CN111320758A - Polypropylene-grafted graphene composite material and preparation method thereof - Google Patents
Polypropylene-grafted graphene composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a polypropylene grafted graphene composite material and a preparation method thereof. Wherein, the preparation method comprises the following steps: (1) a step of modifying and reducing graphene oxide with an aniline compound; and (2) reacting the graphene modified and reduced in the step (1) with maleic anhydride grafted polypropylene to obtain the polypropylene grafted graphene. According to the method, the graphene is grafted to the polypropylene long chain by a chemical method, so that the problem of uneven dispersion of the graphene in a matrix is effectively solved, and the flame retardant property, the thermal stability and the mechanical property of the polypropylene material can be improved after the graphene is further blended with the polypropylene.
Description
Technical Field
The invention relates to the field of high polymer material chemistry, in particular to a polypropylene grafted graphene composite material and a preparation method thereof.
Background
Graphene is a sheet crystal with a two-dimensional structure due to the unique sp of carbon atoms2The hybrid track is formed by arranging honeycomb lattices, has excellent heat-conducting property and heat-conducting coefficient up to 5300 W.m-1·K-1And the graphene has extremely low resistivity, excellent mechanical property and good processing property, so that the graphene is very suitable for preparing the functional composite material. However, graphene is composed of extremely stable benzene six-membered rings, has good chemical stability, and is difficult to dissolve in water and most organic solvents due to the inert surface.
The graphene oxide is obtained by oxidizing graphite with concentrated sulfuric acid, potassium permanganate and the like, the surface of the graphene oxide contains a large number of oxygen-containing groups, mainly has derived carboxylic acid groups at the edge, phenolic hydroxyl groups and epoxy groups on the surface, and the oxygen-containing groups can be fully utilized to realize the functionalization of the graphene through chemical reactions such as amidation, esterification, free radical reaction and the like. GO is used as a derivative of graphene, has a layered honeycomb structure of graphene, retains excellent mechanical and thermal properties of graphene, and has good hydrophilicity and repairability due to a large amount of oxygen-containing groups on the surface.
Compared with maleic anhydride grafted graphene of published patent (with the patent number of CN 104371115A), the published patent (with the patent number of CN 106810630A) modifies GO with a metal organic reagent, the published patent (with the patent number of CN105924767A) uses aminoalkyl trialkoxysilane to activate the surface of GO, the GO is modified and reduced by aniline compounds, and the aniline compounds are utilized to activate the GO surfaceThe special para-amino conjugated aromatic amine structure of the compound can react with oxygen-containing groups on the surface of GO and can reduce GO while functionalizing the GO. Due to protonation-N contained in aniline compounds+So that the modified graphene is well dissolved in water and organic solvents. The modified graphene is grafted with MAPP to obtain PP-G-G, and the PP-G-G is provided with a propylene chain segment similar to polypropylene, can be uniformly mixed with a polypropylene matrix, and is expected to improve the heat-conducting property and the mechanical property of the polypropylene material.
Disclosure of Invention
The invention aims to provide a preparation method of a polypropylene grafted graphene composite material. The composite material prepared by the method has excellent heat-conducting property, low resistivity and good dispersibility in water and organic solvents, and can well improve the mechanical and thermal properties of polypropylene.
The invention also aims to provide the polypropylene grafted graphene composite material prepared by the preparation method.
In order to achieve the above object, in one aspect, the present invention provides a method for preparing a polypropylene-grafted graphene composite material, wherein the method comprises the following steps:
(1) a step of modifying and reducing graphene oxide with an aniline compound; and
(2) and (2) reacting the graphene modified and reduced in the step (1) with maleic anhydride grafted polypropylene to obtain the polypropylene grafted graphene composite material.
According to some embodiments of the invention, the aniline compound of step (1) is selected from one or more of 1, 2-phenylenediamine, 1, 3-phenylenediamine and 1, 4-phenylenediamine.
According to some specific embodiments of the present invention, in the step (1), the mass ratio of the graphene oxide to the aniline compound is 1: (2-10).
According to some specific embodiments of the present invention, the modification and reduction of graphene oxide with an aniline compound in the step (1) comprises reacting the aniline compound and graphene oxide at 90-100 ℃ for 2-5 h.
According to some specific embodiments of the present invention, the modification and reduction of graphene oxide with an aniline compound in the step (1) comprises reacting the aniline compound and graphene oxide at 95 ℃ for 3 hours.
According to some embodiments of the present invention, step (1) comprises modifying and reducing graphene oxide with an aniline compound under weakly alkaline conditions using deionized water as a reaction medium.
According to some embodiments of the invention, wherein the weakly alkaline conditions are pH values in the range of 7.0-8.5.
According to some specific embodiments of the present invention, the step (1) includes dissolving graphene oxide in deionized water, performing ultrasonic treatment to peel off the graphene oxide in the solution, adding an aniline compound, adjusting the reaction solution to be weakly alkaline with ammonia water, and reacting to obtain the modified and reduced graphene.
According to some embodiments of the present invention, the step (1) includes filtering the reaction solution after the reaction is finished, dissolving the filtered solid in ethanol, performing ultrasonic treatment to disperse the solid in the ethanol solution, filtering again to wash the unreacted residual aniline compound, and drying the finally filtered solid to obtain the modified and reduced graphene.
According to some embodiments of the present invention, the step (1) is a step of repeating the steps of dissolving in an ethanol solution, ultrasonic dispersing and filtering 1 to 4 times.
According to some specific embodiments of the present invention, the step (2) includes reacting the graphene modified and reduced in the step (1) with maleic anhydride grafted polypropylene using toluene as a reaction medium to obtain the polypropylene grafted graphene composite material.
According to some embodiments of the invention, wherein step (2) is carried out under nitrogen atmosphere.
According to some specific embodiments of the present invention, the step (2) includes dispersing the graphene modified and reduced in the step (1) in toluene, adding maleic anhydride grafted polypropylene, performing a reaction under a nitrogen atmosphere, then removing the toluene, and drying to obtain the polypropylene grafted graphene composite material.
According to some specific embodiments of the present invention, the step (2) comprises dispersing the graphene modified and reduced by the step (1) in toluene using ultrasound.
According to some embodiments of the present invention, wherein the reaction in step (2) is performed at 120-160 ℃ for 1-4 h.
According to some embodiments of the invention, the reaction in step (2) is carried out at 160 ℃ for 2 h.
According to some embodiments of the present invention, the mass of the graphene modified and reduced in the step (1) in the step (2) is 2-10% of the mass of the maleic anhydride grafted polypropylene.
According to some specific embodiments of the invention, the method specifically comprises:
(1) and modifying and reducing graphene oxide by using an aniline compound. The specific method comprises the following steps: and modifying and reducing graphene oxide by using the aniline compound. The specific method comprises the following steps: and dissolving the graphene oxide solid in 360ml of deionized water, and performing ultrasonic treatment to strip the graphene in the solution. Adding aniline compound as modifier and reductant into the mixture. Slowly dropping ammonia water solution dropwise until the mixed solution is alkalescent. The mixture is refluxed and stirred for reaction, the solid obtained after filtration is dissolved in ethanol solution, ultrasonic treatment is carried out to ensure that the obtained solid matter is dispersed in the ethanol solution as much as possible, and then filtration is carried out again. This was repeated several times until the ungrafted residual aniline compound was washed out. And finally, drying the filtered sample in a drying oven at 80 ℃ for 24h to obtain the modified graphene.
(2) And (3) reacting the modified graphene with maleic anhydride grafted polypropylene to obtain the polypropylene grafted graphene. The specific method comprises the following steps: modified graphene with different proportions is suspended in 100ml of toluene and is evenly dispersed by ultrasonic treatment for 10min, then the graphene is transferred into a three-neck flask, and 10g of MAPP (maleic anhydride grafted polypropylene) is added and heated to reflux. After the reaction was complete, the solvent toluene was removed by rotary evaporator at 60 ℃. And finally, drying the product in a vacuum drying oven at 80 ℃ for 12h to prepare the PP-G-G (polypropylene grafted graphene).
Wherein, the reflux stirring temperature in the step (1) is 95 ℃ and the time is 3h, so as to ensure that PPD and GO are fully reacted.
Wherein the heating reflux condition in the step (2) is 160 ℃, nitrogen atmosphere and 2 hours. The modified graphene was grafted to MAPP.
On the other hand, the invention also provides the polypropylene grafted graphene composite material prepared by the preparation method.
In summary, the invention provides a polypropylene grafted graphene composite material and a preparation method thereof. The method of the invention has the following advantages:
the composite material prepared by the method can be further blended with polypropylene to improve the flame retardant property, the thermal stability and the mechanical property of the polypropylene material. According to the method, the graphene is grafted to the polypropylene long chain by a chemical method, so that the problem of uneven dispersion of the graphene in a matrix is effectively solved, and the interface thermal resistance is reduced, so that the composite material has good heat-conducting property.
The polypropylene grafted graphene composite material is blended with polypropylene according to a certain proportion, so that the impact property can be improved by 12%, and the tensile property can be improved by 8%. The peak values of heat release and heat release rate in the combustion process are reduced by 45% and 40%, respectively.
Drawings
FIG. 1 is an infrared spectrum of GO and PPD-G.
Detailed Description
The following detailed description is provided for the purpose of illustrating the embodiments and the advantageous effects thereof, and is not intended to limit the scope of the present disclosure.
Example 1:
0.18g of graphene oxide solid was dissolved in 360ml of deionized water and sonicated for 30min to allow the graphene to exfoliate in solution. 1.8g of PPD was added to the mixture, and an aqueous ammonia solution was slowly dropped dropwise until the mixture became weakly alkaline. The mixture is refluxed and stirred at 95 ℃ for reaction for 3h, the solid obtained after filtration is dissolved in ethanol solution, ultrasonic treatment is carried out for 3min, the obtained solid matter is dispersed in the ethanol solution as much as possible, and then filtration is carried out again. This was repeated 4 times until the ungrafted residual aniline compound was washed out. And finally, drying the filtered graphene sample in a drying oven at 80 ℃ for 24h to obtain the modified graphene.
0.6g of modified graphene is suspended in 100ml of toluene, is subjected to ultrasonic treatment for 10min to be uniformly dispersed, is transferred into a three-neck flask, and is added with 9.4MAPP to be heated and refluxed. After the reaction was complete, the solvent toluene was removed by rotary evaporator at 60 ℃. And finally, drying the product in a vacuum drying oven at 80 ℃ for 12h to prepare the PP-G-G. As can be seen from fig. 1, GO contains a large number of oxygen-containing functional groups, and corresponds to stretching vibration peaks of water molecule (H2O), carbonyl (C ═ O), aromatic skeleton carbon ring (C ═ C), carboxyl (C ═ O), epoxy (C-O), and alkoxy (C-O), respectively, from left to right. Three new absorption peaks, N-H stretching, bending vibration and C-N stretching vibration, were observed in the PPD-G infrared image, indicating successful grafting of G by PDD. The absorption peaks of Carboxyl (COOH) and epoxy (C-O-C) groups in PPD-G are reduced or even disappeared compared to GO, indicating that the group content is reduced or disappeared, i.e. GO is reduced. The obtained PP-G-G and PP were mixed at 180 ℃ in a 1: 5 to obtain the blending material of the polypropylene grafted graphene composite material and the polypropylene, wherein the content of the graphene is 1 wt%. Compared with PP, the tensile property of the blended material is improved by 7 percent. The peak values of heat release and heat release rate during combustion are reduced by 22% and 30%, respectively.
Example 2:
0.18g of graphene oxide solid was dissolved in 360ml of deionized water and sonicated for 30min to allow the graphene to exfoliate in solution. 1.8g of PPD was added to the mixture, and an aqueous ammonia solution was slowly dropped dropwise until the mixture became weakly alkaline. The mixture is refluxed and stirred at 95 ℃ for reaction for 3h, the solid obtained after filtration is dissolved in ethanol solution, ultrasonic treatment is carried out for 3min, the obtained solid matter is dispersed in the ethanol solution as much as possible, and then filtration is carried out again. This was repeated 4 times until the ungrafted residual aniline compound was washed out. And finally, drying the filtered graphene sample in a drying oven at 80 ℃ for 24h to obtain the modified graphene.
Taking 1.2g of modified graphene, suspending the modified graphene in 100ml of toluene, carrying out ultrasonic treatment for 10min to uniformly disperse the modified graphene, transferring the modified graphene into a three-neck flask, and adding 8.8MAPP to heat and reflux. After the reaction was complete, the solvent toluene was removed by rotary evaporator at 60 ℃. And finally, drying the product in a vacuum drying oven at 80 ℃ for 12h to prepare the PP-G-G. PP-G-G and PP were mixed at 180 ℃ in a 1: 5 to obtain the blending material of the polypropylene grafted graphene composite material and the polypropylene, wherein the content of the graphene is 2 wt%. Compared with PP, the impact performance of the blended material can be improved by 12 percent, and the tensile property is improved by 8 percent. The peak values of heat release and heat release rate in the combustion process are reduced by 45% and 40%, respectively.
Example 3:
0.18g of graphene oxide solid was dissolved in 360ml of deionized water and sonicated for 30min to allow the graphene to exfoliate in solution. 1.8g of PPD was added to the mixture, and an aqueous ammonia solution was slowly dropped dropwise until the mixture became weakly alkaline. The mixture is refluxed and stirred at 95 ℃ for reaction for 3h, the solid obtained after filtration is dissolved in ethanol solution, ultrasonic treatment is carried out for 3min, the obtained solid matter is dispersed in the ethanol solution as much as possible, and then filtration is carried out again. This was repeated 4 times until the ungrafted residual aniline compound was washed out. And finally, drying the filtered graphene sample in a drying oven at 80 ℃ for 24h to obtain the modified graphene.
Taking 3g of modified graphene, suspending the modified graphene in 100ml of toluene, carrying out ultrasonic treatment for 10min to uniformly disperse the modified graphene, transferring the modified graphene into a three-neck flask, and adding 7MAPP (methyl acrylamide) to heat and reflux. After the reaction was complete, the solvent toluene was removed by rotary evaporator at 60 ℃. And finally, drying the product in a vacuum drying oven at 80 ℃ for 12h to prepare the PP-G-G.
Mixing the obtained PP-G-G and polypropylene according to the proportion of 1: and 5, melting and blending to obtain the blending material of the polypropylene grafted graphene composite material and the polypropylene, wherein the content of the graphene is 5 wt%. Compared with PP, the peak values of heat release and heat release rate in the combustion process of the blend material are respectively reduced by 18 percent and 28 percent.
Claims (15)
1. A preparation method of a polypropylene grafted graphene composite material, wherein the method comprises the following steps:
(1) a step of modifying and reducing graphene oxide with an aniline compound; and
(2) and (2) reacting the graphene modified and reduced in the step (1) with maleic anhydride grafted polypropylene to obtain the polypropylene grafted graphene composite material.
2. The production method according to claim 1, wherein the aniline compound in the step (1) is one or more selected from the group consisting of 1, 2-phenylenediamine, 1, 3-phenylenediamine and 1, 4-phenylenediamine.
3. The production method according to claim 1, wherein the mass ratio of the graphene oxide to the aniline compound in the step (1) is 1: (2-10).
4. The preparation method according to claim 1, wherein the modification and reduction of graphene oxide with the aniline compound in the step (1) comprises reacting the aniline compound and graphene oxide at 90-100 ℃ for 2-5 h.
5. The preparation method according to claim 1, wherein the step (1) comprises modifying and reducing graphene oxide with an aniline compound under weakly alkaline conditions using deionized water as a reaction medium.
6. The preparation method according to claim 5, wherein the step (1) comprises dissolving graphene oxide in deionized water, performing ultrasonic treatment to peel off the graphene oxide in the solution, adding an aniline compound, and adjusting the reaction solution to be weakly alkaline with ammonia water to react to obtain the modified and reduced graphene.
7. The preparation method according to claim 5, wherein the step (1) comprises, after the reaction is completed, filtering the reaction solution, dissolving the filtered solid in ethanol, performing ultrasonic treatment to disperse the solid in the ethanol solution, then filtering again to wash out unreacted residual aniline compound, and drying the finally filtered solid to obtain the modified and reduced graphene.
8. The preparation method according to claim 7, wherein the step (1) of dissolving in ethanol, ultrasonic dispersing and filtering is repeated 1 to 4 times.
9. The preparation method according to claim 1, wherein the step (2) comprises reacting the graphene modified and reduced in the step (1) with maleic anhydride grafted polypropylene by using toluene as a reaction medium to obtain the polypropylene grafted graphene composite material.
10. The production method according to claim 9, wherein the reaction in step (2) is carried out under a nitrogen atmosphere.
11. The preparation method of claim 9, wherein the step (2) comprises dispersing the graphene modified and reduced in the step (1) in toluene, adding maleic anhydride grafted polypropylene, performing reaction under a nitrogen atmosphere, then removing the toluene, and drying to obtain the polypropylene grafted graphene composite material.
12. The preparation method according to claim 11, wherein the step (2) is to disperse the graphene modified and reduced in the step (1) in toluene under ultrasonic conditions.
13. The method according to any one of claims 1 and 9 to 11, wherein the reaction in step (2) is carried out at 160 ℃ for 1-4 h.
14. The production method according to any one of claims 1 and 9 to 11, wherein the mass of the graphene modified and reduced in step (1) in step (2) is 2 to 10% of the mass of the maleic anhydride-grafted polypropylene.
15. The polypropylene grafted graphene composite material prepared by the preparation method of any one of claims 1 to 14.
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| CN112175286A (en) * | 2020-09-02 | 2021-01-05 | 兰州大学 | Graphene-polypropylene composite master batch and preparation method and application thereof |
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| CN115651307A (en) * | 2022-09-07 | 2023-01-31 | 深圳力越新材料有限公司 | Polypropylene composite material and preparation method thereof |
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Application publication date: 20200623 |