CN104529382B - A kind of preparation method of the graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare - Google Patents
A kind of preparation method of the graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare Download PDFInfo
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Abstract
The preparation method of a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare, it relates to a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare and preparation method thereof.The present invention is to solve that existing aluminosilicate polymer mechanical performance is low, poor toughness and the problem that is directly added into graphene powder reunion bad dispersibility.Utilizing graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing is be prepared from by graphene oxide suspension, alkali-activated carbonatite solution and aluminosilicate powder body；Method: one, the preparation of graphene oxide suspension；Two, the preparation of alkali-activated carbonatite solution；Three, the preparation of graphene oxide/alkali-activated carbonatite mixed liquor；Four, the preparation of graphene/aluminum silicate polymer slurry；Five, curing molding.The present invention is used for preparing graphene/aluminum silicate polymer composite.This preparation method is easy, and cost is low, can prepare on a large scale, widely applicable.
Description
Technical field
The present invention relates to a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare and preparation method thereof.
Background technology
Aluminosilicate polymer material environmental protection, preparation temperature is low, technique is simple, energy consumption is low, and have that density is low, cost is low, the advantage such as high temperature resistant, heat-resisting and fire resistance is good, be widely used in building and aviation field.But, to compare with traditional cement, the factors such as itself intrinsic fragility, poor toughness, mechanical strength are low seriously limit its range of application.Preparing aluminosilicate polymer based composites at present and be concentrated mainly on granule and two kinds of forms of fiber reinforcement, this seminar is all achieved with related ends.But, in existing fibre reinforcement, the simple mechanical bond of fiber and basal body interface does not change it from nanoscale and combines essence, and after high-temperature process, fiber again limit its whole structure and application conditions with the mismatch of basal body interface thermal coefficient of expansion；Particulates reinforcements in conjunction with in good condition, however it is necessary that Granular composite is uniform with matrix.
Graphene is a kind of monoatomic layer two dimensional crystal being connected with sp2 hydridization by carbon atom and being formed, and has mechanics and the electric property of excellence, is widely used in as nanometer reinforcement in pottery and polymer matrix composites.Compared to Graphene, surface of graphene oxide contains substantial amounts of oxy radical and shows stronger hydrophilic and easily disperse in an aqueous medium, there is good wettability and surface activity, Graphene can be reduced in specific environment, there is the series of advantages such as process stabilizing, easily processing, cost are low.Graphene oxide is applied in the composite, in improving the combination properties such as the calorifics of material, electricity, mechanics, has played very important effect.Experience have shown that at present, Graphene is directly made an addition to the shortcoming that there is Graphene reunion, bad dispersibility in the process of aluminosilicate polymer；And it is less that graphene oxide makes an addition to the research report in aluminosilicate polymer.
Summary of the invention
The present invention is to solve that existing aluminosilicate polymer mechanical performance is low, poor toughness and be directly added into the problem of graphene powder reunion bad dispersibility, and provide a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare and preparation method thereof.
A kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare of the present invention is prepared from by graphene oxide suspension, alkali-activated carbonatite solution and aluminosilicate powder body；
Described graphene oxide suspension is mixed by graphene oxide powder and deionized water；The quality of described graphene oxide powder and the volume ratio of deionized water are (1～20) mg:1mL；
Described alkali-activated carbonatite solution is mixed by the Ludox that potassium hydroxide and mass concentration are 25%～45%；In described potassium hydroxide potassium element and mass concentration be 25%～45% Ludox in the mol ratio of element silicon be 1:(0.5～1.5)；
Graphene oxide powder and the mass ratio of aluminosilicate powder body in described graphene oxide suspension are (0.01～0.15): 100；
In described aluminosilicate powder body, element silicon is 1:1 with the mol ratio of aluminium element；
In the described graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare, element silicon is (1～4) with the mol ratio of aluminium element: 1.
The preparation method of a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare of the present invention is to sequentially include the following steps:
One, the preparation of graphene oxide suspension: graphene oxide powder ultrasonic is scattered in deionized water, supersound process 2h～6h, obtain brown color graphene oxide suspension；The quality of described graphene oxide powder and the volume ratio of deionized water are (1～20) mg:1mL；
Two, the preparation of alkali-activated carbonatite solution: potassium hydroxide is joined in the Ludox that mass concentration is 25%～45%, magnetic agitation mixing 20h～80h, obtain alkali-activated carbonatite solution；In described potassium hydroxide potassium element and mass concentration be 25%～45% Ludox in the mol ratio of element silicon be 1:(0.5～1.5)；
Three, the preparation of graphene oxide/alkali-activated carbonatite mixed liquor: brown color graphene oxide suspension step one obtained joins in the alkali-activated carbonatite solution that step 2 obtains, after magnetic agitation mixing 10min～30min, in-situ reducing 0.01h～72h when temperature is 20 DEG C～80 DEG C, obtains graphene oxide/alkali-activated carbonatite mixed liquor；
Four, the preparation of graphene/aluminum silicate polymer slurry: graphene oxide step 3 obtained/alkali-activated carbonatite mixed liquor is placed in the ice-water bath that temperature is 0 DEG C～5 DEG C, add aluminosilicate powder body, ultrasonic and mechanical agitation 25min～45min, obtain graphene/aluminum silicate polymer slip, it is subsequently adding deionized water, regulates to graphene/aluminum silicate polymer slip at shear rate 60S-1～80S-1Time viscosity be 150mPa s～500mPa s, obtain graphene/aluminum silicate polymer slurry；In described aluminosilicate powder body, element silicon is 1:1 with the mol ratio of aluminium element；
Five, curing molding: graphene/aluminum silicate polymer slurry step 4 obtained is poured in mould, it is placed in vacuum tank aerofluxus, it is subsequently placed in maintenance 24h～240h in the drying baker that temperature is 40 DEG C～80 DEG C, is obtained by graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing；In the described graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare, element silicon is (1～4) with the mol ratio of aluminium element: 1；
The mass ratio of graphene oxide powder described in step one and aluminosilicate powder body described in step 4 is (0.01～0.15): 100.
The invention has the beneficial effects as follows:
The graphene/aluminum silicate polymer composite that the present invention prepares, with graphene oxide for raw material, utilize the hydrophilic of surface of graphene oxide oxygen-containing functional group, can be easier to be scattered in water base silicate solutions, carry out reaction in-situ simultaneously with aluminosilicate polymer alkali-activated carbonatite solution, and then polymerization obtains required composite；Owing to there is bonding action between alkali-activated carbonatite solution and graphene oxide, graphene oxide is not easy to reunite, and has good dispersibility and the compatibility in aluminosilicate polymer slurry.After curing molding, obtaining graphene/aluminum silicate polymer composite, technique is simple, and reducing degree is controlled, and the composite machinery performance prepared is good, and density is about 1.1g/cm3～1.5g/cm3Between, fracture toughness can arrive 0.12MPa m1/2～0.21MPa m1/2Bending strength can reach 10～20MPa, it is improved compared to un-added matrix material, elastic modelling quantity can reach 7GPa～8GPa, the controlled easy adjustment of reducing degree of graphene/aluminum silicate polymer composite Graphene prepared by the present invention, solves Graphene problem of bad dispersibility, easily reunion in aluminosilicate polymer；Preparation is simple, good manufacturability, and the Graphene after reduction is evenly distributed, good dispersion, and intensity is high, good toughness；And make aluminosilicate polymer material more for structure-function integration potential, preparation condition energy-conserving and environment-protective, can be used for structural material and sensing original paper uses.
Accompanying drawing explanation
Fig. 1 is the Graphene after reducing in graphene oxide/alkali-activated carbonatite mixed liquor in embodiment one step 3 and the FT-IR comparison diagram of graphene oxide powder in step one, wherein 1 is the FT-IR curve of graphene oxide powder in step one, and 2 is the FT-IR curve of the Graphene after reducing in graphene oxide/alkali-activated carbonatite mixed liquor in embodiment one step 3；
Fig. 2 is the graphene/aluminum silicate polymer composite fracture SEM figure utilizing graphene oxide in-situ reducing to prepare that embodiment one obtains；
Fig. 3 is the XRD figure of the graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare that embodiment one obtains；Wherein 1 is quartz phase, and A is the XRD curve of graphene/aluminum silicate polymer composite, and B is the XRD curve of metakaolin.
Detailed description of the invention
Detailed description of the invention one: a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare of present embodiment is prepared from by graphene oxide suspension, alkali-activated carbonatite solution and aluminosilicate powder body；
Described graphene oxide suspension is mixed by graphene oxide powder and deionized water；The quality of described graphene oxide powder and the volume ratio of deionized water are (1～20) mg:1mL；
Described alkali-activated carbonatite solution is mixed by the Ludox that potassium hydroxide and mass concentration are 25%～45%；In described potassium hydroxide potassium element and mass concentration be 25%～45% Ludox in the mol ratio of element silicon be 1:(0.5～1.5)；
Graphene oxide powder and the mass ratio of aluminosilicate powder body in described graphene oxide suspension are (0.01～0.15): 100；
In described aluminosilicate powder body, element silicon is 1:1 with the mol ratio of aluminium element；
In the described graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare, element silicon is (1～4) with the mol ratio of aluminium element: 1.
Deionized water described in present embodiment is neutral.
Aluminosilicate powder body described in present embodiment is a kind of or wherein several mixture in metakaolin, flyash, volcanic ash, montmorillonite and illitic soil etc., is mixed by any ratio during for mixture.
Detailed description of the invention two: present embodiment and detailed description of the invention one the difference is that: the quality of described graphene oxide powder and the volume ratio of deionized water are 16.7mg:1mL.Other are identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two the difference is that: in described potassium hydroxide potassium element and mass concentration be 25%～45% Ludox in the mol ratio of element silicon be 1:1.Other are identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three the difference is that: in the described graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare, element silicon is 2:1 with the mol ratio of aluminium element.Other are identical with one of detailed description of the invention one to three.
Detailed description of the invention five: the preparation method of a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare of present embodiment is to sequentially include the following steps:
One, the preparation of graphene oxide suspension: graphene oxide powder ultrasonic is scattered in deionized water, supersound process 2h～6h, obtain brown color graphene oxide suspension；The quality of described graphene oxide powder and the volume ratio of deionized water are (1～20) mg:1mL；
Two, the preparation of alkali-activated carbonatite solution: potassium hydroxide is joined in the Ludox that mass concentration is 25%～45%, magnetic agitation mixing 20h～80h, obtain alkali-activated carbonatite solution；In described potassium hydroxide potassium element and mass concentration be 25%～45% Ludox in the mol ratio of element silicon be 1:(0.5～1.5)；
Three, the preparation of graphene oxide/alkali-activated carbonatite mixed liquor: brown color graphene oxide suspension step one obtained joins in the alkali-activated carbonatite solution that step 2 obtains, after magnetic agitation mixing 10min～30min, in-situ reducing 0.01h～72h when temperature is 20 DEG C～80 DEG C, obtains graphene oxide/alkali-activated carbonatite mixed liquor；
Four, the preparation of graphene/aluminum silicate polymer slurry: graphene oxide step 3 obtained/alkali-activated carbonatite mixed liquor is placed in the ice-water bath that temperature is 0 DEG C～5 DEG C, add aluminosilicate powder body, ultrasonic and mechanical agitation 25min～45min, obtain graphene/aluminum silicate polymer slip, it is subsequently adding deionized water, regulates to graphene/aluminum silicate polymer slip at shear rate 60S-1～80S-1Time viscosity be 150mPa s～500mPa s, obtain graphene/aluminum silicate polymer slurry；In described aluminosilicate powder body, element silicon is 1:1 with the mol ratio of aluminium element；
Five, curing molding: graphene/aluminum silicate polymer slurry step 4 obtained is poured in mould, it is placed in vacuum tank aerofluxus, it is subsequently placed in maintenance 24h～240h in the drying baker that temperature is 40 DEG C～80 DEG C, is obtained by graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing；In the described graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare, element silicon is (1～4) with the mol ratio of aluminium element: 1；
The mass ratio of graphene oxide powder described in step one and aluminosilicate powder body described in step 4 is (0.01～0.15): 100.
Deionized water described in present embodiment is neutral.
Aluminosilicate powder body described in present embodiment is a kind of or wherein several mixture in metakaolin, flyash, volcanic ash, montmorillonite and illitic soil etc., is mixed by any ratio during for mixture.
Detailed description of the invention six: present embodiment and detailed description of the invention five the difference is that: the quality of graphene oxide powder described in step one and the volume ratio of deionized water are 16.7mg:1mL.Other are identical with detailed description of the invention five.
Detailed description of the invention seven: present embodiment and detailed description of the invention five or six the difference is that: in potassium hydroxide described in step 2 potassium element and mass concentration be 25%～45% Ludox in the mol ratio of element silicon be 1:1.Other are identical with detailed description of the invention one or two.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention five to seven the difference is that: in step 3 when temperature is 60 DEG C in-situ reducing 72h.Other are identical with one of detailed description of the invention five to seven.
Detailed description of the invention nine: one of present embodiment and detailed description of the invention five to eight the difference is that: step 5 is placed in maintenance 168h in the drying baker that temperature is 60 DEG C.Other are identical with one of detailed description of the invention five to eight.
Detailed description of the invention ten: one of present embodiment and detailed description of the invention five to eight the difference is that: utilizing the mol ratio of element silicon and aluminium element in graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing described in step 5 is 2:1.Other are identical with one of detailed description of the invention five to nine.
Beneficial effects of the present invention is verified by following example:
Embodiment one: the preparation method of a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare is to sequentially include the following steps:
One, the preparation of graphene oxide suspension: graphene oxide powder ultrasonic is scattered in deionized water, supersound process 5h, obtain brown color graphene oxide suspension；The quality of described graphene oxide powder and the volume ratio of deionized water are 16.7mg:1mL；
Two, the preparation of alkali-activated carbonatite solution: potassium hydroxide is joined in the Ludox that mass concentration is 40%, magnetic agitation mixing 20h～80h, obtain alkali-activated carbonatite solution；In described potassium hydroxide potassium element and mass concentration be 40% Ludox in the mol ratio of element silicon be 1:1；
Three, the preparation of graphene oxide/alkali-activated carbonatite mixed liquor: brown color graphene oxide suspension step one obtained joins in the alkali-activated carbonatite solution that step 2 obtains, after magnetic agitation mixing 15min, the in-situ reducing 72h when temperature is 60 DEG C, obtains graphene oxide/alkali-activated carbonatite mixed liquor；
Four, the preparation of graphene/aluminum silicate polymer slurry: graphene oxide step 3 obtained/alkali-activated carbonatite mixed liquor is placed in the ice-water bath that temperature is 0 DEG C～5 DEG C, add metakaolin powder body, ultrasonic and mechanical agitation 25min～45min, obtain graphene/aluminum silicate polymer slip, it is subsequently adding deionized water, regulates to graphene/aluminum silicate polymer slip at shear rate 60S-1～80S-1Time viscosity be 150mPa s～500mPa s, obtain graphene/aluminum silicate polymer slurry；Described metakaolin powder body by Kaolin temperature be under 800 DEG C of conditions calcine 2h obtain；In described metakaolin powder body, element silicon is 1:1 with the mol ratio of aluminium element；
Five, curing molding: graphene/aluminum silicate polymer slurry step 4 obtained is poured in mould, it is placed in vacuum tank aerofluxus, it is subsequently placed in maintenance 168h in the drying baker that temperature is 60 DEG C, is obtained by graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing；In the described graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare, element silicon is 2:1 with the mol ratio of aluminium element；
The mass ratio of graphene oxide powder described in step one and metakaolin powder body described in step 4 is 0.1:100.
Fig. 1 is the Graphene after reducing in graphene oxide/alkali-activated carbonatite mixed liquor in embodiment one step 3 and the FT-IR comparison diagram of graphene oxide powder in step one, wherein 1 is the FT-IR curve of graphene oxide powder in step one, and 2 is the FT-IR curve of the Graphene after reducing in graphene oxide/alkali-activated carbonatite mixed liquor in embodiment one step 3；From the change of Tu Zhong functional group it can be seen that graphene oxide is reduced alkali-activated carbonatite solution.
Fig. 2 is the graphene/aluminum silicate polymer composite fracture SEM figure utilizing graphene oxide in-situ reducing to prepare that embodiment one obtains；Sample incision position from figure, it can be seen that with aluminosilicate polymer matrix in conjunction with fine and equally distributed Graphene, fracture is uneven, has the effect that corner angle fluctuating produces after mostly relatively being addition Graphene.
Fig. 3 is the XRD figure of the graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare that embodiment one obtains；Wherein 1 is quartz phase, and A is the XRD curve of graphene/aluminum silicate polymer composite, and B is the XRD curve of metakaolin；As can be seen from the figure there is the feature amorphous peak of aluminosilicate polymer near 28 °, illustrate that the present invention utilizes graphene oxide in-situ reducing to prepare graphene/aluminum silicate polymer composite.The impurity that wherein peak of quartz phase comes from raw material metakaolin has neither part nor lot in synthetic reaction.
In graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing that what the present embodiment obtained utilize, graphene oxide is 1% with metakaolin mass ratio in aluminosilicate polymer based composites, and fracture toughness is (0.11～0.17) MPam1/2, bending strength is (12.3～13.3) MPa, and elastic modelling quantity is (5.8～6.2) GPa.
Embodiment two: the present embodiment and embodiment one are different in that: the quality of graphene oxide powder described in step one and the volume ratio of deionized water are 7.5mg:1mL；Brown color graphene oxide suspension step one obtained in step 3 joins in the alkali-activated carbonatite solution that step 2 obtains, after magnetic agitation mixing 15min, and the in-situ reducing 5min when temperature is 25 DEG C.Other are identical with embodiment one.
In graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing that what the present embodiment obtained utilize, graphene oxide is 0.3% with metakaolin mass ratio in aluminosilicate polymer based composites, and fracture toughness is (0.14～0.2) MPam1/2, bending strength is (17.5～18.3) MPa, and elastic modelling quantity is (7.5～7.9) GPa.
Embodiment three: the present embodiment and embodiment one or two are different in that: the volume ratio of the quality of graphene oxide powder described in rapid one and deionized water is 12.5mg:1mL.
In graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing that what the present embodiment obtained utilize, graphene oxide is 0.5% with metakaolin mass ratio in aluminosilicate polymer based composites, and fracture toughness is (0.15～0.27) MPam1/2, bending strength is (9.3～10.7) MPa, and elastic modelling quantity is (6.5～7.3) GPa.
Claims (6)
1. the preparation method of the graphene/aluminum silicate polymer composite that a kind utilizes graphene oxide in-situ reducing to prepare, it is characterised in that the preparation method utilizing graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing is to sequentially include the following steps:
One, the preparation of graphene oxide suspension: graphene oxide powder ultrasonic is scattered in deionized water, supersound process 2h～6h, obtain brown color graphene oxide suspension；The quality of described graphene oxide powder and the volume ratio of deionized water are (1～20) mg:1mL；
Two, the preparation of alkali-activated carbonatite solution: potassium hydroxide is joined in the Ludox that mass concentration is 25%～45%, magnetic agitation mixing 20h～80h, obtain alkali-activated carbonatite solution；In described potassium hydroxide potassium element and mass concentration be 25%～45% Ludox in the mol ratio of element silicon be 1:(0.5～1.5)；
Three, the preparation of graphene oxide/alkali-activated carbonatite mixed liquor: brown color graphene oxide suspension step one obtained joins in the alkali-activated carbonatite solution that step 2 obtains, after magnetic agitation mixing 10min～30min, in-situ reducing 0.01h～72h when temperature is 20 DEG C～80 DEG C, obtains graphene oxide/alkali-activated carbonatite mixed liquor；
Four, the preparation of graphene/aluminum silicate polymer slurry: graphene oxide step 3 obtained/alkali-activated carbonatite mixed liquor is placed in the ice-water bath that temperature is 0 DEG C～5 DEG C, add aluminosilicate powder body, ultrasonic and mechanical agitation 25min～45min, obtain graphene/aluminum silicate polymer slip, it is subsequently adding deionized water, regulates to graphene/aluminum silicate polymer slip at shear rate 60S-1～80S-1Time viscosity be 150mPa s～500mPa s, obtain graphene/aluminum silicate polymer slurry；In described aluminosilicate powder body, element silicon is 1:1 with the mol ratio of aluminium element；
Five, curing molding: graphene/aluminum silicate polymer slurry step 4 obtained is poured in mould, it is placed in vacuum tank aerofluxus, it is subsequently placed in maintenance 24h～240h in the drying baker that temperature is 40 DEG C～80 DEG C, is obtained by graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing；In the described graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare, element silicon is (1～4) with the mol ratio of aluminium element: 1；
The mass ratio of graphene oxide powder described in step one and aluminosilicate powder body described in step 4 is (0.01～0.15): 100.
2. the preparation method of a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare according to claim 1, it is characterised in that the quality of graphene oxide powder described in step one and the volume ratio of deionized water are 16.7mg:1mL.
3. the preparation method of a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare according to claim 1, it is characterised in that in potassium hydroxide described in step 2 potassium element and mass concentration be 25%～45% Ludox in the mol ratio of element silicon be 1:1.
4. the preparation method of a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare according to claim 1, it is characterised in that in step 3 when temperature is 60 DEG C in-situ reducing 72h.
5. the preparation method of a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare according to claim 1, it is characterised in that be placed in maintenance 168h in the drying baker that temperature is 60 DEG C in step 5.
6. the preparation method of a kind of graphene/aluminum silicate polymer composite utilizing graphene oxide in-situ reducing to prepare according to claim 1, it is characterised in that utilizing the mol ratio of element silicon and aluminium element in graphene/aluminum silicate polymer composite prepared by graphene oxide in-situ reducing described in step 5 is 2:1.
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| CN103865114A (en) * | 2014-02-27 | 2014-06-18 | 上海工程技术大学 | Imvite/natural rubber composite and preparation method thereof |
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