CN115038201B - Preparation method and application of multifunctional flexible heating film - Google Patents
Preparation method and application of multifunctional flexible heating film Download PDFInfo
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- CN115038201B CN115038201B CN202210605440.4A CN202210605440A CN115038201B CN 115038201 B CN115038201 B CN 115038201B CN 202210605440 A CN202210605440 A CN 202210605440A CN 115038201 B CN115038201 B CN 115038201B
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- heating film
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/36—Hydroxylated esters of higher fatty acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3855—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur
- C08G18/3863—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur containing groups having sulfur atoms between two carbon atoms, the sulfur atoms being directly linked to carbon atoms or other sulfur atoms
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Surface Heating Bodies (AREA)
Abstract
The invention discloses a preparation method and application of a multifunctional flexible heating film, wherein the method comprises the following steps: step one, putting a heating element into polyurethane or PDMS precursor liquid with bubbles removed, curing for 2-12 h at 50-100 ℃, and packaging into a polymer: and step two, dispersing 0.2-2 g of hydrophobic nano particles in 0.5-10 g of volatile solvent, spraying the dispersion liquid on the upper surface of the heating film, and volatilizing the solvent to obtain the multifunctional flexible heating film. According to the invention, after the heating film is prepared by compounding the flexible material and the heating element, the super-hydrophobic surface is obtained by using the method of spraying the hydrophobic nano particles, compared with other preparation methods such as blade coating, spin coating, deposition method and template method, the spraying method has the advantages of simple operation, low cost, large-area preparation and the like, and the heating film can obtain self-cleaning performance by introducing the super-hydrophobic surface, so that the heating film can be better used under various environmental conditions.
Description
Technical Field
The invention relates to a preparation method of a flexible heating film, in particular to a preparation method and application of a self-adhesion and super-hydrophobic heating film.
Background
The resistance heating is the most widely used electric heating mode, people produce electric heating film materials according to the needs of production and life, and compared with the traditional electric heating element, the electric heating film has the advantages of high heating efficiency, safety, reliability, variable geometric shapes, wide application range and the like, so the electric heating film has wide application in many fields of heat preservation of industrial pipelines, vegetable greenhouses and living rooms, platform heating, road snow melting and the like.
The electric heating membrane material comprises conductive heating layer and substrate layer, and the heating membrane on the market is the polyimide substrate mostly now, and the unable self-adhesion of this kind of substrate is on the material surface, so there is the gum in the one side of heating membrane, and this kind of glue can't used repeatedly many times, in external environment moreover, receives the pollution easily, influences the heat transfer and the use of heating membrane, so need one kind can reversible adhesion, resistant various environment's electric heating membrane.
Disclosure of Invention
In order to solve the problems that the existing heating film cannot be reversibly adhered and cannot adapt to various environments, the invention provides a preparation method and application of a multifunctional flexible heating film which is reversibly adhered, self-cleaned, anti-icing and corrosion-resistant.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a multifunctional flexible heating film comprises the following steps:
step one, putting a heating element into polyurethane or PDMS precursor liquid with bubbles removed, curing at 50-100 ℃ for 2-12 h, and packaging into a polymer, wherein:
the heating element is a resistance wire or a resistance card;
the resistance wire is made of iron-nickel-chromium alloy;
the polyurethane is prepared by uniformly mixing castor oil, isophorone diisocyanate (IPDI), bis (2-hydroxyethyl) disulfide (HEDS) and a catalyst (dibutyltin dilaurate), wherein: the mass ratio of castor oil, isophorone diisocyanate (IPDI) and bis (2-hydroxyethyl) disulfide (HEDS) is 7-13: 4 to 6: 1-2, the addition of the catalyst is 0.2-1 wt% of the polyurethane;
in the PDMS precursor, the proportion of PDMS to the curing agent is 10:0.25 to 1.5.
Step two, dispersing 0.2-2 g of hydrophobic nano particles in 0.5-10 g of volatile solvent, spraying the dispersion liquid on the upper surface of the heating film, and obtaining the multifunctional heating film after the solvent is volatilized, wherein:
the hydrophobic nano particles are multi-walled carbon nano tubes, hydrophobic gas phase nano silicon dioxide or nano titanium dioxide and the like;
the volatile solvent is dichloromethane, ethyl acetate, trichloromethane or ethanol and the like;
the concentration of the dispersion liquid is 1-5 mg/mL;
the multifunctional heating film has excellent heating stability, can be adhered to the surface of a special-shaped structure to be heated randomly, reversibly and repeatedly to heat the special-shaped structure, and meanwhile, the exposed surface has excellent self-cleaning performance, so that the heating film is prevented from being polluted.
The application of the multifunctional flexible heating film prepared by the method in the special-shaped structure to be heated is as follows:
the multifunctional heating film is adhered to the surface of a special-shaped structure to be heated at will, reversibly and repeatedly, the heating element is utilized to heat the structure to be heated, heating time, heating power and the like are determined according to the characteristics of the special-shaped body to be heated, meanwhile, in the heating process, heat is transferred to the back of the heating film, water cannot freeze, the surface is a super-hydrophobic thin layer, the multifunctional heating film has self-cleaning performance, the multifunctional heating film can keep a clean surface in an external environment, liquid drops cannot be attached to the surface of the multifunctional heating film when the heating film does not work, and therefore the anti-icing effect is achieved.
Compared with the prior art, the invention has the following advantages:
1. the back adhesive layer of the electrothermal film in the market cannot be reused for obtaining larger adhesive force, and once the back adhesive layer is removed, not only residues are left, but also objects cannot be adhered again. The polyurethane and PDMS used in the invention are common flexible materials, and can obtain larger adhesion performance by adjusting the content of the curing component, and can be reversibly adhered to various objects to meet the use requirements, and the adhesion force is basically unchanged after heating; and no residue is left on the surface of the object after desorption, and the adhesion performance of the heating film substrate cannot be reduced, so that the heating film substrate can be repeatedly used, the using number of the heating films can be reduced in the actual using process, and the cost is reduced.
2. Compared with other preparation methods, such as blade coating, spin coating, deposition method and template method, the spray coating method has the advantages of simple operation, low cost, large-area preparation and the like, and the heating film can obtain self-cleaning performance by introducing the super-hydrophobic surface, so that the heating film can be better used under various environmental conditions.
3. The polyurethane and the PDMS have good environmental stability, and after the polyurethane and the PDMS are placed in an acid-base salt environment for 12 hours, the adhesion performance and the hydrophobic property of the super-hydrophobic coating cannot be obviously changed, so that the adhered object can be protected, and the influence of the acid-base salt on the adhered object can be prevented.
Drawings
FIG. 1 shows the adhesion properties of different raw material ratios of polyurethane and PDMS, (a) the adhesion strength of polyurethane prepared at different molar ratios (IPDI: castor oil: HEDS), (b) the adhesion strength of PDMS prepared at different curing agent contents;
FIG. 2 is the contact angle of the polyurethane surface after spraying solutions of different carbon nanotube concentrations, a) 1mg/mL-135 degrees, b) 2mg/mL-145 degrees, c) 3mg/mL-153 degrees, d) 4mg/mL-160 degrees;
FIG. 3 is a front electron micrograph of films at different MWCNT concentrations, a) 1mg/mL, b) 2mg/mL, c) 3mg/mL, d) 4mg/mL;
FIG. 4 is the contact angle of the polyurethane surface after soaking in solutions of different pH values for 12 h.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
the embodiment provides a preparation method of a multifunctional flexible heating film, which comprises the following steps:
And 2, selecting polyurethane as a heating film substrate material, putting the resistance wire into the polyurethane with bubbles removed, curing for 2h at 80 ℃, and packaging the resistance wire into a polymer. In order to allow the heating element to be in the middle position of the material, half of the polymer may be pre-cured, the resistive element placed and the remaining polymer added.
The preparation process of the polyurethane comprises the following steps: (1) Uniformly mixing castor oil, isophorone diisocyanate (IPDI), 1-2 g bis (2-hydroxyethyl) disulfide (HEDS) and a catalyst dibutyltin dilaurate, and controlling the ratio of IPDI: castor oil: HEDS =2, 0.74. The adhesion performance of the polyurethane according to the ratio of different raw materials is shown in fig. 1 (a), the material prepared by continuously increasing the content of castor oil is not molded, and residues are left on the surface after adhesion.
And 3, dispersing the multi-wall carbon nano-tube in dichloromethane by ultrasonic or stirring to prepare dispersion liquid with the concentration of 1mg/mL, 2mg/mL, 3mg/mL and 4 mg/mL. And spraying the dispersion liquid on the upper surface of the heating film, wherein the polyurethane is swelled by the solvent, and after the solvent is volatilized by heating, the nano particles can be firmly attached to the matrix to obtain the super-hydrophobic surface. Fig. 2 is a contact angle of the surface of the polyurethane after the polyurethane surface is sprayed with carbon nanotube solutions of different concentrations, and it can be seen that the contact angle of the polyurethane surface becomes larger with the increasing concentration, and finally becomes super-hydrophobic. As can be seen from the SEM picture of polyurethane of fig. 3, the higher the concentration of the dispersion, the more the stacking of the surface multi-walled carbon nanotubes is severe, and the greater the surface roughness of the composite material obtained by spraying, which is consistent with the increasing trend of the contact angle.
The polyurethane surface has adhesive property, can be reversibly adhered to various base materials, has no residue after being peeled off, and can be repeatedly used, wherein the adhesive strength of the polyurethane can reach 0.45MPa; the super-hydrophobic thin layer enables the heating film to have self-cleaning performance, and the heating film can keep a clean surface in an external environment. Through testing, as can be seen from fig. 4, the surface superhydrophobic coating can still maintain superhydrophobicity after being soaked in solutions with different pH (pH = 1-13) for 12 h. In addition, in the working process of the heating film, heat is transferred to the back of the heating film, water cannot freeze, and because the surface is super-hydrophobic, liquid drops cannot be attached to the surface of the heating film when the heating film does not work, so that the anti-icing effect is achieved.
Tests show that the heating film can be heated to 80 ℃ within 5min under the action of 20V voltage, the bonding property of the heating film and a substrate is good after the heating film is heated, the separation phenomenon cannot occur, and the use requirement is basically met.
Example 2:
the embodiment provides a preparation method of a multifunctional flexible heating film, which comprises the following steps:
and step 1, using the finished product of the resistance card as a heating element.
And 2, selecting PDMS as a substrate material of the heating film. Putting the resistance chip into the bubble-removed PDMS precursor liquid, and controlling the proportion of PDMS and a curing agent to be 10:0.25, 10: 5. 10:0.75, 10:1. 10:1.25 And curing at 50 ℃ for 4h to encapsulate the epoxy resin into a polymer. In order to allow the heating element to be in the middle position of the material, one half of the polymer may be pre-cured, the resistive element placed and the remaining polymer added.
The adhesion performance of different raw material ratios of PDMS is shown in FIG. 1, the material prepared by continuously reducing the content of PDMS curing agent is not molded, and the surface has residue after adhesion.
And 3, dispersing the hydrophobic gas-phase nano silicon dioxide in ethanol by ultrasonic or stirring, preparing dispersion liquid with the concentration of 1mg/mL, 2mg/mL, 3mg/mL or 4mg/mL, and spraying the dispersion liquid on the upper surface of the heating film.
The PDMS surface has adhesive property, can be reversibly adhered to various base materials, has no residue after being removed, and can be repeatedly used; the super-hydrophobic thin layer enables the heating film to have self-cleaning performance, and the heating film can keep a clean surface in an external environment. In addition, in the working process of the heating film, heat is transferred to the back of the heating film, water cannot freeze, and liquid drops cannot be attached to the surface of the heating film when the heating film does not work due to the fact that the surface is super-hydrophobic, so that the anti-icing effect is achieved.
Claims (7)
1. A preparation method of a multifunctional flexible heating film is characterized by comprising the following steps:
step one, putting a heating element into polyurethane or PDMS precursor liquid with bubbles removed, curing at 50-100 ℃ for 2-12 h, and encapsulating into a polymer; the polyurethane is prepared by uniformly mixing castor oil, isophorone diisocyanate, bis (2-hydroxyethyl) disulfide and a catalyst, wherein: the mass ratio of castor oil to isophorone diisocyanate to bis (2-hydroxyethyl) disulfide is 7 to 13:4 to 6:1 to 2, wherein the addition amount of the catalyst is 0.2 to 1wt% of the polyurethane; in the PDMS precursor, the proportion of PDMS to the curing agent is 10:0.25 to 1.5;
and secondly, dispersing 0.2 to 2g of hydrophobic nano particles in 0.5 to 10g of volatile solvent, spraying the dispersion liquid on the upper surface of the heating film, and volatilizing the solvent to obtain the multifunctional flexible heating film, wherein the volatile solvent is dichloromethane, ethyl acetate, trichloromethane or ethanol.
2. The method for preparing the multifunctional flexible heating film according to claim 1, wherein the heating element is a resistance wire or a resistance card, and the resistance wire is made of iron-nickel-chromium alloy.
3. The method for preparing a multifunctional flexible heating film according to claim 1, wherein the catalyst is dibutyltin dilaurate.
4. The method for preparing a multifunctional flexible heating film according to claim 1, wherein the hydrophobic nanoparticles are multi-walled carbon nanotubes, hydrophobic fumed nanosilica or nano-titania.
5. The method for preparing the multifunctional flexible heating film according to claim 1, wherein the concentration of the dispersion is 1 to 5 mg/mL.
6. Use of a multifunctional flexible heating film prepared by the method of any one of claims 1 to 5 in a shaped structure to be heated.
7. The multifunctional flexible heating film of claim 6, wherein the specific method of application is as follows:
the multifunctional heating film is adhered to the surface of the special-shaped structure to be heated at will, reversibly and repeatedly, the heating element is utilized to heat the structure to be heated, heat is transferred to the back of the heating film in the heating process, water cannot freeze, the surface is a super-hydrophobic thin layer, the multifunctional heating film has self-cleaning performance, the multifunctional heating film can keep a clean surface in an external environment, and liquid drops cannot be adhered to the surface of the multifunctional heating film when the heating film does not work, so that the anti-icing effect is achieved.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6847018B2 (en) * | 2002-02-26 | 2005-01-25 | Chon Meng Wong | Flexible heating elements with patterned heating zones for heating of contoured objects powered by dual AC and DC voltage sources without transformer |
| JP2010169303A (en) * | 2009-01-22 | 2010-08-05 | Panasonic Corp | Electric warmer |
| CN105032731B (en) * | 2015-08-05 | 2018-12-28 | 北京航空航天大学 | A kind of energy-saving prevention de-icing coating preparation method that super-hydrophobic coat is compound with heating coating |
| CN107987787A (en) * | 2017-12-15 | 2018-05-04 | 阜阳市龙建包装材料有限公司 | A kind of high flame-retardant polyurethane adhesive |
| CN110951109B (en) * | 2019-11-05 | 2021-07-20 | 东华大学 | Bacterial cellulose/polypyrrole/polyurethane flexible multifunctional conductive composite material and preparation method thereof |
| CN112552717A (en) * | 2020-11-20 | 2021-03-26 | 武汉理工大学 | Novel anti-icing and deicing coating for composite material wing of airplane and preparation method thereof |
| CN112940308B (en) * | 2021-01-14 | 2023-01-03 | 西安交通大学 | Preparation method of PDMS (polydimethylsiloxane) super-hydrophobic flexible film with switchable transparent/opaque state |
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