CN114456526B - Polymer composite material and preparation method and application thereof - Google Patents
Polymer composite material and preparation method and application thereof Download PDFInfo
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- CN114456526B CN114456526B CN202210191375.5A CN202210191375A CN114456526B CN 114456526 B CN114456526 B CN 114456526B CN 202210191375 A CN202210191375 A CN 202210191375A CN 114456526 B CN114456526 B CN 114456526B
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08J2329/00—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 at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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 polymer composite material, which comprises polyvinyl alcohol and fluorinated graphene nano-sheets with the mass ratio of 85-99:1-15, wherein the fluorinated graphene nano-sheets are connected with polyvinyl alcohol molecules through hydrogen bonding and uniformly dispersed in the polyvinyl alcohol. The invention also discloses a preparation method and application of the polymer composite material. Compared with the prior art, the polymer composite material provided by the invention uses the polyvinyl alcohol as a polymer matrix, realizes modification by using the fluorinated graphene nano-sheets with large doping amount, realizes stable connection of the fluorinated graphene and the polyvinyl alcohol through the hydrogen bond action between molecules of the fluorinated graphene and the polyvinyl alcohol, realizes uniform dispersion of the fluorinated graphene in the polyvinyl alcohol, and simultaneously uses the fluorinated graphene nano-sheets as the center for directional arrangement of the polyvinyl alcohol, thereby increasing the crystallinity; the composite material provided by the invention is biodegradable and has excellent electrical insulation performance, thermal performance and stability.
Description
Technical Field
The invention relates to a polymer composite material and a preparation method thereof.
Background
Polymeric materials refer to high molecular weight (typically up to 10 to 106) compounds formed from a plurality of identical, simple structural units repeatedly joined by covalent bonds. And polymer composites (polymer composites), also known as polymer matrix composites, are added to the polymer with reinforcing substances to increase the desired properties.
Polyvinyl alcohol is a representative of the wide variety of polymeric materials that are widely used, and is a linear polymer that is non-toxic, odorless, biodegradable, and has good mechanical, chemical, and thermal stability. In recent years, the polymer has been widely applied to application matrixes such as film adhesives, hydrogels, photoelectricity and the like, and fields such as pharmacy, biology and the like. However, the thermal and mechanical properties of polyvinyl alcohol are very weak. Thus, improving the thermal and mechanical properties of polyvinyl alcohol is a hot spot of research in recent decades. Various literature reports have demonstrated that the addition of fillers such as metal oxides, carbon nanomaterials, etc. can significantly improve the thermal properties of polyvinyl alcohol. However, due to the influence of the dispersity of various materials in the polyvinyl alcohol, the addition amount of the existing scheme is low (lower than 1 wt%), so that the improvement effect on the thermal performance of the polyvinyl alcohol is not obvious, and new materials and schemes are required to be searched for to realize the remarkable improvement on the thermal performance of the polyvinyl alcohol.
Disclosure of Invention
The invention aims to solve the technical problems of overcoming the defects of the prior art and providing a biodegradable polymer composite material with excellent electrical insulation performance and thermal performance, which takes polyvinyl alcohol as a polymer matrix, realizes modification by a large doping amount of fluorinated graphene nano-sheets, and has good material stability and extremely low manufacturing cost.
The technical scheme provided by the invention is as follows:
a polymer composite material comprises polyvinyl alcohol and fluorinated graphene nano-sheets with the mass ratio of 85-99:1-15, wherein the fluorinated graphene nano-sheets are connected with polyvinyl alcohol molecules through hydrogen bonding and uniformly dispersed in the polyvinyl alcohol.
Preferably, the mass ratio of the polyvinyl alcohol to the fluorinated graphene nano-sheets is 95-99:1-5.
According to the preparation method of the polymer composite material, the fluorinated graphene nano-sheet aqueous dispersion with the concentration of 0.5-1.0 mg/mL and the polyvinyl alcohol aqueous dispersion with the concentration of 20.0-50.0 mg/mL are uniformly mixed according to the mass ratio, and then the mixture is dried in vacuum at the temperature of 60-80 ℃.
Preferably, the aqueous dispersion of the fluorinated graphene nano-sheets is prepared by the following method: dispersing the fluorinated graphene in a solvent, and carrying out ultrasonic and centrifugal treatment to obtain exfoliated fluorinated graphene nano sheets; the fluorinated graphene nanoplatelets are then dispersed in water.
Further preferably, the solvent is one or more of isopropanol, N-methyl pyrrolidone and N, N-dimethylformamide dichloromethane.
Further preferably, the ultrasonic treatment is performed by using a water bath ultrasonic instrument, the power of the water bath ultrasonic instrument is 30-100W, and the ultrasonic time is 15-32 h.
Further preferably, the rotational speed of the centrifugal treatment is 1000 to 3000 rpm, and the treatment time is 15 to 30 minutes.
Preferably, the aqueous dispersion of the fluorinated graphene nano-sheets is uniformly mixed with the aqueous dispersion of the polyvinyl alcohol by using an ultrasonic mode.
Preferably, the polymer composite is vacuum dried into a film, and then peeled from the support to form a polymer composite film.
The application of the polymer composite material to the surface of a power electronic component.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
according to the polymer composite material provided by the invention, the polyvinyl alcohol is used as a polymer matrix, the modification is realized by using the fluorinated graphene nano-sheets with large doping amount, the stable connection of the fluorinated graphene and the polyvinyl alcohol is realized through the hydrogen bond action between the fluorinated graphene and the polyvinyl alcohol molecules, the uniform dispersion of the fluorinated graphene in the polyvinyl alcohol is realized, and meanwhile, the polyvinyl alcohol is directionally arranged by taking the fluorinated graphene nano-sheets as the center, so that the crystallinity is increased; the composite material provided by the invention is biodegradable, has excellent electrical insulation performance, thermal performance and stability, and when the doping amount of the fluorinated graphene nanosheets is about 3wt%, the thermal conductivity of the composite material can reach 2.04W/(m.K), is 7.29 times higher than that of polyvinyl alcohol, the thermal decomposition temperature is increased by 30 ℃, and the composite material can be widely applied to application occasions with higher requirements on thermal conductivity and insulativity, such as the surfaces of power electronic components, and can greatly improve the upper limit of the service temperature of the components through good heat dissipation while ensuring electrical insulation.
The preparation method adopts a solution casting method to realize the uniform dispersion of the fluorinated graphene nano-sheets in the polyvinyl alcohol, has simple preparation process and low preparation cost, and is suitable for large-scale production; meanwhile, due to the mutual repulsive interaction of fluorine atoms, agglomeration can not occur even if heating is carried out in the drying film forming process, so that the doping amount can be greatly increased, and the aim of greatly improving the thermal performance is fulfilled.
Drawings
FIG. 1 is a scanning electron microscope image of a polyvinyl alcohol composite film obtained in example 3; wherein, (a) is a surface graph of the composite film, and (b) is a brittle fracture surface graph of the composite film;
FIG. 2 is an infrared spectrum comparison of a polyvinyl alcohol composite with polyvinyl alcohol at 5wt% and 15 wt% fluorinated graphene addition; wherein, (a) is an infrared spectrogram, and (b) is an infrared normalized spectrogram;
FIG. 3 is a thermal weight graph of a polyvinyl alcohol composite of the invention;
FIG. 4 is a graph showing the thermal conductance of the polyvinyl alcohol composite material of the invention.
Detailed Description
Aiming at the defects of the prior art, the solution idea of the invention is to utilize the fluorinated graphene nano-sheet (FGN for short) with large doping amount to realize the improvement of the heat conductivity, the electrical insulation and the stability of the polyvinyl alcohol material.
Carbon nanomaterials generally have high basic thermal conductivity, such as graphene (-5300W/(m.k)), carbon nanotubes (-3500W/(m.k)), and the like, and small addition can improve various properties of the polymer, and can increase the addition amount by a complicated method, but the large addition amount inevitably leads to the increase of electrical conductivity, which limits the application of the carbon nanomaterials in electrical aspects. Fluorinated graphene is a very important derivative of graphene, and can be regarded as a single-layer structure of the fluorinated graphene (namely fluorine atoms are partially or completely attached to carbon atoms at the edge of the graphene), and the carbon skeleton of the fluorinated graphene is kept intact, so that the fluorinated graphene not only inherits the excellent performance of the graphene, but also has unique performances, including low surface energy, large interlayer spacing, wide band gap, good chemical stability, high thermal conductivity and good insulativity. According to the literature, the fluorinated graphene is reported to be improved along with the degree of fluorination, the electrical conductivity can be rapidly reduced, namely, the conductive state is rapidly changed into the insulator state, meanwhile, the thermal conductivity is in a U-shaped rule, the fluorine content is greater than 90%, the thermal conductivity is increased along with the increase, and the maximum thermal conductivity of the fluorinated graphene can reach about 35% (namely-1800W/(m.K)). Considering the insulativity and high thermal conductivity of the fluorinated graphene, the inventor considers that the immobilization and uniform dispersion of the fluorinated graphene in the polyvinyl alcohol matrix can be realized through the hydrogen bond action of fluorine atoms at the edge of the fluorinated graphene and the polyvinyl alcohol, so that the limit of the addition amount of the modifier is broken through to greatly improve the thermal performance of the polyvinyl alcohol, and the requirements of power electronic components on the insulating and high thermal performance polymer composite material are met.
Specifically, the polymer composite material provided by the invention comprises polyvinyl alcohol and fluorinated graphene nano-sheets with the mass ratio of 85-99:1-15, wherein the fluorinated graphene nano-sheets are connected with polyvinyl alcohol molecules through hydrogen bonding and uniformly dispersed in the polyvinyl alcohol.
Preferably, the mass ratio of the polyvinyl alcohol to the fluorinated graphene nano-sheets is 95-99:1-5.
According to the preparation method of the polymer composite material, the fluorinated graphene nano-sheet aqueous dispersion with the concentration of 0.5-1.0 mg/mL and the polyvinyl alcohol aqueous dispersion with the concentration of 20.0-50.0 mg/mL are uniformly mixed according to the mass ratio, and then the mixture is dried in vacuum at the temperature of 60-80 ℃.
Preferably, the aqueous dispersion of the fluorinated graphene nano-sheets is prepared by the following method: dispersing the fluorinated graphene in a solvent, and carrying out ultrasonic and centrifugal treatment to obtain exfoliated fluorinated graphene nano sheets; the fluorinated graphene nanoplatelets are then dispersed in water.
Further preferably, the solvent is one or more of isopropanol, N-methyl pyrrolidone and N, N-dimethylformamide dichloromethane.
Further preferably, the ultrasonic treatment is performed by using a water bath ultrasonic instrument, the power of the water bath ultrasonic instrument is 30-100W, and the ultrasonic time is 15-32 h.
Further preferably, the rotational speed of the centrifugal treatment is 1000 to 3000 rpm, and the treatment time is 15 to 30 minutes.
Preferably, the aqueous dispersion of the fluorinated graphene nano-sheets is uniformly mixed with the aqueous dispersion of the polyvinyl alcohol by using an ultrasonic mode.
Preferably, the polymer composite is vacuum dried into a film, and then peeled from the support to form a polymer composite film.
For the convenience of public understanding, the following further details of the technical solution of the present invention are provided by several examples:
the fluorinated graphene and polyvinyl alcohol used in the following examples are commercial materials purchased from the market, wherein the fluorinated graphene has a size of 0.2-5 microns and a fluorocarbon ratio of 1:1; m of polyvinyl alcohol v ~1.45×10 5 Degree of alcoholysis: 98.0 to 99.0 percent.
Example 1
(1) Dispersing the fluorinated graphene powder in N-methylpyrrolidone, refluxing for 2 h at 60 ℃, performing ultrasonic treatment on the mixture on a water bath ultrasonic instrument for 24 h (50W), and centrifuging the dispersion liquid at a rotating speed of 3000 rpm for 30 min to obtain exfoliated fluorinated graphene nano sheets; the dispersion was filtered, weighed and redispersed in water to prepare an aqueous dispersion of fluorinated graphene at 1 mg/mL.
(2) Polyvinyl alcohol particles were added to water and stirred at 80℃until all dissolved to prepare a polyvinyl alcohol aqueous dispersion of 20.0. 20.0 mg/mL.
(3) Adding 2.0. 2.0 mL graphene fluoride aqueous dispersion into 9.9 mL polyvinyl alcohol aqueous dispersion, carrying out ultrasonic treatment for 30 min, stirring for 30 min, pouring into a glass surface dish, and drying in a vacuum drying oven at 60-80 ℃ to form a film, thereby obtaining the uniform light brown transparent polyvinyl alcohol composite material film.
Example 2
(1) The fluorinated graphene powder is dispersed in N-methyl pyrrolidone, reflux is carried out at 60 ℃ for 2 h, ultrasonic is carried out on the mixture on a water bath ultrasonic instrument for 24 h (50W), and then the dispersion is centrifuged at 3000 rpm for 30 min, so that the exfoliated fluorinated graphene nano-sheets are obtained. The dispersion was filtered, weighed and redispersed in water to prepare an aqueous dispersion of fluorinated graphene at 1.0. 1.0 mg/mL.
(2) Polyvinyl alcohol particles were added to water and stirred at 80℃until all dissolved to prepare a 30.0. 30.0 mg/mL polyvinyl alcohol aqueous dispersion.
(3) Adding the aqueous dispersion of 6.0 mL fluorinated graphene into the aqueous dispersion of 6.5 mL polyvinyl alcohol, carrying out ultrasonic treatment for 30 min, stirring for 30 min, pouring into a glass surface dish, and drying in a vacuum drying oven at 60-80 ℃ to form a film, thereby obtaining the uniform light brown transparent polyvinyl alcohol composite material film.
Example 3
(1) The fluorinated graphene powder is dispersed in N-methyl pyrrolidone, reflux is carried out at 60 ℃ for 2 h, ultrasonic is carried out on the mixture on a water bath ultrasonic instrument for 24 h (50W), and then the mixed dispersion liquid is centrifuged at 3000 rpm for 30 min, so that the exfoliated fluorinated graphene nano-sheets are obtained. The dispersion was filtered, weighed and redispersed in water to prepare an aqueous dispersion of fluorinated graphene at 1.0. 1.0 mg/mL.
(2) Polyvinyl alcohol particles were added to water and stirred at 80℃until all dissolved to prepare a 40.0. 40.0 mg/mL polyvinyl alcohol aqueous dispersion.
(3) Adding 10.0. 10.0 mL aqueous dispersion of the fluorinated graphene into 4.75-mL aqueous dispersion of polyvinyl alcohol, carrying out ultrasonic treatment for 30 min, stirring for 30 min, pouring into a glass surface dish, and drying to form a film to obtain the uniform light brown transparent polyvinyl alcohol composite film.
Example 4
(1) Commercial fluorinated graphene powder is dispersed in N-methyl pyrrolidone, reflux is carried out at 60 ℃ for 2 h, ultrasonic treatment is carried out on the obtained product on a water bath ultrasonic instrument for 24 h (50W), and then the dispersion liquid is centrifuged at 3000 rpm for 30 min, so that the exfoliated fluorinated graphene nano-sheets are obtained. The dispersion was filtered, weighed and redispersed in water to prepare an aqueous dispersion of fluorinated graphene at 1.0. 1.0 mg/mL.
(2) Polyvinyl alcohol particles were added to water and stirred at 80℃until all dissolved to prepare 50.0. 50.0 mg/mL of an aqueous polyvinyl alcohol dispersion.
(3) Adding 20.0. 20.0 mL graphene fluoride aqueous dispersion into 3.6mL polyvinyl alcohol aqueous dispersion, carrying out ultrasonic treatment for 30 min, stirring for 30 min, pouring into a glass surface dish, and drying to form a film to obtain the uniform light brown transparent polyvinyl alcohol composite film.
Example 5
(1) Dispersing the fluorinated graphene powder in N-methylpyrrolidone, refluxing for 2 h at 60 ℃, performing ultrasonic treatment on the mixture on a water bath ultrasonic instrument for 24 h (50W), and centrifuging the mixed dispersion liquid at a rotating speed of 3000 rpm for 30 min to obtain the exfoliated fluorinated graphene nano-sheets. The dispersion was filtered, weighed and redispersed in water to prepare an aqueous dispersion of fluorinated graphene at 1.0. 1.0 mg/mL.
(2) Polyvinyl alcohol particles were added to water and stirred at 80℃until all dissolved to prepare 50.0. 50.0 mg/mL of an aqueous polyvinyl alcohol dispersion.
(3) Adding 30.0 mL of the aqueous dispersion of the fluorinated graphene into 3.4 mL of the aqueous dispersion of the polyvinyl alcohol, carrying out ultrasonic treatment for 30 min, stirring for 30 min, pouring into a glass surface dish, and drying to form a film to obtain the uniform light brown transparent polyvinyl alcohol composite film.
In order to verify the technical effect of the technical scheme of the invention, the polyvinyl alcohol composite material prepared by the above embodiments is tested and compared with polyvinyl alcohol:
the fluorinated graphene nano sheets in the polyvinyl alcohol composite material films prepared in the examples 1 to 5 can be observed to be uniformly distributed in the polyvinyl alcohol through a scanning electron microscope, and no agglomeration phenomenon occurs. Fig. 1 shows a scanning electron microscope image of a polyvinyl alcohol composite film with a fluorinated graphene content of 3wt%, wherein (a) is a surface image of the composite film, and (b) is a brittle fracture surface image of the composite film.
The infrared spectrogram and the infrared normalized spectrogram of the polyvinyl alcohol composite film are shown in fig. 2, which shows that: compared with the polyvinyl alcohol film, the polyvinyl alcohol composite film prepared by the invention has the advantages that the polyvinyl alcohol composite film is 3300 and 3300 cm -1 A weak red shift occurs from side to side, indicating the presence of hydrogen bonds between the fluorinated graphene and the polyvinyl alcohol molecules.
The thermogravimetric graph of the polyvinyl alcohol composite film is shown in fig. 3, which shows that: with the increase of the addition amount of the fluorinated graphene nano-sheets, the thermal decomposition temperature shows a trend of increasing and then decreasing, wherein when the addition amount of the fluorinated graphene nano-sheets is 3wt%, the thermal decomposition temperature is increased by 30 ℃ compared with that of the polyvinyl alcohol film.
The thermal conductivity profile of the polyvinyl alcohol composite film is shown in fig. 4, indicating that: with the increase of the addition amount of the fluorinated graphene nano-sheets, the thermal conductivity tends to be increased and then reduced, wherein when the addition amount of the fluorinated graphene nano-sheets is 1 wt% -5 wt%, the thermal conductivity of the polyvinyl alcohol composite film is far higher than that of the polyvinyl alcohol film, and particularly when the addition amount is 3wt%, the thermal conductivity of the polyvinyl alcohol composite film is 7.29 times that of the polyvinyl alcohol film.
In summary, the invention provides the environment-friendly polyvinyl alcohol composite material with high thermal conductivity and thermal stability, which can meet the requirements of power electronic components on the insulating and high thermal performance polymer composite material, and has extremely high application value.
Claims (7)
1. The polymer composite material is characterized by comprising polyvinyl alcohol and fluorinated graphene nano-sheets in a mass ratio of 85-99:1-15, wherein the fluorinated graphene nano-sheets are connected with polyvinyl alcohol molecules through hydrogen bonding and uniformly dispersed in the polyvinyl alcohol; the preparation method of the polymer composite material comprises the following steps: uniformly mixing 0.5-1.0 mg/mL of fluorinated graphene nano-sheet aqueous dispersion with 20.0-50.0 mg/mL of polyvinyl alcohol aqueous dispersion according to the mass ratio, and then vacuum drying at 60-80 ℃; the mass ratio of the polyvinyl alcohol to the fluorinated graphene nano-sheets is 95-99:1-5; the fluorinated graphene nano sheet aqueous dispersion is prepared by the following method: and dispersing the fluorinated graphene in a solvent, performing ultrasonic and centrifugal treatment to obtain exfoliated fluorinated graphene nano-sheets, and dispersing the fluorinated graphene nano-sheets in water.
2. A method for preparing a polymer composite material according to claim 1, wherein the solvent is one or more of isopropanol, N-methylpyrrolidone, and N, N-dimethylformamide dichloromethane.
3. The method of producing a polymer composite according to claim 2, wherein the ultrasonic treatment is performed using a water bath ultrasonic apparatus having a power of 30 to 100W and an ultrasonic time of 15 to 32 h.
4. The method for preparing a polymer composite according to claim 2, wherein the rotational speed of the centrifugal treatment is 1000 to 3000 rpm and the treatment time is 15 to 30 minutes.
5. The method for preparing a polymer composite material according to claim 2, wherein the aqueous dispersion of the fluorinated graphene nanoplatelets and the aqueous dispersion of the polyvinyl alcohol are uniformly mixed by using an ultrasonic method.
6. The method of producing a polymer composite according to claim 2, wherein the polymer composite is vacuum-dried into a film, and then peeled off from the support to form a polymer composite film.
7. Use of the polymer composite according to claim 1 on the surface of a power electronic component.
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