CN111556595A - Durable quick-heating multifunctional electrothermal film based on amyloid protein/reduced graphene oxide - Google Patents
Durable quick-heating multifunctional electrothermal film based on amyloid protein/reduced graphene oxide Download PDFInfo
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—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
-
- 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
- H05B3/146—Conductive polymers, e.g. polyethylene, thermoplastics
-
- 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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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a durable quick-heating multifunctional electric heating film based on amyloid protein/reduced graphene oxide, which comprises an upper insulating layer, electric heating sheets and a lower insulating layer, wherein the electric heating sheets are amyloid protein/reduced graphene oxide composite films, the electric heating sheets are adhered to the lower insulating layer at intervals and are packaged in the upper insulating layer and the lower insulating layer, and heating and conducting circuits are printed on the electric heating sheets. The invention utilizes the characteristics of amyloid protein/reduced graphene oxide composite membrane such as self stability, bending resistance, lightness, thinness and rapid temperature rise as the heating unit of the electrothermal film, can realize rapid temperature rise and durability, can be used for aspects such as electrothermal physical therapy blankets, thermal clothes, building heating, heating floors, far infrared health care rooms and household electric blankets, and provides better use experience for life.
Description
Technical Field
The invention belongs to the technical field of heating materials, and particularly relates to a durable quick-heating multifunctional electric heating film based on amyloid protein/reduced graphene oxide.
Background
The electric blanket is a household consumer product widely applied to life heating, and the electric blankets on the market are various in types but have the following defects: (1) the resistance wire electric blanket has large radiation to human body, unbalanced heating, slow heating temperature rise, insufficient flexibility, difficult bending and easy bending, and the like. (2) The carbon fiber electric blanket has the advantages of light weight, softness, good fitting degree and the like, and is widely used in recent years, but the problems of poor safety, easy combustion, easy breakage of internal fibers, low heating speed, easy loss of temperature, unbalanced heating and the like are gradually shown. (3) Compared with the two common electric blankets in the market, the graphene electric heating film is safe and environment-friendly, high in thermoelectric conversion rate, balanced in heating temperature, easy to control and the like, and is widely researched in recent years, but the graphene electric heating film also has the problems of insufficient flexibility, easiness in breaking, poor bending resistance, low heating temperature rise speed, short service life and the like.
The Yanpeng et al, university of Shaanxi, university of teahouse, is inspired by the marine organism barnacle, a certain amount of disulfide bond reducing agent tris (2-carboxyethyl) phosphine hydrochloride is added into lysozyme aqueous solution, lysozyme can rapidly generate phase transition to carry out amyloid-like aggregation in an aqueous phase mild environment close to physiological conditions, and the amyloid-like aggregation contains a large amount of beta-folding structures and can be firmly adhered to surface interfaces of various materials (inorganic, organic, metal, polymer and the like). Therefore, biomimetic adhesion based on protein amyloid transformation shows great potential in multifunctional graphene coating preparation.
Disclosure of Invention
The invention aims to provide a durable quick-heating multifunctional electrothermal film taking an amyloid protein/reduced graphene oxide composite film as an electrothermal material, wherein the electrothermal material has good adhesiveness, flexibility and stability, is not easy to short-circuit and can quickly raise the temperature of the electrothermal film in a short time.
The durable quick-heating multifunctional electric heating film based on the amyloid protein/reduced graphene oxide comprises an upper insulating layer, electric heating sheets and a lower insulating layer, wherein the electric heating sheets are amyloid protein/reduced graphene oxide composite films, the electric heating sheets are adhered to the lower insulating layer at intervals and are packaged inside the upper insulating layer and the lower insulating layer, and heating and conducting circuits are printed on the electric heating sheets.
The durable quick-heating multifunctional electrothermal film is prepared by the following method:
1. uniformly mixing a protein aqueous solution, a graphene oxide dispersion solution and a tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 3-10 of 10-100 mmol/L, and reacting the obtained mixed solution at 25-40 ℃ to enable the protein to generate amyloid-like conversion; wherein, the protein is one or more of lysozyme, bovine serum albumin, insulin and alpha-lactalbumin.
2. And (3) adjusting the pH value of the turbid liquid obtained after the reaction in the step (1) to 2-3, and reducing graphene oxide at 70-90 ℃.
3. Firstly, mounting a lower insulating layer at the bottom of a mould, then pouring the reduced graphene oxide turbid liquid obtained in the step (2) into the mould, and drying to form an amyloid protein/reduced graphene oxide composite membrane on the upper surface of the lower insulating layer, namely adhering electric heating sheets on the upper surface of the lower insulating layer at intervals; and taking out the lower insulating layer adhered with the electric heating sheet, printing a heating conductive circuit on the electric heating sheet, and fixing the upper insulating layer on the electric heating sheet through hot melt adhesive or hot-pressing adhesion, so that the electric heating sheet is packaged in the upper insulating layer and the lower insulating layer and the inside of the electric heating sheet is ensured to be in a vacuum state.
In the step 1, the protein is one or more of lysozyme, bovine serum albumin, insulin and alpha-lactalbumin; the concentration of the protein aqueous solution is 0.5-10 mg/mL, and the graphene oxide dispersion liquid is obtained by dispersing graphene oxide prepared by an improved Hummers method into deionized water by using ultrasonic waves, wherein the concentration of the graphene oxide is 0.1-10 mg/mL. Preferably, the concentration of the protein aqueous solution is 2-5 mg/mL, the concentration of graphene oxide in the graphene oxide dispersion liquid is 1-7 mg/mL, the pH value of the tris (2-carboxyethyl) phosphine hydrochloride aqueous solution is 4-7, and the concentration is 30-70 mmol/L.
In the step 1, it is further preferable that the obtained mixture is reacted at 25 to 40 ℃ for 2 to 10 hours.
In the step 2, preferably, the pH value of the mixed solution after the reaction in the step 1 is adjusted to 2-3 by using 1mol/L hydrochloric acid, and the graphene oxide is reduced for 6-9 hours at 70-90 ℃.
In the durable quick-heating multifunctional electrothermal film, the length of the electrothermal sheets is preferably 20-50 cm, the width of the electrothermal sheets is preferably 1-5 cm, and the interval between the electrothermal sheets is preferably 0.5-2.0 cm.
In the durable quick-heating multifunctional electrothermal film, the upper insulating layer and the lower insulating layer can be any one of a PI film, a PET film, a PVC film, a PP film, a PC film, a PS film, a PE film, ceramics, glass, a silica gel film, a mica sheet and the like.
In the durable quick-heating multifunctional electrothermal film, a preferable heating conductive circuit consists of a silver paste layer and a conductive sheet bonded on the silver paste layer, wherein the width of the silver paste layer is 0.5-2 cm, the thickness of the silver paste layer is 0.1-0.3 cm, the conductive sheet is any one of a copper sheet, a copper foil, an iron strip and a silver strip, the width of the conductive sheet is 0.5-2 cm, and the thickness of the conductive sheet is 0.1-1 cm.
The invention has the following beneficial effects:
1. the invention has mild operation condition, and does not need large-scale equipment and high energy consumption process.
2. In the process of preparing the electrothermal film, the amyloid protein/reduced graphene oxide composite film has good adhesiveness, and is fixed on the lower insulating layer without adding any glue additionally in the process of preparing the electrothermal sheet.
3. The electrothermal film has strong flexibility, bending resistance, stability, durability and long service life.
4. The electrothermal film has high thermoelectric conversion rate, can quickly respond thermally and obviously improve the temperature of the electrothermal film, can be used for aspects of electrothermal physical therapy blankets, thermal clothes, building heating, heating floors, far infrared health care rooms, household electric blankets and the like, and provides better use experience for life.
Drawings
Fig. 1 is a schematic structural view of a durable quick-heating multifunctional electrothermal film of the present invention.
Fig. 2 is a graph showing tensile properties of the graphene thin film, the amyloid lysozyme/reduced graphene oxide composite film in example 1, and the amyloid bovine serum albumin/reduced graphene oxide composite film in example 7.
Fig. 3 is an infrared thermal imaging diagram of the durable quick-heating multifunctional electrothermal film prepared in example 1.
FIG. 4 is a cross-sectional field emission scanning electron microscope photograph of the amyloid lysozyme-like/reduced graphene oxide composite membrane of example 1.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Example 1
Referring to fig. 1, the durable quick-heating multifunctional electrothermal film of the present embodiment is composed of a lower insulating layer 1, an electrothermal sheet 2, a silver paste layer 3, a copper sheet 4 and an upper insulating layer 5.
The electric heating pieces 2 are adhered to the lower insulating layer 1 at intervals, the electric heating pieces 2 are composed of 15 groups of amyloid protein/reduced graphene oxide composite membranes with equal length and width, and the length of each electric heating piece 2 is 40cm, the width of each electric heating piece is 1cm, and the interval of each electric heating piece is 1 cm. The two ends of the electric heating piece 2 are coated with silver paste layers 3 in the vertical direction, and the width of each silver paste layer 3 is 1cm, and the thickness of each silver paste layer is 0.1 cm. The copper sheet 4 is fixed on the silver paste layer 3, so that the electric heating sheets 2 are connected into a closed circuit, the width of the copper sheet 4 is 1cm, the thickness of the copper sheet 4 is 0.2cm, and the copper sheet 4 is used for being connected with a power line. The upper insulating layer 5 is bonded and fixed on the electric heating sheet 2 through hot melt adhesive, so that the electric heating sheet 2 is packaged inside the upper insulating layer 5 and the lower insulating layer 1 and the inside of the electric heating sheet is ensured to be in a vacuum state. The upper insulating layer 2 and the lower insulating layer 4 are both polyvinyl chloride films (PVC).
The preparation method of the durable quick-heating multifunctional electrothermal film comprises the following steps:
1. 3mL of a 3.6mg/mL lysozyme aqueous solution, 3mL of a 3mg/mL graphene oxide dispersion solution and 3mL of a 50mmol/LpH ═ 4.5 tris (2-carboxyethyl) phosphine hydrochloride aqueous solution are stirred and mixed uniformly in a 50mL single-neck flask, then the flask is sealed and placed in a 30 ℃ oven, and a light black suspension is obtained after reaction for 8 hours. During the process, lysozyme has amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 2 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 90 ℃ to further reduce the graphene oxide, stopping the reaction after 9 hours, stirring and cooling to obtain the black suspension.
3. Firstly, a polyvinyl chloride film is installed at the bottom of a mould as a lower insulating layer 1, then the reduced graphene oxide turbid liquid obtained in the step 2 is poured into the mould, and after drying at 30 ℃, an amyloid lysozyme/reduced graphene oxide composite film is formed on the upper surface of the lower insulating layer 1, namely, the electric heating piece 2 is formed. Then taking out the lower insulating layer 1 adhered with the electric heating piece 2, respectively coating a layer of silver paste on the two ends of the electric heating piece 2 in the vertical direction, fixedly installing the copper sheet 4 at the position coated with the silver paste, and drying the silver paste to form a silver paste layer 3. And then a layer of polyvinyl chloride film is bonded and fixed on the electric heating piece 2 through hot melt adhesive to be used as an upper insulating layer 5, so that the electric heating piece 2 is packaged in the upper insulating layer 5 and the lower insulating layer 1, and the interior of the electric heating piece is ensured to be in a vacuum state.
Example 2
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of 2mg/mL lysozyme aqueous solution, 3mL of 1mg/mL graphene oxide dispersion and 3mL of 30mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 4.5 are stirred and mixed uniformly in a 50mL single-neck flask, then the flask is sealed and put into an oven at 25 ℃, and a light black suspension is obtained after reaction for 10 hours. During the process, lysozyme has amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 2 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 80 ℃ to further reduce the graphene oxide, stopping the reaction after 9 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 3
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of 5mg/mL lysozyme aqueous solution, 3mL of 6mg/mL graphene oxide dispersion and 3mL of 70mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 4.5 are stirred and mixed uniformly in a 50mL single-neck flask, then the flask is sealed and put into a 40 ℃ oven to react for 5 hours to obtain light black suspension. During the process, lysozyme has amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 2.5 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 70 ℃ to further reduce the graphene oxide, stopping the reaction after 8 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 4
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of a 3.6mg/mL lysozyme aqueous solution, 3mL of a 4mg/mL graphene oxide dispersion solution and 3mL of a 50mmol/LpH ═ 6.5 tris (2-carboxyethyl) phosphine hydrochloride aqueous solution are stirred and mixed uniformly in a 50mL single-neck flask, then the flask is sealed and placed in a 30 ℃ oven, and a light black suspension is obtained after reaction for 8 hours. During the process, lysozyme has amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 3 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 70 ℃ to further reduce the graphene oxide, stopping the reaction after 9 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 5
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of 2mg/mL lysozyme aqueous solution, 3mL of 1mg/mL graphene oxide dispersion and 3mL of 30mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 6.5 are stirred and mixed uniformly in a 50mL single-neck flask, then the flask is sealed and put into an oven at 25 ℃, and a light black suspension is obtained after reaction for 9 hours. During the process, lysozyme has amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 2 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 80 ℃ to further reduce the graphene oxide, stopping the reaction after 6 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 6
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of 5mg/mL lysozyme aqueous solution, 3mL of 7mg/mL graphene oxide dispersion and 3mL of 70mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 6.5 are stirred and mixed uniformly in a 50mL single-neck flask, then the flask is sealed and put into a 40 ℃ oven to react for 3 hours to obtain light black suspension. During the process, lysozyme has amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 3 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 90 ℃ to further reduce the graphene oxide, stopping the reaction after 8 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 7
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of a 3mg/mL bovine serum albumin aqueous solution, 3mL of a 4mg/mL graphene oxide dispersion, and 3mL of a 50mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 4.0 were stirred and mixed uniformly in a 50mL single-neck flask, and then the flask was sealed and placed in an oven at 30 ℃ to react for 8 hours to obtain a light black suspension. During the process, bovine serum albumin undergoes amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 3 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 70 ℃ to further reduce the graphene oxide, stopping the reaction after 9 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 8
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of a 2mg/mL bovine serum albumin aqueous solution, 3mL of a 1mg/mL graphene oxide dispersion, and 3mL of a 30mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 4.0 were stirred and mixed uniformly in a 50mL single-neck flask, and then the flask was sealed and put into an oven at 25 ℃ to react for 10 hours to obtain a light black suspension. During the process, bovine serum albumin undergoes amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 2 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 80 ℃ to further reduce the graphene oxide, stopping the reaction after 9 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 9
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of a 5mg/mL bovine serum albumin aqueous solution, 3mL of a 6mg/mL graphene oxide dispersion, and 3mL of a 70mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 4.0 were stirred and mixed uniformly in a 50mL single-neck flask, and then the flask was sealed and placed in an oven at 40 ℃ to react for 5 hours to obtain a light black suspension. During the process, bovine serum albumin undergoes amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 3 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 70 ℃ to further reduce the graphene oxide, stopping the reaction after 8 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 10
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of a 3mg/mL bovine serum albumin aqueous solution, 3mL of a 3mg/mL graphene oxide dispersion, and 3mL of a 50mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 5.5 were stirred and mixed uniformly in a 50mL single-neck flask, and then the flask was sealed and put into an oven at 25 ℃ to react for 10 hours to obtain a light black suspension. During the process, bovine serum albumin undergoes amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 2 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 90 ℃ to further reduce the graphene oxide, stopping the reaction after 9 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 11
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of a 2mg/mL bovine serum albumin aqueous solution, 3mL of a 1mg/mL graphene oxide dispersion, and 3mL of a 30mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with a pH of 5.5 were stirred and mixed uniformly in a 50mL single-neck flask, and then the flask was sealed and placed in an oven at 40 ℃ to react for 3 hours to obtain a light black suspension. During the process, bovine serum albumin undergoes amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 2 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 80 ℃ to further reduce the graphene oxide, stopping the reaction after 9 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 12
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of a 5mg/mL bovine serum albumin aqueous solution, 3mL of a 6.5mg/mL graphene oxide dispersion, and 3mL of a 70mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution having a pH of 5.5 were stirred and mixed uniformly in a 50mL single-neck flask, and then the flask was sealed and placed in an oven at 30 ℃ to react for 6 hours to obtain a light black suspension. During the process, bovine serum albumin undergoes amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 3 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 85 ℃ to further reduce the graphene oxide, stopping the reaction after 9 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 13
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of a 3mg/mL bovine serum albumin aqueous solution, 3mL of a 1.5mg/mL graphene oxide dispersion, and 3mL of a 50mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution having a pH of 7.0 were stirred and mixed uniformly in a 50mL single-neck flask, and then the flask was sealed and placed in an oven at 40 ℃ to react for 2 hours to obtain a light black suspension. During the process, bovine serum albumin undergoes amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 2.5 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 75 ℃ to further reduce the graphene oxide, stopping the reaction after 9 hours, stirring and cooling to obtain the black suspension.
The other steps are the same as in example 1.
Example 14
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of a 2mg/mL bovine serum albumin aqueous solution, 3mL of a 5mg/mL graphene oxide dispersion, and 3mL of a 30mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 7.0 were stirred and mixed uniformly in a 50mL single-neck flask, and then the flask was sealed and put into an oven at 25 ℃ to react for 10 hours to obtain a light black suspension. During the process, bovine serum albumin undergoes amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 2 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 90 ℃ to further reduce the graphene oxide, stopping the reaction after 6 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
Example 15
The structure of the durable quick-heating multifunctional electrothermal film of the embodiment is the same as that of the embodiment 1, and the preparation method is as follows:
1. 3mL of a 5mg/mL bovine serum albumin aqueous solution, 3mL of a 7mg/mL graphene oxide dispersion, and 3mL of a 70mmol/L tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 7.0 were stirred and mixed uniformly in a 50mL single-neck flask, and then the flask was sealed and placed in an oven at 30 ℃ to react for 6 hours to obtain a light black suspension. During the process, bovine serum albumin undergoes amyloid-like transformation, and graphene oxide is partially reduced.
2. And (3) adjusting the pH value of the light black suspension obtained in the step (1) to 3 by using 1mol/L hydrochloric acid, simultaneously increasing the reaction temperature to 80 ℃ to further reduce the graphene oxide, stopping the reaction after 7.5 hours, stirring and cooling to obtain the black suspension.
3. This step is the same as step 3 of example 1.
In embodiments 1 to 15, the upper insulating layer and the lower insulating layer may be replaced by any one of a PI film, a PET film, a PP film, a PC film, a PS film, a PE film, a ceramic, a glass, a silicone film, and a mica sheet.
The lysozyme or bovine serum albumin in the above examples may also be replaced by insulin or alpha-lactalbumin.
In order to prove the beneficial effects of the invention, the inventor tests the performances of the electrothermal films prepared in the examples 1 and 7, and the specific tests are as follows:
1. durability test
The tensile properties of the graphene thin film (GO), the amyloid lysozyme-like/reduced graphene oxide composite film (Lyz/rGO) prepared in example 1 and the amyloid bovine serum albumin-like/reduced graphene oxide composite film (BSA/rGO) prepared in example 7 were tested by using a trissen tensile machine. The specimen size was 3cm by 0.5cm, and the test was repeated 3 times for each sample. The samples were taped at both ends (0.5cm) in the length direction and clamped in the grips of the tester. The measuring range of the sensor is 1000N, the set pull-up speed is 5mm/min, and the span is 15-20 mm. All tests were performed at room temperature.
As can be seen from fig. 2, the tensile strength of the graphene film is 40MPa, and the tensile modulus is 1200 MPa; the tensile strength of the amyloid lysozyme/reduced graphene oxide composite membrane is 62MPa, and the tensile modulus is 1540 MPa; the tensile strength of the amyloid bovine serum albumin/reduced graphene oxide composite membrane is 66MPa, and the tensile modulus is 1601 MPa. Therefore, compared with a graphene film, the tensile strength of the amyloid lysozyme/reduced graphene oxide composite film is improved by 55%, and the tensile modulus of the composite film is improved by 28.3%; compared with a graphene film, the amyloid bovine serum albumin/reduced graphene oxide composite film has the advantages that the tensile strength is improved by 65% and the tensile modulus is improved by 33%. Therefore, the amyloid protein/reduced graphene oxide composite membrane has remarkable tensile property, so that the obtained electrothermal membrane has good durability.
2. Rate of temperature rise test
The electric heating film prepared in example 1 was applied with a voltage of 50V at both ends, and the temperature change was measured after 5 min. The results are shown in FIG. 3.
As can be seen from fig. 3, in the same time, the temperature rising speed of the electric heating film based on the amyloid lysozyme/reduced graphene oxide composite film in example 1 is obviously higher than that of the common electric blanket. The amyloid lysozyme/reduced graphene oxide composite membrane has high thermoelectric conversion efficiency, and each group of electrothermal materials are connected in parallel, so that the electrothermal conversion is fast, and the temperature can be rapidly increased. The infrared thermal imaging graph of the heating of the electric heating material shows that the temperature of the electric heating film based on the amyloid lysozyme/reduced graphene oxide composite is 34.7 ℃ within the same 5min time and at the voltage of 50V. Therefore, the heating rate of the electrothermal film based on the amyloid lysozyme/reduced graphene oxide composite film is 6.94 ℃/min. Therefore, the electrothermal film based on the amyloid protein/reduced graphene oxide composite film has the effect of rapid temperature rise.
3. Electrothermal film structure and peel force testing
A structural test of the amyloid lysozyme-like/reduced graphene oxide composite membrane (Lyz/rGO) prepared in example 1 was performed by using a field emission scanning electron microscope, and as can be seen from a field emission scanning electron microscope photograph of a coating cross section in fig. 4, reduced graphene oxide in the amyloid lysozyme-like/reduced graphene oxide composite membrane is in a layered close-packed structure.
The peel force performance of the amyloid lysozyme/reduced graphene oxide-like composite membrane (Lyz/rGO) prepared in example 1 on PVC was tested using the ASTM D4541-09 adhesion test method. The result shows that the peeling force of the amyloid lysozyme-like/reduced graphene oxide composite membrane adhered to the PVC is 0.71 +/-0.12 MPa. Therefore, the amyloid lysozyme/reduced graphene oxide composite membrane has good adhesion on the PVC substrate.
Claims (10)
1. A durable quick-heating multifunctional electrothermal film based on amyloid protein/reduced graphene oxide is characterized in that: the electric heating plate is an amyloid protein/reduced graphene oxide composite membrane, the electric heating plate is adhered to the lower insulating layer at intervals and packaged inside the upper insulating layer and the lower insulating layer, and a heating and conducting circuit is printed on the electric heating plate.
2. The durable rapid-heating multifunctional electrothermal film according to claim 1, wherein the electrothermal film is prepared by the following method:
(1) uniformly mixing a protein aqueous solution, a graphene oxide dispersion solution and a tris (2-carboxyethyl) phosphine hydrochloride aqueous solution with the pH value of 3-10 of 10-100 mmol/L, and reacting the obtained mixed solution at 25-40 ℃ to enable the protein to generate amyloid-like conversion; wherein the protein is one or more of lysozyme, bovine serum albumin, insulin and alpha-lactalbumin;
(2) adjusting the pH value of the suspension reacted in the step (1) to 2-3, and reducing graphene oxide at 70-90 ℃;
(3) firstly, mounting a lower insulating layer at the bottom of a mould, then pouring the reduced graphene oxide turbid liquid obtained in the step (2) into the mould, and drying to form an amyloid protein/reduced graphene oxide composite membrane on the upper surface of the lower insulating layer, namely adhering electric heating sheets on the upper surface of the lower insulating layer at intervals; and taking out the lower insulating layer adhered with the electric heating sheet, printing a heating conductive circuit on the electric heating sheet, and fixing the upper insulating layer on the electric heating sheet through hot melt adhesive or hot-pressing adhesion, so that the electric heating sheet is packaged in the upper insulating layer and the lower insulating layer and the inside of the electric heating sheet is ensured to be in a vacuum state.
3. The durable rapid-heating multifunctional electrothermal film according to claim 2, wherein: in the step (1), the concentration of the protein aqueous solution is 0.5-10 mg/mL, and the graphene oxide dispersion liquid is obtained by dispersing graphene oxide prepared by an improved Hummers method into deionized water by using ultrasonic waves, wherein the concentration of the graphene oxide is 0.1-10 mg/mL.
4. The durable rapid-heating multifunctional electrothermal film according to claim 3, wherein: in the step (1), the concentration of the protein water solution is 2-5 mg/mL, and the concentration of graphene oxide in the graphene oxide dispersion liquid is 1-7 mg/mL.
5. The durable rapid-heating multifunctional electrothermal film according to claim 2, wherein: in the step (1), the pH value of the aqueous solution of tris (2-carboxyethyl) phosphine hydrochloride is 4-7, and the concentration is 30-70 mmol/L.
6. The durable rapid-heating multifunctional electrothermal film according to claim 2, wherein: in the step (1), the obtained mixed solution is reacted for 2-10 hours at the temperature of 25-40 ℃.
7. The durable rapid-heating multifunctional electrothermal film according to claim 2, wherein: in the step (2), the mixed solution reacted in the step (1) is adjusted to pH value of 2-3 by 1mol/L hydrochloric acid, and reacted for 6-9 hours at 70-90 ℃; in the step (3), the temperature for volatilizing the solvent is 30-50 ℃.
8. The durable rapid-heating multifunctional electrothermal film according to claim 1 or 2, wherein: the length of the electric heating pieces is 20-50 cm, the width of the electric heating pieces is 1-5 cm, and the interval between the electric heating pieces is 0.5-2.0 cm.
9. The durable rapid-heating multifunctional electrothermal film according to claim 1, wherein: the upper insulating layer and the lower insulating layer are any one of a PI film, a PET film, a PVC film, a PP film, a PC film, a PS film, a PE film, ceramics, glass, a silica gel film and a mica sheet.
10. The durable rapid-heating multifunctional electrothermal film according to claim 1, wherein: the heating conductive circuit is composed of a silver paste layer and a conductive sheet bonded on the silver paste layer, wherein the width of the silver paste layer is 0.5-2 cm, the thickness of the silver paste layer is 0.1-0.3 cm, the conductive sheet is any one of a copper sheet, a copper foil, an iron strip and a silver strip, the width of the conductive sheet is 0.5-2 cm, and the thickness of the conductive sheet is 0.1-1 cm.
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| CN112695400A (en) * | 2020-12-29 | 2021-04-23 | 陕西师范大学 | Protein fiber capable of being prepared in large scale and application thereof |
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