to 1.5 mm.
The conductive heating paste may be coated on the surface of the PI film by a screen printing, blade coating, or spraying method, and the conductive heating paste may be coated on the surface of the PI film by a blade coater, for example.
Further, the step S3 specifically includes:
according to the graphene: silicone resin: and (3) stirring and mixing the graphene, the silicone resin and the conductive paste according to the proportion of 2:7:1, and dispersing at a high speed to obtain the electrothermal paste.
In the above step, the graphene, the silicone resin and the conductive paste are dispersed at a high speed by a high-speed disperser, wherein the speed of the high-speed disperser is 1000-2000 r/min, and the processing time is 30-40 min.
In addition, the graphene: silicone resin: the proportion of the conductive paste can be adjusted according to actual conditions, and the ratio of the graphene: silicone resin: the conductive paste is 2:7:1, which is a preferred mixing ratio in this embodiment.
Further, the step S2 specifically includes:
adding a catalyst into the silicone resin, carrying out heating reaction at 100-150 ℃ for 30-60 min, and then cooling to room temperature of 25 ℃;
the catalyst is hydrogen chloride.
The silicone resin is a siloxane polymer with a branched structure, and is further subjected to a heating reaction under the action of a catalyst to generate a high polymer, and the silicone resin has high bonding energy of a silicon-oxygen bond and special molecular structure, so that the silicone resin has high heat resistance and excellent electrical performance.
Further, the dispersing agent comprises one or more of carboxylic acid cellulose, polyethylene glycol and acetic acid cellulose.
It should be noted that the dispersant can reduce the time and energy required for the conductive paste to complete the dispersion process, and the actual production personnel can select the proper type of dispersant according to the requirements.
Further, the leveling agent comprises one or more of diethylene glycol ethyl ether acetate, isophorone, polydimethylsiloxane and polymethylphenyl siloxane.
The leveling agent can effectively reduce the surface tension of the conductive paste and improve the leveling property and uniformity of the conductive paste, and actual production personnel can select a proper type of leveling agent according to requirements.
Further, the conductive agent comprises one or more of conductive graphite powder, acetylene black, carbon nanotubes, carbon nanofibers and ketjen black.
The conductive agent can improve the conductive performance of the conductive paste, and the conductive paste and the graphene are matched for use, so that the conductive path formed by the graphene electric heating film is lower in internal resistance, better in conductive performance and higher in conductivity, the heating performance of the graphene electric heating PI film is better and more stable, and the requirements of users are met;
the actual production personnel can select the proper type of conductive agent according to the requirement.
Further, the wetting agent comprises one or more of polyoxyethylene alkylamine, sodium butylnaphthalene sulfonate and sodium alkyl sulfate;
it should be noted that the wetting agent is a surfactant which can make the material more easily wet by water by reducing the surface tension thereof, and the actual manufacturer can select an appropriate type of wetting agent according to the requirement.
The defoaming agent comprises one or more of a fatty acid defoaming agent, a polyurethane defoaming agent and an organic fluorine defoaming agent.
It should be noted that the defoaming agent functions to suppress the generation of foam in the conductive paste, and an appropriate type of defoaming agent can be selected by a practical manufacturer according to the need.
Further, the graphene electric heating PI membrane obtained by the manufacturing process of the embodiment can be applied to gloves, clothes, mattresses, physiotherapy heating pastes, blankets and the like, and heating of the graphene electric heating membrane can be realized by connecting the graphene electric heating membrane on the graphene electric heating PI membrane to a power supply circuit.
The above description describes in detail a manufacturing process of a graphene electrothermal PI film provided by the present invention, and for those skilled in the art, there may be changes in the specific implementation and application ranges according to the ideas of the embodiments of the present invention.
Claims (10)
1. A manufacturing process of a graphene electric heating PI membrane is characterized by comprising the following steps;
s1, mixing a conductive agent, a dispersing agent, a leveling agent, a wetting agent, a defoaming agent and conductive carbon black, and performing high-speed dispersion and grinding treatment to obtain conductive slurry;
s2, adding a catalyst into the silicone resin, heating for reaction for a preset time, and then cooling to room temperature of 25 ℃;
s3, stirring and mixing the graphene, the silicon resin and the conductive paste according to a preset mixing proportion, and dispersing at a high speed to obtain electrothermal paste;
s4, preparing a PI membrane, coating the electric heating slurry on the surface of the PI membrane, and then heating and drying the electric heating slurry to form a graphene electric heating film on the surface of the PI membrane, so that the graphene electric heating PI membrane is obtained.
2. The manufacturing process of the graphene electric heating PI diaphragm as claimed in claim 1, wherein the conductive slurry comprises, by mass, 5-55% of conductive carbon black, 5-20% of a conductive agent, 1-15% of a dispersing agent, 0.11-5% of a leveling agent, 0.11-5% of a wetting agent, and 0.11-5% of an antifoaming agent.
3. The manufacturing process of the graphene electrothermal PI film according to claim 1, wherein the step S4 specifically includes:
preparing a PI membrane, coating the electric heating slurry on the surface of the PI membrane in a screen printing or blade coating or spraying manner, and drying the electric heating slurry through a baking oven, so that a graphene electric heating film is formed on the surface of the PI membrane, and the graphene electric heating PI membrane is obtained, wherein the baking temperature is 200-250 ℃, and the baking time is 30-40 min.
4. The manufacturing process of the graphene electrothermal PI film according to claim 1, wherein the step S3 specifically includes:
according to the graphene: silicone resin: and (3) stirring and mixing the graphene, the silicone resin and the conductive paste according to the proportion of 2:7:1, and dispersing at a high speed to obtain the electrothermal paste.
5. The manufacturing process of the graphene electrothermal PI film according to claim 1, wherein the step S2 specifically includes:
adding a catalyst into the silicone resin, carrying out heating reaction at the temperature of 100-150 ℃ for 30-60 min, and then cooling to room temperature of 25 ℃.
6. The manufacturing process of the graphene electrothermal PI membrane according to claim 5, wherein the catalyst is hydrogen chloride.
7. The manufacturing process of the graphene electrothermal PI membrane according to claim 1, wherein the dispersant comprises one or more of carboxylic acid-based cellulose, polyethylene glycol and acetate-based cellulose.
8. The manufacturing process of the graphene electrothermal PI membrane according to claim 1, wherein the leveling agent comprises one or more of diethylene glycol ethyl ether acetate, isophorone, polydimethylsiloxane and polymethylphenylsiloxane.
9. The manufacturing process of the graphene electrothermal PI film according to claim 1, wherein the conductive agent comprises one or more of conductive graphite powder, acetylene black, carbon nanotubes, carbon nanofibers and Ketjen black.
10. The manufacturing process of the graphene electrothermal PI film according to claim 1, wherein the wetting agent comprises one or more of polyoxyethylene alkylamine, sodium butylnaphthalene sulfonate and sodium alkyl sulfate;
the defoaming agent comprises one or more of a fatty acid defoaming agent, a polyurethane defoaming agent and an organic fluorine defoaming agent.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210051140.6A CN114205937A (en) | 2022-01-17 | 2022-01-17 | Manufacturing process of graphene electric heating PI (polyimide) membrane |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559226A (en) * | 2018-05-03 | 2018-09-21 | 万美石墨烯科技无锡有限公司 | A kind of graphene heating film |
| CN109817385A (en) * | 2018-12-28 | 2019-05-28 | 常州碳森石墨烯科技有限公司 | A kind of preparation method that environment-friendly type graphene conductive carbon is starched and its application on flexible heating film |
| KR20190115639A (en) * | 2018-04-03 | 2019-10-14 | 비엔비머티리얼 주식회사 | Transparent heating film and preparation method thereof |
| CN111432508A (en) * | 2020-04-15 | 2020-07-17 | 威海无缝新材料有限公司 | Graphene fast heating film and preparation method thereof |
| CN112521796A (en) * | 2020-12-08 | 2021-03-19 | 苏州烯时代材料科技有限公司 | Graphene heating ink and preparation method and application thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190115639A (en) * | 2018-04-03 | 2019-10-14 | 비엔비머티리얼 주식회사 | Transparent heating film and preparation method thereof |
| CN108559226A (en) * | 2018-05-03 | 2018-09-21 | 万美石墨烯科技无锡有限公司 | A kind of graphene heating film |
| CN109817385A (en) * | 2018-12-28 | 2019-05-28 | 常州碳森石墨烯科技有限公司 | A kind of preparation method that environment-friendly type graphene conductive carbon is starched and its application on flexible heating film |
| CN111432508A (en) * | 2020-04-15 | 2020-07-17 | 威海无缝新材料有限公司 | Graphene fast heating film and preparation method thereof |
| CN112521796A (en) * | 2020-12-08 | 2021-03-19 | 苏州烯时代材料科技有限公司 | Graphene heating ink and preparation method and application thereof |
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