CN114456526A - 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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- CN114456526A CN114456526A CN202210191375.5A CN202210191375A CN114456526A CN 114456526 A CN114456526 A CN 114456526A CN 202210191375 A CN202210191375 A CN 202210191375A CN 114456526 A CN114456526 A CN 114456526A
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- 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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Abstract
The invention discloses a polymer composite material which comprises polyvinyl alcohol and fluorinated graphene nanosheets in a mass ratio of 85-99: 1-15, wherein the fluorinated graphene nanosheets are connected with polyvinyl alcohol molecules through hydrogen bonding and are 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 takes polyvinyl alcohol as a polymer matrix, realizes modification by using fluorinated graphene nanosheets with large doping amount, realizes stable connection of the fluorinated graphene and the polyvinyl alcohol through hydrogen bonding between molecules of the fluorinated graphene and the polyvinyl alcohol, realizes uniform dispersion of the fluorinated graphene in the polyvinyl alcohol, and simultaneously increases crystallinity by taking the fluorinated graphene nanosheets as a center for directional arrangement; the composite material of 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 are high molecular weight (typically up to 10-106) compounds made by repeated covalent bonding of many identical, simple structural units. Polymer composites, also known as polymer matrix composites, add reinforcing substances to the polymer to add desired properties.
Polyvinyl alcohol is a representative of the many widely used polymeric materials, a linear polymer that is non-toxic, odorless, biodegradable, and has good mechanical, chemical, and thermal stability. In recent years, the adhesive has been widely used in the fields of film adhesives, hydrogels, substrates for photovoltaic applications, pharmaceutical and biological applications, and the like. However, polyvinyl alcohol has weak thermal and mechanical properties. Therefore, improving the thermal and mechanical properties of polyvinyl alcohol is a hot spot studied in recent decades. Various literature reports have demonstrated that the thermal properties of polyvinyl alcohol can be significantly improved by adding fillers such as metal oxides, carbon nanomaterials and the like. However, due to the influence of the dispersion degree of various materials in the polyvinyl alcohol, the addition amount of the existing scheme is low (less than 1 wt%), so that the effect of improving the thermal property of the polyvinyl alcohol is not obvious, and new materials and schemes are urgently needed to be searched for so as to realize the remarkable improvement of the thermal property of the polyvinyl alcohol.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide 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 nanosheet, 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 nanosheets in a mass ratio of 85-99: 1-15, wherein the fluorinated graphene nanosheets are connected with polyvinyl alcohol molecules through hydrogen bonding and are uniformly dispersed in the polyvinyl alcohol.
Preferably, the mass ratio of the polyvinyl alcohol to the fluorinated graphene nanosheets is 95-99: 1-5.
According to the preparation method of the polymer composite material, the fluorinated graphene nanosheet 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 fluorinated graphene nanosheet aqueous dispersion is prepared by the following method: dispersing fluorinated graphene in a solvent, and performing ultrasonic and centrifugal treatment to obtain an exfoliated fluorinated graphene nanosheet; 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, a water bath ultrasonic instrument is used for carrying out the ultrasonic treatment, the power of the water bath ultrasonic instrument is 30-100W, and the ultrasonic time is 15-32 h.
More preferably, the rotation speed of the centrifugal treatment is 1000-3000 rpm, and the treatment time is 15-30 min.
Preferably, the fluorinated graphene nanosheet aqueous dispersion and the polyvinyl alcohol aqueous dispersion are uniformly mixed by using an ultrasonic mode.
Preferably, after the polymer composite is vacuum dried into a film shape, it is peeled off from the support to form a polymer composite film.
The polymer composite material is applied to the surface of a power electronic component.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
the polymer composite material provided by the invention takes polyvinyl alcohol as a polymer matrix, realizes modification by using fluorinated graphene nanosheets with large doping amount, realizes stable connection of the fluorinated graphene and the polyvinyl alcohol through 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 increases crystallinity by taking the fluorinated graphene nanosheets as a center for directional arrangement; the composite material is biodegradable and has excellent electrical insulation performance, thermal performance and stability, when the doping amount of the fluorinated graphene nanosheet is about 3wt%, the thermal conductivity of the composite material can reach 2.04W/(m.K), is improved by 7.29 times compared with that of polyvinyl alcohol, the thermal decomposition temperature is improved 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 nanosheets in the polyvinyl alcohol, has simple preparation process and low preparation cost, and is suitable for large-scale production; meanwhile, due to mutual repulsion of fluorine atoms, agglomeration cannot occur even heating in the drying film forming process, so that the doping amount can be greatly increased, and the purpose of greatly improving the thermal performance is achieved.
Drawings
FIG. 1 is a scanning electron micrograph of a polyvinyl alcohol composite film obtained in example 3; wherein, (a) is a surface picture of the composite film, and (b) is a brittle section picture of the composite film;
FIG. 2 is a comparison of the IR spectra of polyvinyl alcohol composites and 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 thermogravimetric plot of a polyvinyl alcohol composite of the present invention;
FIG. 4 is a graph showing the thermal conductivity of the polyvinyl alcohol composite material of the present invention.
Detailed Description
Aiming at the defects in the prior art, the solution idea of the invention is to improve the thermal conductivity, electrical insulation and stability of the polyvinyl alcohol material by using fluorinated graphene nano sheets (FGN for short) with large doping amount.
Carbon nanomaterials generally have high basic thermal conductivity, such as graphene (-5300W/(m · K)), carbon nanotubes (-3500W/(m · K)), and the like, and small amounts of addition can improve various properties of polymers, and the addition amount can also be increased by a complicated method, but a large addition amount inevitably leads to an increase in electrical conductivity, which limits the electrical application thereof. The fluorinated graphene is a very important derivative of graphene, and can be regarded as a single-layer structure of the fluorinated graphene (i.e. fluorine atoms are partially or completely attached to edge carbon atoms of the graphene), and a carbon skeleton of the fluorinated graphene is kept complete, so that the fluorinated graphene inherits excellent performances of the graphene, and has unique performances including low surface energy, large interlayer spacing, wide band gap, good chemical stability, high thermal conductivity and good insulation. According to the literature, the electric conductivity of the fluorinated graphene rapidly decreases with the increase of the fluorination degree, namely, the fluorinated graphene is rapidly changed from a conductor state to an insulator state, meanwhile, the thermal conductivity is in a U-shaped rule, the fluorine content is more than 90%, the thermal conductivity is increased, and the maximum thermal conductivity can reach about 35% of that of the graphene (namely 1800W/(m.K)). In consideration of the insulation property and high thermal conductivity of the fluorinated graphene, the inventor thinks that the immobilization and uniform dispersion of the fluorinated graphene in a polyvinyl alcohol matrix can be realized through the hydrogen bonding action of the edge fluorine atoms of the fluorinated graphene and polyvinyl alcohol, so that the limitation of the addition amount of the modifier is broken through to greatly improve the thermal property of the polyvinyl alcohol and meet the requirements of power electronic components on insulating and high-thermal-property polymer composite materials.
Specifically, the polymer composite material provided by the invention comprises polyvinyl alcohol and fluorinated graphene nanosheets in a mass ratio of 85-99: 1-15, wherein the fluorinated graphene nanosheets are connected with polyvinyl alcohol molecules through hydrogen bonding and are uniformly dispersed in the polyvinyl alcohol.
Preferably, the mass ratio of the polyvinyl alcohol to the fluorinated graphene nanosheets is 95-99: 1-5.
According to the preparation method of the polymer composite material, the fluorinated graphene nanosheet 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 fluorinated graphene nanosheet aqueous dispersion is prepared by the following method: dispersing fluorinated graphene in a solvent, and performing ultrasonic and centrifugal treatment to obtain an exfoliated fluorinated graphene nanosheet; 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, a water bath ultrasonic instrument is used for carrying out the ultrasonic treatment, the power of the water bath ultrasonic instrument is 30-100W, and the ultrasonic time is 15-32 h.
More preferably, the rotation speed of the centrifugal treatment is 1000-3000 rpm, and the treatment time is 15-30 min.
Preferably, the fluorinated graphene nanosheet aqueous dispersion and the polyvinyl alcohol aqueous dispersion are uniformly mixed by using an ultrasonic mode.
Preferably, after the polymer composite is vacuum dried into a film shape, it is peeled off from the support to form a polymer composite film.
For the understanding of the public, the technical solution of the present invention is further described in detail by the following embodiments:
the fluorinated graphene and the polyvinyl alcohol used in the following examples are commercial materials purchased from the market, wherein the size of the fluorinated graphene is 0.2-5 microns, and the fluorine-carbon ratio is 1: 1; m of polyvinyl alcoholv~1.45×105Degree of alcoholysis: 98.0-99.0%.
Example 1
(1) Dispersing fluorinated graphene powder in N-methylpyrrolidone, refluxing for 2 h at 60 ℃, performing ultrasonic treatment on the obtained product for 24 h (50W) on a water bath ultrasonic instrument, and centrifuging the dispersion liquid for 30 min at the rotating speed of 3000 rpm to obtain peeled fluorinated graphene nanosheets; the dispersion was weighed and redispersed in water to prepare a 1 mg/mL aqueous dispersion of fluorinated graphene.
(2) The polyvinyl alcohol particles are added into water and stirred at 80 ℃ until the polyvinyl alcohol particles are completely dissolved, and then 20.0 mg/mL polyvinyl alcohol aqueous dispersion is prepared.
(3) Adding 2.0 mL of fluorinated graphene aqueous dispersion into 9.9 mL of polyvinyl alcohol aqueous dispersion, carrying out ultrasonic treatment for 30 min, stirring for 30 min, injecting into a glass surface dish, and drying in a vacuum drying oven at 60-80 ℃ to form a film, thus obtaining the uniform light brown transparent polyvinyl alcohol composite film.
Example 2
(1) Dispersing fluorinated graphene powder in N-methylpyrrolidone, refluxing for 2 h at 60 ℃, performing ultrasonic treatment on the obtained product for 24 h (50W) on a water bath ultrasonic instrument, and centrifuging the dispersion liquid for 30 min at the rotating speed of 3000 rpm to obtain the peeled fluorinated graphene nanosheet. The dispersion was weighed and redispersed in water to prepare a 1.0 mg/mL aqueous dispersion of fluorinated graphene.
(2) The polyvinyl alcohol particles are added into water and stirred at 80 ℃ until the polyvinyl alcohol particles are completely dissolved, so as to prepare 30.0 mg/mL of polyvinyl alcohol aqueous dispersion.
(3) Adding 6.0 mL of aqueous dispersion of fluorinated graphene into 6.5 mL of aqueous dispersion of polyvinyl alcohol, performing ultrasonic treatment for 30 min, stirring for 30 min, injecting 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 film.
Example 3
(1) Dispersing fluorinated graphene powder in N-methylpyrrolidone, refluxing for 2 h at 60 ℃, performing ultrasonic treatment on the obtained product for 24 h (50W) on a water bath ultrasonic instrument, and centrifuging the obtained mixed dispersion liquid for 30 min at the rotating speed of 3000 rpm to obtain the peeled fluorinated graphene nanosheet. The dispersion was weighed and redispersed in water to prepare a 1.0 mg/mL aqueous dispersion of fluorinated graphene.
(2) The polyvinyl alcohol particles are added into water and stirred at 80 ℃ until the polyvinyl alcohol particles are completely dissolved, and then 40.0 mg/mL polyvinyl alcohol aqueous dispersion is prepared.
(3) And adding 10.0 mL of aqueous dispersion of fluorinated graphene into 4.75 mL of aqueous dispersion of polyvinyl alcohol, performing ultrasonic treatment for 30 min, stirring for 30 min, injecting into a glass surface dish, and drying to form a film, thereby obtaining the uniform light brown transparent polyvinyl alcohol composite film.
Example 4
(1) Dispersing commercial fluorinated graphene powder in N-methylpyrrolidone, refluxing for 2 h at 60 ℃, performing ultrasonic treatment on the obtained product for 24 h (50W) on a water bath ultrasonic instrument, and centrifuging the dispersion liquid for 30 min at the rotating speed of 3000 rpm to obtain the peeled fluorinated graphene nanosheet. The dispersion was weighed and redispersed in water to prepare a 1.0 mg/mL aqueous dispersion of fluorinated graphene.
(2) The polyvinyl alcohol particles are added into water and stirred at 80 ℃ until the polyvinyl alcohol particles are completely dissolved, and 50.0 mg/mL of polyvinyl alcohol aqueous dispersion is prepared.
(3) And adding 20.0 mL of fluorinated graphene aqueous dispersion into 3.6mL of polyvinyl alcohol aqueous dispersion, performing ultrasonic treatment for 30 min, stirring for 30 min, injecting into a glass surface dish, and drying to form a film, thereby obtaining the uniform light brown transparent polyvinyl alcohol composite film.
Example 5
(1) Dispersing fluorinated graphene powder in N-methylpyrrolidone, refluxing for 2 h at 60 ℃, performing ultrasonic treatment on the obtained product for 24 h (50W) on a water bath ultrasonic instrument, and centrifuging the obtained mixed dispersion liquid for 30 min at the rotating speed of 3000 rpm to obtain the peeled fluorinated graphene nanosheet. The dispersion was weighed and redispersed in water to prepare a 1.0 mg/mL aqueous dispersion of fluorinated graphene.
(2) The polyvinyl alcohol particles are added into water and stirred at 80 ℃ until the polyvinyl alcohol particles are completely dissolved, and 50.0 mg/mL of polyvinyl alcohol aqueous dispersion is prepared.
(3) And adding 30.0 mL of aqueous dispersion of fluorinated graphene into 3.4 mL of aqueous dispersion of polyvinyl alcohol, performing ultrasonic treatment for 30 min, stirring for 30 min, injecting into a glass surface dish, and drying to form a film, thereby obtaining 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 nanosheets in the polyvinyl alcohol composite material film prepared in the embodiments 1-5 can be observed to be uniformly distributed in polyvinyl alcohol through a scanning electron microscope, and the agglomeration phenomenon is not generated. Fig. 1 is a scanning electron microscope image of a polyvinyl alcohol composite film with a fluorinated graphene content of 3wt%, wherein (a) is a surface view of the composite film, and (b) is a brittle cross-sectional view of the composite film.
The infrared spectrogram and infrared normalized spectrogram of the polyvinyl alcohol composite membrane are shown in figure 2, which shows that: compared with a polyvinyl alcohol film, the polyvinyl alcohol composite film prepared by the invention is 3300 cm-1The weak red shift occurs on the left and right, which indicates the existence of hydrogen bonds between the fluorinated graphene and the polyvinyl alcohol molecules.
The thermogravimetric graph of the polyvinyl alcohol composite membrane is shown in fig. 3, and shows that: with the increase of the addition amount of the fluorinated graphene nanosheets, the thermal decomposition temperature tends to increase first and then decrease, wherein when the addition amount of the fluorinated graphene nanosheets is 3wt%, the thermal decomposition temperature is increased by 30 ℃ compared with that of the polyvinyl alcohol film.
The thermal conductivity graph of the polyvinyl alcohol composite film is shown in fig. 4, which shows that: with the increase of the addition amount of the fluorinated graphene nanosheets, the thermal conductivity tends to increase first and then decrease, wherein when the addition amount of the fluorinated graphene nanosheets 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 conclusion, 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 insulating and high-thermal-performance polymer composite materials and has extremely high application value.
Claims (10)
1. The polymer composite material is characterized by comprising polyvinyl alcohol and fluorinated graphene nanosheets in a mass ratio of 85-99: 1-15, wherein the fluorinated graphene nanosheets are connected with polyvinyl alcohol molecules through hydrogen bonding and are uniformly dispersed in the polyvinyl alcohol.
2. The polymer composite material according to claim 1, wherein the mass ratio of the polyvinyl alcohol to the fluorinated graphene nanoplatelets is 95-99: 1-5.
3. The preparation method of the polymer composite material according to claim 1 or 2, wherein the fluorinated graphene nanoplatelet aqueous dispersion with a concentration of 0.5-1.0 mg/mL and the polyvinyl alcohol aqueous dispersion with a concentration of 20.0-50.0 mg/mL are uniformly mixed according to the mass ratio, and then vacuum-dried at a temperature of 60-80 ℃.
4. The method for preparing the polymer composite material according to claim 3, wherein the aqueous dispersion of fluorinated graphene nanoplatelets is prepared by: dispersing fluorinated graphene in a solvent, and performing ultrasonic and centrifugal treatment to obtain an exfoliated fluorinated graphene nanosheet; the fluorinated graphene nanoplatelets are then dispersed in water.
5. The method for preparing the polymer composite material according to claim 4, wherein the solvent is one or more of isopropanol, N-methylpyrrolidone and N, N-dimethylformamide dichloromethane.
6. The preparation method of the polymer composite material as claimed in claim 4, wherein the ultrasonic treatment is carried out 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.
7. The method for preparing the polymer composite material according to claim 4, wherein the rotation speed of the centrifugal treatment is 1000-3000 rpm, and the treatment time is 15-30 min.
8. The method for preparing the polymer composite material according to claim 3, 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.
9. The method of claim 3, wherein the polymer composite is vacuum-dried into a film form and then peeled from the support to form the polymer composite film.
10. The use of the polymer composite material as claimed in claim 1 or 2 in the surface of power electronic components.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115849357A (en) * | 2022-12-09 | 2023-03-28 | 陕西科技大学 | Fluorinated graphene, preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040072075A1 (en) * | 2002-10-15 | 2004-04-15 | Quallion Llc | Fluorinated carbon active material |
| CN109912912A (en) * | 2019-03-06 | 2019-06-21 | 东华大学 | A kind of flexible, electrical isolation fluorinated graphene heat conduction composite membrane and its preparation and application |
| US20200168356A1 (en) * | 2018-11-27 | 2020-05-28 | Nanotek Instruments, Inc. | Conducting polymer composite containing ultra-low loading of graphene |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040072075A1 (en) * | 2002-10-15 | 2004-04-15 | Quallion Llc | Fluorinated carbon active material |
| US20200168356A1 (en) * | 2018-11-27 | 2020-05-28 | Nanotek Instruments, Inc. | Conducting polymer composite containing ultra-low loading of graphene |
| CN109912912A (en) * | 2019-03-06 | 2019-06-21 | 东华大学 | A kind of flexible, electrical isolation fluorinated graphene heat conduction composite membrane and its preparation and application |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115849357A (en) * | 2022-12-09 | 2023-03-28 | 陕西科技大学 | Fluorinated graphene, preparation method and application |
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