CN110606968A - Preparation method of titanium dioxide/graphene flexible electrothermal film - Google Patents
Preparation method of titanium dioxide/graphene flexible electrothermal film Download PDFInfo
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- CN110606968A CN110606968A CN201911013398.1A CN201911013398A CN110606968A CN 110606968 A CN110606968 A CN 110606968A CN 201911013398 A CN201911013398 A CN 201911013398A CN 110606968 A CN110606968 A CN 110606968A
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- graphene
- methyl ether
- glycol methyl
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- acrylic resin
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- 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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- 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
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- 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
Abstract
The invention discloses a preparation method of a titanium dioxide/graphene flexible electrothermal film, which comprises the steps of respectively cleaning a PET film by deionized water and ethanol, and airing; weighing graphene and adding TiF4Reacting in the solution, after the reaction is finished, washing the precipitate with water and ethanol, and drying to obtain TiO2Graphene powder; respectively weighing acrylic resin, propylene glycol methyl ether acetate, propylene glycol methyl ether and dipropylene glycol methyl ether, placing the acrylic resin, the propylene glycol methyl ether acetate, the propylene glycol methyl ether and the dipropylene glycol methyl ether in a reaction kettle, and carrying out homogeneous reaction to obtain an acrylic resin solution; weighing TiO2Adding graphene powder and carbon black into acrylic resin solution, and stirring to obtain TiO2Graphene slurry; adding TiO into the mixture2Coating the graphene slurry on a PET film, and dryingDrying to obtain TiO2A graphene flexible electrothermal film. The invention prepares TiO2The graphene flexible electrothermal film has the advantages of simple process, good repeatability and low cost.
Description
Technical Field
The invention relates to a preparation method of an electrothermal film, in particular to a preparation method of a titanium dioxide/graphene flexible electrothermal film.
Background
With the continuous development of economy and the enhancement of environmental awareness, the demand of people on electric heating equipment, electric heating physiotherapy products and the like is continuously increased. Carbon materials such as carbon crystals and carbon fibers are the most common electrocaloric materials. Graphene, as a novel carbon material, has unique structure and physicochemical properties. When the graphene is used as an electrothermal film, the graphene has the advantages of quick heating, uniform heating, high heating efficiency and the like. However, the graphene electrothermal film prepared by the prior art has the problems of high cost, poor flexibility, short service life and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a titanium dioxide/graphene flexible electrothermal film to overcome the defects of the prior art, and the invention prepares TiO2The graphene flexible electrothermal film has the advantages of simple process, good repeatability and low cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a titanium dioxide/graphene flexible electrothermal film comprises the following steps:
1) washing the PET film with deionized water and ethanol respectively, and drying;
2) weighing graphene and adding TiF4Reacting in the solution, after the reaction is finished, washing the precipitate with water and ethanol, and drying to obtain TiO2Graphene powder;
3) respectively weighing acrylic resin, propylene glycol methyl ether acetate, propylene glycol methyl ether and dipropylene glycol methyl ether, placing the acrylic resin, the propylene glycol methyl ether acetate, the propylene glycol methyl ether and the dipropylene glycol methyl ether in a reaction kettle, and carrying out homogeneous reaction to obtain an acrylic resin solution;
4) weighing TiO2Adding graphene powder and carbon black into the acrylic resin solution obtained in the step 3), and stirring to obtain TiO2Graphene slurry;
5) adding TiO into the mixture2Coating the graphene slurry on the PET film obtained in the step 1), and drying to obtain TiO2A graphene flexible electrothermal film.
Further, every 100mltiF in step 2)4Adding 10g of graphene and TiF into the solution4The concentration of the solution was 40 mM.
Further, the reaction temperature in the step 2) is 60 ℃, and the reaction time is 1-3 h.
Further, the mass ratio of the acrylic resin, the propylene glycol methyl ether acetate, the propylene glycol methyl ether and the dipropylene glycol methyl ether in the step 3) is 9:3:1: 27.
Further, the homogeneous reaction temperature in the step 3) is 100 ℃, and the time is 5 hours.
Further, TiO in step 4)2The mass ratio of the graphene powder to the carbon black is 1 (3-5).
Further, 10g of TiO was added to 50g of the acrylic resin solution in the step 4)2A mixture of graphene powder and carbon black.
Further, the drying temperature in the step 5) is 120 ℃ and the time is 10 min.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention is used for preparing the TiF of the graphene at lower temperature4Treatment to obtain TiO2Graphene composites, TiO2The nano particles are uniformly distributed on the graphene sheet, so that the accumulation of graphene sheet layers is effectively prevented, and the specific surface area of the graphene sheet is increased. Adding TiO into the mixture2Mixing graphene with carbon black and acrylic resin solution to obtain TiO2Graphene paste, TiO obtained by coating2The graphene flexible electrothermal film has good electrothermal characteristics, and the temperature can reach 70-110 ℃ under the action of 15V constant voltageAnd the application prospect is good.
Drawings
FIG. 1 shows TiO prepared in example 22SEM image of/graphene.
FIG. 2 shows TiO prepared in example 2 at 15V DC voltage2A temperature-time relation diagram of the graphene flexible electric heating film.
Detailed Description
Embodiments of the invention are described in further detail below:
a preparation method of a titanium dioxide/graphene flexible electrothermal film comprises the following steps:
1) the PET film was washed with deionized water and with ethanol, respectively, and dried.
2) 10g of graphene are weighed into 100ml of 40mM TiF4Reacting in the solution for 1-3 hours at 60 ℃, and cleaning and drying the precipitate with water and ethanol to obtain TiO2Graphene powder.
3) 9g of an acrylic resin, 3g of propylene glycol methyl ether acetate, 1g of propylene glycol methyl ether and 27g of dipropylene glycol methyl ether were weighed and placed in a reaction vessel, and heated at 100 ℃ for 5 hours in a homogeneous reactor to obtain an acrylic resin solution.
4) 10g of TiO are weighed2Adding graphene and carbon black (the mass ratio is 1: 3-5) into 50g of the acrylic resin solution obtained in the step 3), and stirring for 1 hour to obtain TiO2Graphene slurry.
5) The prepared TiO is mixed with2Coating the graphene slurry on a PET (polyethylene terephthalate) film through screen printing, and drying at 120 ℃ for 10 minutes to obtain TiO2A graphene flexible electrothermal film.
The present invention is described in further detail below with reference to examples:
example 1
1) The PET film was washed with deionized water and with ethanol, respectively, and dried.
2) 10g of graphene are weighed into 100ml of 40mM TiF4Reacting in the solution at 60 ℃ for 3 hours, washing and drying the precipitate with water and ethanol to obtain TiO2Graphene powder.
3) 9g of an acrylic resin, 3g of propylene glycol methyl ether acetate, 1g of propylene glycol methyl ether and 27g of dipropylene glycol methyl ether were weighed and placed in a reaction vessel, and heated at 100 ℃ for 5 hours in a homogeneous reactor to obtain an acrylic resin solution.
4) 10g of TiO are weighed2Adding graphene and carbon black (the mass ratio is 1:3) into the acrylic resin solution obtained in the step 3), and stirring for 1 hour to obtain TiO2Graphene slurry.
5) The prepared TiO is mixed with2Coating the graphene slurry on a PET (polyethylene terephthalate) film through screen printing, and drying at 120 ℃ for 10 minutes to obtain TiO2A graphene flexible electrothermal film. After 15V voltage is applied to two ends of the electric heating film, the temperature can reach about 105 ℃ after the electric heating film is stabilized.
Example 2
1) The PET film was washed with deionized water and with ethanol, respectively, and dried.
2) 10g of graphene are weighed into 100ml of 40mM TiF4Reacting in the solution at 60 ℃ for 3 hours, washing and drying the precipitate with water and ethanol to obtain TiO2Graphene powder.
3) 9g of an acrylic resin, 3g of propylene glycol methyl ether acetate, 1g of propylene glycol methyl ether and 27g of dipropylene glycol methyl ether were weighed and placed in a reaction vessel, and heated at 100 ℃ for 5 hours in a homogeneous reactor to obtain an acrylic resin solution.
4) 10g of TiO are weighed2Adding graphene and carbon black (the mass ratio is 1:4) into the acrylic resin solution obtained in the step 3), and stirring for 1 hour to obtain TiO2Graphene slurry.
5) The prepared TiO is mixed with2Coating the graphene slurry on a PET (polyethylene terephthalate) film through screen printing, and drying at 120 ℃ for 10 minutes to obtain TiO2A graphene flexible electrothermal film. After 15V voltage is applied to two ends of the electric heating film, the temperature can reach about 85 ℃ after the electric heating film is stabilized.
As can be seen from FIG. 1, graphene is in TiF4After standing in the solution for 3 hours, TiO uniformly grows on the graphene sheet2The nano particles effectively prevent the graphene sheets from being stacked and agglomerated.
As can be seen from fig. 2, after a voltage of 15V is applied to both ends of the electric heating film of example 2, the temperature rises to about 85 ℃ after about 55 seconds, and the temperature tends to be stable.
Example 3
1) The PET film was washed with deionized water and with ethanol, respectively, and dried.
2) 10g of graphene are weighed into 100ml of 40mM TiF4Reacting in the solution for 1-3 hours at 60 ℃, and cleaning and drying the precipitate with water and ethanol to obtain TiO2Graphene powder.
3) 9g of an acrylic resin, 3g of propylene glycol methyl ether acetate, 1g of propylene glycol methyl ether and 27g of dipropylene glycol methyl ether were weighed and placed in a reaction vessel, and heated at 100 ℃ for 5 hours in a homogeneous reactor to obtain an acrylic resin solution.
4) 10g of TiO are weighed2Adding graphene and carbon black (the mass ratio is 1:5) into the acrylic resin solution obtained in the step 3), and stirring for 1 hour to obtain TiO2Graphene slurry.
5) The prepared TiO is mixed with2Coating the graphene slurry on a PET (polyethylene terephthalate) film through screen printing, and drying at 120 ℃ for 10 minutes to obtain TiO2A graphene flexible electrothermal film. After 15V voltage is applied to two ends of the electric heating film, the temperature can reach about 70 ℃ after the electric heating film is stabilized.
Claims (8)
1. A preparation method of a titanium dioxide/graphene flexible electrothermal film is characterized by comprising the following steps:
1) washing the PET film with deionized water and ethanol respectively, and drying;
2) weighing graphene and adding TiF4Reacting in the solution, after the reaction is finished, washing the precipitate with water and ethanol, and drying to obtain TiO2Graphene powder;
3) respectively weighing acrylic resin, propylene glycol methyl ether acetate, propylene glycol methyl ether and dipropylene glycol methyl ether, placing the acrylic resin, the propylene glycol methyl ether acetate, the propylene glycol methyl ether and the dipropylene glycol methyl ether in a reaction kettle, and carrying out homogeneous reaction to obtain an acrylic resin solution;
4) weighing TiO2Adding graphene powder and carbon black into the acrylic resin solution obtained in the step 3), and stirring to obtain TiO2Graphene slurry;
5) adding TiO into the mixture2Coating the graphene slurry on the PET film obtained in the step 1), and drying to obtain TiO2A graphene flexible electrothermal film.
2. The preparation method of the titanium dioxide/graphene flexible electrothermal film according to claim 1, wherein in the step 2), every 100ml of the film is subjected to heating4Adding 10g of graphene and TiF into the solution4The concentration of the solution was 40 mM.
3. The preparation method of the titanium dioxide/graphene flexible electrothermal film according to claim 1, wherein the reaction temperature in the step 2) is 60 ℃ and the reaction time is 1-3 h.
4. The preparation method of the titanium dioxide/graphene flexible electrothermal film according to claim 1, wherein in the step 3), the mass ratio of the acrylic resin to the propylene glycol methyl ether acetate to the propylene glycol methyl ether to the dipropylene glycol methyl ether is 9:3:1: 27.
5. The preparation method of the titanium dioxide/graphene flexible electrothermal film according to claim 1, wherein the homogeneous reaction temperature in the step 3) is 100 ℃ and the time is 5 hours.
6. The preparation method of the titanium dioxide/graphene flexible electrothermal film according to claim 1, wherein TiO in the step 4) is adopted2The mass ratio of the graphene powder to the carbon black is 1 (3-5).
7. The preparation method of the titanium dioxide/graphene flexible electrothermal film according to claim 1, wherein 10g of TiO is added to 50g of acrylic resin solution in the step 4)2A mixture of graphene powder and carbon black.
8. The preparation method of the titanium dioxide/graphene flexible electrothermal film according to claim 1, wherein the drying temperature in the step 5) is 120 ℃ and the drying time is 10 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375439A (en) * | 2020-10-30 | 2021-02-19 | 陕西惠泽热能有限公司 | Preparation method of photo-curing carbon slurry for far infrared heating |
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2019
- 2019-10-23 CN CN201911013398.1A patent/CN110606968A/en active Pending
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375439A (en) * | 2020-10-30 | 2021-02-19 | 陕西惠泽热能有限公司 | Preparation method of photo-curing carbon slurry for far infrared heating |
| CN112375439B (en) * | 2020-10-30 | 2022-05-24 | 陕西惠泽热能有限公司 | Preparation method of photo-curing carbon paste for far infrared heating |
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Application publication date: 20191224 |