CN111485418A - Preparation method of plant fiber cloth with surface grafted with graphene oxide-silicon dioxide - Google Patents
Preparation method of plant fiber cloth with surface grafted with graphene oxide-silicon dioxide Download PDFInfo
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- CN111485418A CN111485418A CN202010193549.2A CN202010193549A CN111485418A CN 111485418 A CN111485418 A CN 111485418A CN 202010193549 A CN202010193549 A CN 202010193549A CN 111485418 A CN111485418 A CN 111485418A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 96
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 81
- 239000004744 fabric Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 241000196324 Embryophyta Species 0.000 claims description 80
- 239000000243 solution Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000009210 therapy by ultrasound Methods 0.000 claims description 18
- 239000000084 colloidal system Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 235000004431 Linum usitatissimum Nutrition 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 10
- 238000003760 magnetic stirring Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000006070 nanosuspension Substances 0.000 claims description 3
- 244000198134 Agave sisalana Species 0.000 claims description 2
- 240000008564 Boehmeria nivea Species 0.000 claims description 2
- 240000006240 Linum usitatissimum Species 0.000 claims 1
- 238000013001 point bending Methods 0.000 abstract description 12
- 239000011347 resin Substances 0.000 abstract description 10
- 229920005989 resin Polymers 0.000 abstract description 10
- 239000002131 composite material Substances 0.000 abstract description 8
- 238000012986 modification Methods 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000003822 epoxy resin Substances 0.000 abstract 1
- 229920000647 polyepoxide Polymers 0.000 abstract 1
- 239000000463 material Substances 0.000 description 15
- 241000208202 Linaceae Species 0.000 description 13
- 239000000805 composite resin Substances 0.000 description 12
- 238000013329 compounding Methods 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- 239000003733 fiber-reinforced composite Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 239000000203 mixture Substances 0.000 description 1
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- D—TEXTILES; PAPER
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D06B13/00—Treatment of textile materials with liquids, gases or vapours with aid of vibration
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
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- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
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Abstract
A preparation method of plant fiber cloth with surface grafted with graphene oxide-silicon dioxide. The invention belongs to the field of plant fiber modification. The invention aims to solve the technical problems of lower mechanical property and poorer humidity resistance of the traditional plant fiber composite material. The method comprises the following steps: growing silicon dioxide on the surface of graphene oxide, and then adding tetraethoxysilane to prepare a graphene oxide-silicon dioxide suspension; secondly, cleaning the plant fiber cloth by water and alkali solution; and thirdly, treating the plant fiber cloth by using the graphene oxide-silicon dioxide suspension under the ultrasonic action, and grafting a graphene oxide-silicon dioxide nano material on the surface of the fiber to obtain the plant fiber cloth with the graphene oxide-silicon dioxide grafted on the surface. The treated plant fiber can greatly improve the interface bonding property with a resin matrix, improve the mechanical property of the plant fiber reinforced epoxy resin matrix composite material, reduce the dispersion degree of the mechanical property, and achieve the three-point bending strength of 126.0-150 MPa.
Description
Technical Field
The invention belongs to the field of plant fiber modification, and particularly relates to a preparation method of plant fiber cloth with a surface grafted with graphene oxide-silicon dioxide.
Background
The plant fiber reinforced composite material has the advantages of short production period, wide source, low price, biodegradability, high specific strength/modulus and the like, and the application and development of the environment-friendly plant fiber reinforced composite material become a research hotspot aiming at the problems that the traditional fiber reinforced composite material consumes a large amount of resources, seriously influences the sustainable development of human beings and the like. However, compared with the traditional fiber, the plant fiber composite material has the problems of lower mechanical property, poorer humidity resistance and the like, and restricts the application of the plant fiber.
The mechanical properties of the plant fiber composite material can be improved by the method of surface modification of the plant fiber, wherein chemical treatment is considered to be one of the most effective methods. In recent years, researches show that the mechanical property of the plant fiber composite material can be greatly improved by improving the interface bonding property of the plant fiber and the resin matrix through the nano particle grafting.
Disclosure of Invention
The invention aims to solve the technical problems of low mechanical property and poor humidity resistance of the conventional plant fiber composite material, and provides a preparation method of plant fiber cloth with the surface grafted with graphene oxide-silicon dioxide.
The preparation method of the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide comprises the following steps:
firstly, preparing a nano suspension:
a. ultrasonically dispersing graphene oxide in a mixed solution of absolute ethyl alcohol/deionized water to obtain a suspension;
b. adjusting the pH value of the suspension obtained in the step one a by using ammonia water, then dropwise adding ethyl orthosilicate into the suspension, sequentially performing ultrasonic treatment and magnetic stirring treatment, centrifuging to obtain a graphene oxide-silicon dioxide colloid, and cleaning the obtained graphene oxide-silicon dioxide colloid by using absolute ethyl alcohol;
c, ultrasonically dispersing the graphene oxide-silicon dioxide colloid cleaned in the step one b in deionized water to obtain a graphene oxide-silicon dioxide suspension solution;
secondly, alkali treatment of the plant fiber cloth:
d. immersing the plant fiber cloth into distilled water for ultrasonic cleaning;
e. d, placing the plant fibers cleaned in the step d in NaOH solution for ultrasonic treatment;
f. taking the steps d-e as a cycle, and repeating the operation until the pH value of the surface of the plant fiber cloth is 6.5-7 to obtain the plant fiber cloth after alkali treatment;
thirdly, grafting graphene oxide-silicon dioxide on the surface of the fiber cloth:
g. placing the plant fiber subjected to alkali treatment obtained in the step two in the graphene oxide-silicon dioxide suspension solution obtained in the step one for ultrasonic treatment;
h. and g, taking out the plant fiber cloth treated in the step g, putting the plant fiber cloth into distilled water for cleaning, taking out the plant fiber cloth after cleaning, and drying to obtain the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide.
Further limiting, the mass fraction of the graphene oxide in the suspension in the step one a is 0.005% -5%.
Further limiting, in the mixed solution of absolute ethyl alcohol/deionized water in the step one a, the volume ratio of absolute ethyl alcohol to deionized water is (1-7): 1.
further defined, the ultrasonic dispersion parameters in the step a are as follows: the ultrasonic power is 200W-1500W, and the ultrasonic time is 0.5 h-3 h.
Further limiting, in the step one b, ammonia water is used for adjusting the pH value of the suspension obtained in the step one a to be 8-12.
Further limiting, the volume ratio of the tetraethoxysilane in the step one b to the absolute ethyl alcohol/deionized water mixed solution in the step one a is (0.1-10): 100.
further defined, the ultrasonic treatment parameters in the step one b are as follows: the ultrasonic power is 200W-1500W, and the ultrasonic time is 0.5 h-3 h.
Further limiting, the magnetic stirring processing parameters in the step one b are as follows: the rotating speed is 100rpm to 1500rpm, and the magnetic stirring time is 1h to 48 h.
Further limiting, the graphene oxide-silicon dioxide colloid obtained in the step one b is washed with absolute ethyl alcohol for 1-10 times.
Further limiting, in the step one c, the mass fraction of the graphene oxide-silica colloid in the graphene oxide-silica suspension solution is 0.005% -5%.
Further defined, the ultrasonic dispersion parameters in the step one c are: the ultrasonic power is 200W-1500W, and the ultrasonic time is 0.5 h-3 h.
Further limiting, the plant fiber cloth in the step two d is formed by weaving one or more of flax fiber, ramie fiber and sisal fiber according to any ratio, and the surface density is 50g/m2～500g/m2。
Further limiting, the ultrasonic cleaning parameters in the step two d are as follows: the ultrasonic power is 200W-1500W, the ultrasonic time is 0.5 min-120 min, and the distilled water temperature is 25 ℃ to 90 ℃ during ultrasonic cleaning.
Further limiting, the mass concentration of the NaOH solution in the step two e is 0.5-10%.
Further defined, the ultrasonic treatment parameters in the step two e are as follows: the ultrasonic power is 200W-1500W, and the ultrasonic time is 0.5 min-30 min.
Further limiting, the ratio of the mass of the graphene oxide-silicon dioxide suspension liquid to the area of the plant fiber cloth in the third g is (10-500) g:0.1m2；
Further defined, the ultrasonic treatment parameters in the third step g are as follows: the ultrasonic power is 200W-1500W, and the ultrasonic time is 0.15 h-3 h.
And further limiting, in the third step, putting the mixture into distilled water for cleaning for 1-10 times.
Further limiting, in the third step, the drying parameters are as follows: the temperature is 60-120 ℃, and the time is 60-1440 min.
Compared with the prior art, the invention has the remarkable effects as follows:
the invention provides an efficient and simple treatment method for grafting novel graphene oxide-silicon dioxide mixed nanoparticles on the surface of plant fiber cloth, the mechanical property and the humidity and heat resistance of a plant fiber composite material can be effectively improved by using the method, and the method is favorable for realizing high performance of plant fibers.
The invention cleans low molecular weight substances on the surface of the plant fiber by water washing and ultrasonic action of aqueous alkali, and increases the roughness of the surface of the fiber; and (3) growing nano silicon dioxide on the surface of the graphene oxide, and preparing a suspension to enable the graphene oxide-silicon dioxide to freely settle on the surface of the plant fiber.
The three-point bending strength of the plant fiber cloth/resin composite material with the surface grafted with the graphene oxide-silicon dioxide prepared by the test is tested to be 126.0MPa-150MPa according to the international standard ASTM D7264.
Drawings
FIG. 1 is a TEM image of a suspension of graphene oxide obtained in step one a of the first embodiment;
FIG. 2 is a TEM image of the graphene oxide-silica suspension obtained in the first step (c) of the embodiment;
fig. 3 is an SEM image of the plant fiber cloth with the graphene oxide-silicon dioxide grafted on the surface, obtained in the third step of the embodiment.
Detailed Description
The first embodiment is as follows: the preparation method of the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide comprises the following steps:
firstly, preparing a nano suspension:
a. ultrasonically dispersing graphene oxide in a mixed solution of absolute ethyl alcohol/deionized water to obtain a suspension; wherein the mass fraction of graphene oxide in the suspension is 0.01%; the volume ratio of the absolute ethyl alcohol to the deionized water in the mixed solution of the absolute ethyl alcohol and the deionized water is 5: 1; the ultrasonic dispersion parameters are as follows: the ultrasonic power is 200W, and the ultrasonic time is 1 h;
b. adjusting the pH value of the suspension obtained in the step one a to 9 by using ammonia water, then dropwise adding ethyl orthosilicate into the suspension, sequentially performing ultrasonic treatment and magnetic stirring treatment, centrifuging to obtain a graphene oxide-silicon dioxide colloid, and cleaning the obtained graphene oxide-silicon dioxide colloid for 3 times by using absolute ethyl alcohol; wherein the volume ratio of the tetraethoxysilane to the absolute ethyl alcohol/deionized water mixed solution in the step one a is 2: 100, respectively; the ultrasonic treatment parameters are as follows: the ultrasonic power is 200W, and the ultrasonic time is 1 h; the magnetic stirring treatment parameters are as follows: the rotating speed is 200rpm, and the magnetic stirring time is 12 hours;
c, ultrasonically dispersing the graphene oxide-silicon dioxide colloid cleaned in the step one b in deionized water to obtain a graphene oxide-silicon dioxide suspension solution; wherein the ultrasonic dispersion parameters are: the ultrasonic power is 200W, and the ultrasonic time is 1 h; the mass fraction of the graphene oxide-silicon dioxide colloid in the graphene oxide-silicon dioxide suspension solution is 0.01%;
secondly, alkali treatment of the plant fiber cloth:
d. immersing the plant fiber cloth into distilled water for ultrasonic cleaning; wherein the plant fiber cloth is woven by flax fibers and has the surface density of 240g/m2(ii) a The ultrasonic cleaning parameters are as follows: the ultrasonic power is 200W, the ultrasonic time is 30min, and the distilled water temperature is 25 ℃ during ultrasonic cleaning;
e. d, placing the plant fibers cleaned in the step d in NaOH solution for ultrasonic treatment; wherein the mass concentration of the NaOH solution is 5%; the ultrasonic treatment parameters are as follows: the ultrasonic power is 200W, and the ultrasonic time is 30 min;
f. taking the steps d-e as a cycle, and repeating the operation until the pH value of the surface of the plant fiber cloth is 7 to obtain the plant fiber cloth after alkali treatment;
thirdly, grafting graphene oxide-silicon dioxide on the surface of the fiber cloth:
g. placing the plant fiber subjected to alkali treatment obtained in the step two in the graphene oxide-silicon dioxide suspension solution obtained in the step one for ultrasonic treatment; wherein the ratio of the mass of the graphene oxide-silicon dioxide suspension to the area of the plant fiber cloth is 500g:1m2(ii) a The ultrasonic treatment parameters are as follows: the ultrasonic power is 200W, and the ultrasonic time is 0.25h；
h. G, taking out the plant fiber cloth treated in the step g, putting the plant fiber cloth into distilled water for cleaning for 2 times, taking out the plant fiber cloth after cleaning, and drying to obtain the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide; wherein the drying parameters are as follows: the temperature is 110 deg.C, and the time is 120 min.
In the embodiment, the graphene oxide is single-layer high-purity graphene oxide, has a sheet diameter of 0.5-5 μm and a thickness of 0.8-1.2 nm, and is purchased from Xiancheng nano material science and technology Limited.
In the embodiment, the purity of the ethyl orthosilicate is more than 99%, the density of the ethyl orthosilicate at normal temperature is 0.933g/m L, and the ethyl orthosilicate is purchased from Shanghai Michelin Biochemical technology Co.
First, transmission electron microscope detection is performed on the graphene oxide suspension obtained in the first step a and the graphene oxide-silica suspension obtained in the first step c of the present embodiment, so as to obtain a TEM image of the graphene oxide suspension shown in fig. 1 and a TEM image of the graphene oxide-silica suspension shown in fig. 2. As can be seen from comparison of fig. 1 and fig. 2, the silica is adsorbed on the surface of the graphene oxide, and the graphene oxide-silica composite nanoparticle is formed.
And (ii) scanning electron microscope detection is performed on the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide obtained in the third step of the embodiment, so as to obtain an SEM image of the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide shown in fig. 3, and as can be seen from fig. 3, the graphene-silicon dioxide is successfully grafted to the surface of the flax fiber.
And (3) verification test: the following experiment is adopted to verify the modification effect of the specific embodiment on the plant fiber cloth, and the specific process is as follows:
preparing a resin and the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide obtained in the embodiment by a vacuum assisted injection molding method to obtain a plant fiber cloth/resin composite material with the surface grafted with the graphene oxide-silicon dioxide;
the resin is normal temperature impregnating adhesive (TS) which is purchased from Shandong Dagong composite material Co., Ltd;
the mass ratio of the resin to the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide is 12: 13;
the vacuum assisted injection molding has the specific parameters of vacuum degree of-0.08 MPa and normal temperature.
As a result: according to the international standard ASTM D7264, the three-point bending strength of the conventional flax fiber/resin composite material which is not treated by the method of the embodiment is tested to be 115.7MPa, and the three-point bending strength of the plant fiber cloth/resin composite material obtained by compounding the flax fiber cloth with the surface grafted with the graphene oxide-silicon dioxide and the resin obtained in the first embodiment is 132.2MPa, which is improved by 14.3%.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: in the step one a, the mass fraction of graphene oxide in the suspension is 0.03%; in the step one c, the mass fraction of the graphene oxide-silicon dioxide colloid in the graphene oxide-silicon dioxide suspension solution is 0.03%; other steps and parameters are the same as those in the first embodiment.
As a result: according to the international standard ASTM D7264, the three-point bending strength of the conventional flax fiber/resin composite material which is not treated by the method of the embodiment is tested to be 115.7MPa, and the three-point bending strength of the plant fiber cloth/resin composite material obtained by compounding the flax fiber cloth with the surface grafted with the graphene oxide-silicon dioxide and the resin obtained by the embodiment II is tested to be 136.9MPa, which is improved by 18.3%.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: in the step one a, the mass fraction of graphene oxide in the suspension is 0.05%; in the step one c, the mass fraction of the graphene oxide-silicon dioxide colloid in the graphene oxide-silicon dioxide suspension solution is 0.05%; other steps and parameters are the same as those in the first embodiment.
As a result: according to the international standard ASTM D7264, the three-point bending strength of the conventional flax fiber/resin composite material which is not treated by the method of the embodiment is tested to be 115.7MPa, and the three-point bending strength of the plant fiber cloth/resin composite material obtained by compounding the flax fiber cloth with the surface grafted with the graphene oxide-silicon dioxide and the resin obtained by the embodiment three is 149.0MPa, which is improved by 28.8%.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: in the step one a, the mass fraction of the graphene oxide in the suspension is 0.075%; in the step one c, the mass fraction of the graphene oxide-silicon dioxide colloid in the graphene oxide-silicon dioxide suspension solution is 0.075%; other steps and parameters are the same as those in the first embodiment.
As a result: according to the international standard ASTM D7264, the three-point bending strength of the conventional flax fiber/resin composite material which is not treated by the method of the embodiment is tested to be 115.7MPa, and the three-point bending strength of the plant fiber cloth/resin composite material obtained by compounding the flax fiber cloth with the surface grafted with the graphene oxide-silicon dioxide and the resin obtained by the embodiment four is 141.3MPa, which is improved by 22.1%.
The fifth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: in the step one a, the mass fraction of graphene oxide in the suspension is 0.1%; in the step one c, the mass fraction of the graphene oxide-silicon dioxide colloid in the graphene oxide-silicon dioxide suspension solution is 0.1%; other steps and parameters are the same as those in the first embodiment.
As a result: according to the international standard ASTM D7264, the three-point bending strength of the conventional flax fiber/resin composite material which is not treated by the method of the embodiment is tested to be 115.7MPa, and the three-point bending strength of the plant fiber cloth/resin composite material obtained by compounding the flax fiber cloth with the surface grafted with the graphene oxide-silicon dioxide and the resin obtained by the embodiment five is 138.4MPa, which is improved by 19.6%.
Claims (10)
1. A preparation method of plant fiber cloth with graphene oxide-silicon dioxide grafted on the surface is characterized by comprising the following steps:
firstly, preparing a nano suspension:
a. ultrasonically dispersing graphene oxide in a mixed solution of absolute ethyl alcohol/deionized water to obtain a suspension;
b. adjusting the pH value of the suspension obtained in the step one a by using ammonia water, then dropwise adding ethyl orthosilicate into the suspension, sequentially performing ultrasonic treatment and magnetic stirring treatment, centrifuging to obtain a graphene oxide-silicon dioxide colloid, and cleaning the obtained graphene oxide-silicon dioxide colloid by using absolute ethyl alcohol;
c, ultrasonically dispersing the graphene oxide-silicon dioxide colloid cleaned in the step one b in deionized water to obtain a graphene oxide-silicon dioxide suspension solution;
secondly, alkali treatment of the plant fiber cloth:
d. immersing the plant fiber cloth into distilled water for ultrasonic cleaning;
e. d, placing the plant fibers cleaned in the step d in NaOH solution for ultrasonic treatment;
f. taking the steps d-e as a cycle, and repeating the operation until the pH value of the surface of the plant fiber cloth is 6.5-7 to obtain the plant fiber cloth after alkali treatment;
thirdly, grafting graphene oxide-silicon dioxide on the surface of the fiber cloth:
g. placing the plant fiber subjected to alkali treatment obtained in the step two in the graphene oxide-silicon dioxide suspension solution obtained in the step one for ultrasonic treatment;
h. and g, taking out the plant fiber cloth treated in the step g, putting the plant fiber cloth into distilled water for cleaning, taking out the plant fiber cloth after cleaning, and drying to obtain the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide.
2. The method for preparing the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide as claimed in claim 1, wherein the mass fraction of the graphene oxide in the suspension in the step one a is 0.005-5%; in the step one a, the volume ratio of the absolute ethyl alcohol to the deionized water in the absolute ethyl alcohol/deionized water mixed solution is (1-7): 1.
3. the method for preparing the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide as claimed in claim 1, wherein the volume ratio of the ethyl orthosilicate in the step one b to the absolute ethyl alcohol/deionized water mixed solution in the step one a is (0.1-10): 100.
4. the method for preparing the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide as claimed in claim 1, wherein the ultrasonic dispersion parameters in the step a are as follows: the ultrasonic power is 200W-1500W, and the ultrasonic time is 0.5 h-3 h; in the step one b, ammonia water is used for adjusting the pH value of the suspension obtained in the step one a to 8-12; the ultrasonic treatment parameters in the step one b are as follows: the ultrasonic power is 200W-1500W, and the ultrasonic time is 0.5 h-3 h; the magnetic stirring treatment parameters in the step one b are as follows: the rotating speed is 100 rpm-1500 rpm, and the magnetic stirring time is 1 h-48 h; in the step one c, the ultrasonic dispersion parameters are as follows: the ultrasonic power is 200W-1500W, and the ultrasonic time is 0.5 h-3 h.
5. The method for preparing the plant fiber cloth with the surface grafted with the graphene oxide-silica according to claim 1, wherein the mass fraction of the graphene oxide-silica colloid in the graphene oxide-silica suspension solution in the step (c) is 0.005-5%.
6. The method for preparing the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide as claimed in claim 1, wherein the plant fiber cloth in the second step is woven by one or more of flax fibers, ramie fibers and sisal fibers, and the areal density of the plant fiber cloth is 50g/m2～500g/m2。
7. The preparation method of the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide as claimed in claim 1, wherein the ultrasonic cleaning parameters in the second step d are as follows: the ultrasonic power is 200W-1500W, the ultrasonic time is 0.5 min-120 min, and the distilled water temperature is 25 ℃ to 90 ℃ during ultrasonic cleaning.
8. The preparation method of the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide as claimed in claim 1, wherein the mass concentration of the NaOH solution in the second step is 0.5-10%; the ultrasonic treatment parameters in the second step e are as follows: the ultrasonic power is 200W-1500W, and the ultrasonic time is 0.5 min-30 min.
9. The method for preparing the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide as claimed in claim 1, wherein the ratio of the mass of the graphene oxide-silicon dioxide suspension to the area of the plant fiber cloth in the third g step is (10-500) g:0.1m2(ii) a The ultrasonic treatment parameters in the third step g are as follows: the ultrasonic power is 200W-1500W, and the ultrasonic time is 0.15 h-3 h.
10. The preparation method of the plant fiber cloth with the surface grafted with the graphene oxide-silicon dioxide as claimed in claim 1, wherein the drying parameters in the third step are as follows: the temperature is 60-120 ℃, and the time is 60-1440 min.
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