CN104650517A - Preparation method of graphene oxide composite material - Google Patents
Preparation method of graphene oxide composite material Download PDFInfo
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- CN104650517A CN104650517A CN201410744384.8A CN201410744384A CN104650517A CN 104650517 A CN104650517 A CN 104650517A CN 201410744384 A CN201410744384 A CN 201410744384A CN 104650517 A CN104650517 A CN 104650517A
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Abstract
The invention discloses a preparation method of a graphene oxide composite material, and belongs to the field of material preparation. The method is characterized by comprising the following steps: adding deionized water into graphene oxide to be ultrasonically dispersed; adding ammonia water to be uniformly stirred; adding hydrazine hydrate to be stirred and transferring into an oil-bath pot to be continuously stirred; cooling and filtering a product; drying the obtained product at the room temperature in the air to prepare graphene RGO with reduced hydrazine hydrate; ultrasonically dispersing RGO into DMF; dissolving PMMA into DMF and mechanically stirring until a mixture is completely dissolved; pouring the RGO dispersion liquid into PMMA solutions to be mixed and stirring at a high speed under the room temperature; finally, drying the obtained product under a vacuum drying box at the temperature of 60 DEG C; and performing hot-pressing and molding. According to the effective improvement of a composite material preparation process, the electrical conductivity of the prepared graphene oxide composite material is improved, the dielectric constants are increased, and the preparation process is relatively simplified, and therefore, the corresponding production cost is saved, the production efficiency is improved, and the graphene oxide composite material has a great popularization value.
Description
Technical field
the invention belongs to field of material preparation, particularly relate to a kind of preparation method of graphene oxide composite material.
Background technology
In the prior art, improve specific inductivity, be generally the stupalith adding high-k in polymkeric substance for capacitance material, but the add-on of stupalith is general higher, this can reduce again the mechanical property of polymkeric substance.Graphene has the performance of many excellences due to the structure of its uniqueness, as the modulus in tension etc. of high carrier mobility, high electroconductibility, large theoretical specific surface area, superelevation, and demonstrates huge potentiality in polymer nanocomposites field.It can be used as electrical-conductive nanometer filler very potential to the specific inductivity improving polymer-based dielectric material.Come and polymkeric substance compound with the Graphene of modification in traditional most of working set, but the conjugated structure of Graphene can be destroyed to Graphene modification, thus greatly weakening the conductivity of Graphene, this is disadvantageous to the polymer/graphene composite material preparing high-k.
Summary of the invention
The present invention is intended to solve the problem, and provides a kind of preparation method of graphene oxide composite material.
A preparation method for graphene oxide composite material, is characterized in that comprising the steps:
(1) take 600 mg graphene oxide GO in beaker, add the deionized water of 600 mL, ultrasonic disperse 2h, obtain the GO dispersion liquid of 1mg/mL; Afterwards, add 10 mL ammoniacal liquor, stir evenly.Add the hydrazine hydrate of 1.2 mL again, after mixture stirs 30min, move into after continuing stirring reaction in oil bath pan, mixture becomes black from yellowish brown; Cooled by product, be the nylon filter membrane filtration of 1.2 μm with aperture, after deionized water wash, ethanol is washed, by the product drying at room temperature in atmosphere obtained, and the Graphene RGO of obtained hydrazine hydrate reduction;
(2) by a certain amount of RGO nanometer sheet ultrasonic disperse in DMF, obtain the RGO dispersion liquid that concentration is 1mg/L; Meanwhile, a certain amount of PMMA to be also dissolved in DMF and machinery is stirred to PMMA dissolves completely; Then, RGO dispersion liquid is poured in PMMA solution and mixes, and at room temperature high-speed stirring; Finally, mixture is precipitated in methyl alcohol, filtration of crude product, hot water wash, methanol wash; Products therefrom is dry in the vacuum drying oven of 60 DEG C, and remove residual solvent, then at 200 DEG C, hot-forming under 15MPa is sheet material.
The preparation method of a kind of graphene oxide composite material of the present invention, it is characterized in that the temperature of oil bath pan described in step (1) is 95 DEG C, the oil bath time is 2h.
The preparation method of a kind of graphene oxide composite material of the present invention, is characterized in that described in step (1), ethanol washes 3 times.
The preparation method of a kind of graphene oxide composite material of the present invention, is characterized in that described in step (2), the high-speed stirring time is 12h.
The preparation method of a kind of graphene oxide composite material of the present invention, is characterized in that the time of drying in loft drier described in step (2) is 12h.
The preparation method of a kind of graphene oxide composite material of the present invention, by the effective improvement to composite material preparation process, the electroconductibility of the graphene composite material prepared is improved, specific inductivity increases, preparation technology's relative simplicity, thus save corresponding production cost, improve production efficiency, there is larger promotional value.
Embodiment
A preparation method for graphene oxide composite material, is characterized in that comprising the steps:
(1) take 600 mg graphene oxide GO in beaker, add the deionized water of 600 mL, ultrasonic disperse 2h, obtain the GO dispersion liquid of 1mg/mL; Afterwards, add 10 mL ammoniacal liquor, stir evenly.Add the hydrazine hydrate of 1.2 mL again, after mixture stirs 30min, move into after continuing stirring reaction in oil bath pan, mixture becomes black from yellowish brown; Cooled by product, be the nylon filter membrane filtration of 1.2 μm with aperture, after deionized water wash, ethanol is washed, by the product drying at room temperature in atmosphere obtained, and the Graphene RGO of obtained hydrazine hydrate reduction;
(2) by a certain amount of RGO nanometer sheet ultrasonic disperse in DMF, obtain the RGO dispersion liquid that concentration is 1mg/L; Meanwhile, a certain amount of PMMA to be also dissolved in DMF and machinery is stirred to PMMA dissolves completely; Then, RGO dispersion liquid is poured in PMMA solution and mixes, and at room temperature high-speed stirring; Finally, mixture is precipitated in methyl alcohol, filtration of crude product, hot water wash, methanol wash; Products therefrom is dry in the vacuum drying oven of 60 DEG C, and remove residual solvent, then at 200 DEG C, hot-forming under 15MPa is sheet material.
The preparation method of a kind of graphene oxide composite material of the present invention, described in step (1), the temperature of oil bath pan is 95 DEG C, and the oil bath time is 2h.Described in step (1), ethanol washes 3 times.The high-speed stirring time described in step (2) is 12h.Time of drying in loft drier described in step (2) is 12h.GO surface is due to containing a large amount of oxy radicals, and its C/O ratio is 2.1, thus makes its specific conductivity be only 1.1 × 10
– 4s/m; And by after hydrazine hydrate reduction, namely the RGO Surface oxygen-containing groups of acquisition has obvious minimizing, and its C/O ratio reaches 12.0, and owing to having higher reducing degree, now the specific conductivity of RGO – N reaches 4.2 × 10
3s/m.After add RGO in PMMA, the specific inductivity of matrix material obviously increases, and under low and medium frequency, the RGO content added is more, and under same frequency, the specific inductivity of matrix material is also larger; On the other hand, in 102 ~ 106 Hz, RGO content is larger, and the amplitude that the specific inductivity of matrix material increases with frequency and declines is larger.RGO, as conducting medium, also can be regarded as the electrode of small electric container, and the PMMA in the middle of RGO lamella can as dielectric medium.Joined by RGO in PMMA, PMMA inside can be made on the one hand to form many trimmer capacitors, and the existence of trimmer capacitor can make the specific inductivity of matrix material larger than pure PMMA; Meanwhile, during energising, the electric charge moved freely of RGO inside can the interface between RGO and PMMA be gathered, thus makes RGO and PMMA produce interfacial polarization effect, and interfacial polarization also can make the specific inductivity of matrix material increase.Therefore, along with the increase of RGO content, the specific inductivity of PMMA/RGO matrix material increases.When the content of RGO is lower, RGO lamella is separated from each other, and only forms the trimmer capacitor of minority in matrix material, and interfacial polarization effect between RGO and PMMA is also more weak.When the content of RGO is higher, now in matrix material, the quantity of trimmer capacitor significantly increases, and trimmer capacitor is more responsive to change of frequency, and now the concentration of current carrier is also higher.
Claims (5)
1. a preparation method for graphene oxide composite material, is characterized in that comprising the steps:
(1) take 600 mg graphene oxide GO in beaker, add the deionized water of 600 mL, ultrasonic disperse 2h, obtain the GO dispersion liquid of 1mg/mL; Afterwards, add 10 mL ammoniacal liquor, stir evenly;
Add the hydrazine hydrate of 1.2 mL again, after mixture stirs 30 min, move into after continuing stirring reaction in oil bath pan, mixture becomes black from yellowish brown; Cooled by product, be the nylon filter membrane filtration of 1.2 μm with aperture, after deionized water wash, ethanol is washed, by the product drying at room temperature in atmosphere obtained, and the Graphene RGO of obtained hydrazine hydrate reduction;
(2) by a certain amount of RGO nanometer sheet ultrasonic disperse in DMF, obtain the RGO dispersion liquid that concentration is 1mg/L; Meanwhile, a certain amount of PMMA to be also dissolved in DMF and machinery is stirred to PMMA dissolves completely; Then, RGO dispersion liquid is poured in PMMA solution and mixes, and at room temperature high-speed stirring; Finally, mixture is precipitated in methyl alcohol, filtration of crude product, hot water wash, methanol wash; Products therefrom is dry in the vacuum drying oven of 60 DEG C, and remove residual solvent, then at 200 DEG C, hot-forming under 15 MPa is sheet material.
2. the preparation method of a kind of graphene oxide composite material as claimed in claim 1, it is characterized in that the temperature of oil bath pan described in step (1) is 95 DEG C, the oil bath time is 2h.
3. the preparation method of a kind of graphene oxide composite material as claimed in claim 1, is characterized in that described in step (1), ethanol washes 3 times.
4. the preparation method of a kind of graphene oxide composite material as claimed in claim 1, is characterized in that described in step (2), the high-speed stirring time is 12h.
5. the preparation method of a kind of graphene oxide composite material as claimed in claim 1, is characterized in that the time of drying in loft drier described in step (2) is 12h.
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| CN201410744384.8A CN104650517A (en) | 2014-12-09 | 2014-12-09 | Preparation method of graphene oxide composite material |
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| CN201410744384.8A CN104650517A (en) | 2014-12-09 | 2014-12-09 | Preparation method of graphene oxide composite material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106906028A (en) * | 2017-03-16 | 2017-06-30 | 柯鹏 | A kind of Graphene antiwear composite agent and preparation method thereof |
| CN107987444A (en) * | 2017-12-12 | 2018-05-04 | 常州工程职业技术学院 | A kind of graphene/PMMA heat-conductive composite materials, preparation method and applications |
| CN112661140A (en) * | 2020-12-11 | 2021-04-16 | 上海交通大学 | Preparation method of novel graphene nano narrow band |
| CN114047232A (en) * | 2021-11-25 | 2022-02-15 | 长春工业大学 | Preparation method of resistance type gas sensor based on sheet-shaped composite film |
| CN114538685A (en) * | 2022-02-15 | 2022-05-27 | 江苏万邦达环保科技有限公司 | Process for removing low-boiling organic matters in high-concentration wastewater |
-
2014
- 2014-12-09 CN CN201410744384.8A patent/CN104650517A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106906028A (en) * | 2017-03-16 | 2017-06-30 | 柯鹏 | A kind of Graphene antiwear composite agent and preparation method thereof |
| CN106906028B (en) * | 2017-03-16 | 2019-07-30 | 深圳市百顺源节能科技有限公司 | A kind of graphene antiwear composite agent and preparation method thereof |
| CN107987444A (en) * | 2017-12-12 | 2018-05-04 | 常州工程职业技术学院 | A kind of graphene/PMMA heat-conductive composite materials, preparation method and applications |
| CN112661140A (en) * | 2020-12-11 | 2021-04-16 | 上海交通大学 | Preparation method of novel graphene nano narrow band |
| CN114047232A (en) * | 2021-11-25 | 2022-02-15 | 长春工业大学 | Preparation method of resistance type gas sensor based on sheet-shaped composite film |
| CN114538685A (en) * | 2022-02-15 | 2022-05-27 | 江苏万邦达环保科技有限公司 | Process for removing low-boiling organic matters in high-concentration wastewater |
| CN114538685B (en) * | 2022-02-15 | 2022-12-02 | 江苏万邦达环保科技有限公司 | Process for removing low-boiling organic matters in high-concentration wastewater |
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