CN105111736A - Preparation method of graphene oxide/polyether type benzimidazole composite material - Google Patents
Preparation method of graphene oxide/polyether type benzimidazole composite material Download PDFInfo
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- CN105111736A CN105111736A CN201510527278.9A CN201510527278A CN105111736A CN 105111736 A CN105111736 A CN 105111736A CN 201510527278 A CN201510527278 A CN 201510527278A CN 105111736 A CN105111736 A CN 105111736A
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Abstract
The invention discloses a preparation method of a graphene oxide/polyether type benzimidazole composite material. The preparation method comprises the following steps: dispersing graphene oxide into dimethyl sulfoxide by adopting a solvent exchange method to obtain a graphene oxide organic solution; taking 3,3'-diaminodiphenyl, 4,4'-dibenzoate ether and PPMA as raw materials to react for 1-3 hours under a nitrogen condition at 140-160 DEG C, and washing to obtain polyether type benzimidazole; and dissolving the polyether type benzimidazole in the graphene oxide organic solvent, and evaporating the solvent to obtain the graphene oxide/polyether type benzimidazole composite material. By adopting the solvent exchange method, the graphene oxide can be completely dispersed in the organic solution, so that the preparation is simple. The obtained composite material has good mechanical properties, is high in thermal stability and can adapt to harsh environments.
Description
Technical field
The application relates to the preparation method of a kind of graphene oxide/polyether-type benzoglyoxaline matrix material.
Background technology
Graphene is a kind of two-dimentional carbon film only having an atomic thickness, it is uniquely a kind of material by individual layer atomic building that people find so far, hexagonal network is connected into by chemical bond-linking between carbon atom in carbon film, because the chemical bond between carbon atom is made up of sp2 hybridized orbital, therefore Graphene is very indomitable, possesses the good characteristic that other novel materials such as bent, electroconductibility is strong, physical strength good, light transmission is good do not possess.Graphene possesses the conductivity be not of the common run, and resistivity is very little, and electronics can move pole efficiently, and this respect performance is higher than traditional conductor and semi-conductor a lot; Electronics moves the collision that there is not electronics and atom in Graphene, can greatly reduce energy waste; Graphene possesses fabulous light transmission, but airtight, can be used for Development of New Generation protective layer material, and can be used for exploitation transparent electron product and wearable electronic product.The preparation method of graphene product is various, but there are some drawbacks, such as dispersiveness in organic solvent and and polymkeric substance between consistency poor.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of graphene oxide/polyether-type benzoglyoxaline matrix material, to overcome deficiency of the prior art.
For achieving the above object, the invention provides following technical scheme:
The embodiment of the present application discloses the preparation method of a kind of graphene oxide/polyether-type benzoglyoxaline matrix material, comprising:
Adopt the method for exchange of solvent to be dispersed in methyl-sulphoxide by graphene oxide, obtain graphene oxide organic solution;
With 3,3 '-benzidine, 4,4 '-dibenzoic acid ether and PPMA are raw material, 140 ~ 160 DEG C, reaction 1 ~ 3 hour under nitrogen atmosphere, after washing, obtain polyether-type benzoglyoxaline;
Polyether-type benzoglyoxaline is dissolved in graphene oxide organic solution, then evaporating solvent, obtains graphene oxide/polyether-type benzoglyoxaline matrix material.
Preferably, in the preparation method of above-mentioned graphene oxide/polyether-type benzoglyoxaline matrix material, the preparation method of described graphene oxide organic solution comprises:
Get 1 ~ 1.5 parts by weight of graphite powder to mix with the vitriol oil and 2 ~ 3 weight part potassium permanganate as graphite raw material, be placed in closed reaction vessel, stirring reaction 4 ~ 6h under 40 ~ 80 DEG C of condition of water bath heating, through decompression, suction filtration, after washing, by overanxious thing vacuum-drying, grinding, by the product ultrasonic disperse after drying and grinding in deionized water, adding hydrochloric acid regulates PH to be less than 3, add 1 ~ 3 weight part potassium permanganate in 0 ~ 10 DEG C of stirring reaction 4 ~ 6h, add hydrogen peroxide, be warming up to 20 ~ 30 DEG C of stirring in water bath reaction 2 ~ 4h, under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring, remove supernatant liquid, get sediment and add dehydrated alcohol, after stirring, carry out centrifugal settling, get sediment absolute ethanol washing, by sediment drying treatment, be scattered in spraying dry in deionized water and namely obtain graphene oxide,
Add graphene oxide in deionized water, ultrasonic disperse, then add methyl-sulphoxide, stir, underpressure distillation centrifugal treating, obtain graphene oxide organic solution.
Preferably, in the preparation method of above-mentioned graphene oxide/polyether-type benzoglyoxaline matrix material, polyether-type benzoglyoxaline is dissolved in graphene oxide organic solution, and the content of graphene oxide is 0.1 ~ 0.7wt%.
Preferably, in the preparation method of above-mentioned graphene oxide/polyether-type benzoglyoxaline matrix material, polyether-type benzoglyoxaline is dissolved in graphene oxide organic solution, and the content of graphene oxide is 0.35wt%.
Compared with prior art, the invention has the advantages that: adopt exchange of solvent method, can fully be dispersed in organic solution by graphene oxide, preparation is simple.The matrix material obtained has good mechanical property, and thermostability is high, adapts to harsh environment.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present application or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the application, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Figure 1 shows that the section SEM of matrix material in the specific embodiment of the invention schemes.
Embodiment
The present invention is described further by the following example: according to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, concrete material ratio, processing condition and result thereof described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
(1), get 1g Graphite Powder 99 to mix with the 10ml vitriol oil and 3g part potassium permanganate as graphite raw material, be placed in closed reaction vessel, stirring reaction 6h under 40 DEG C of condition of water bath heating, after decompression, suction filtration, washing, by overanxious thing vacuum-drying, grinding.By the product ultrasonic disperse after drying and grinding in 10ml deionized water, adding hydrochloric acid regulates PH to be less than 3, add 1g potassium permanganate in 0 DEG C of stirring reaction 4h, add 5ml hydrogen peroxide, be warming up to 20 DEG C of stirring in water bath reaction 2h, under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring 5min, remove supernatant liquid, repeat to add deionized water and centrifugal process 1 time, get sediment and add dehydrated alcohol, after stirring 5min, carry out centrifugal settling, get after sediment repeats absolute ethanol washing 1 time, by sediment drying treatment, be scattered in spraying dry in deionized water and namely obtain graphene oxide.
(2), in 50ml deionized water add 0.1g graphene oxide, ultrasonic disperse 1 hour, then adds the methyl-sulphoxide of 100ml, stirs, underpressure distillation centrifugal treating, obtains graphene oxide organic solution.
(3), by 3,3 '-benzidine 3mmol, 4,4 '-dibenzoic acid ether 3mmol and PPMA47g mixes, be warming up to 160 DEG C, react 1 hour under nitrogen atmosphere, use sodium hydrogen carbonate solution and deionized water wash respectively, obtain polyether-type benzoglyoxaline.
(4), by polyether-type benzoglyoxaline be dissolved in graphene oxide organic solution, the content of graphene oxide is 0.35wt%, then evaporating solvent, obtains graphene oxide/polyether-type benzoglyoxaline matrix material.
Figure 1 shows that the section SEM of obtained matrix material schemes.As can be seen from the figure, fracture surface roughness is large, graphene uniform ground, is distributed in whole polymkeric substance section in an orderly manner, and Graphene is closely embedded in inside polymeric matrix, illustrates that matrix material has good homogeneity.
Carry out mechanical property detection to matrix material, breaking tenacity and the Young's modulus of matrix material reach 200Mpa and 3.78Gpa respectively.
Embodiment as a comparison, this case changes the content of the graphene oxide in step (4) into 0.1wt%, 0.2wt%, 0.5wt% and 0.7wt% respectively under above-mentioned the same terms, find that its physical strength is obviously weaker than 0.35wt%, breaking tenacity and Young's modulus is the highest only has 165.7Mpa and 3.57Gpa, illustrates that the content of graphene oxide exists outstanding effect at 0.35wt%.
At this, also it should be noted that, in order to avoid the present invention fuzzy because of unnecessary details, illustrate only in the accompanying drawings with according to the closely-related structure of the solution of the present invention and/or treatment step, and eliminate other details little with relation of the present invention.
Finally, also it should be noted that, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, article or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, article or equipment.
Claims (4)
1. a preparation method for graphene oxide/polyether-type benzoglyoxaline matrix material, is characterized in that, comprising:
Adopt the method for exchange of solvent to be dispersed in methyl-sulphoxide by graphene oxide, obtain graphene oxide organic solution;
With 3,3 '-benzidine, 4,4 '-dibenzoic acid ether and PPMA are raw material, 140 ~ 160 DEG C, reaction 1 ~ 3 hour under nitrogen atmosphere, after washing, obtain polyether-type benzoglyoxaline;
Polyether-type benzoglyoxaline is dissolved in graphene oxide organic solution, then evaporating solvent, obtains graphene oxide/polyether-type benzoglyoxaline matrix material.
2. the preparation method of graphene oxide according to claim 1/polyether-type benzoglyoxaline matrix material, is characterized in that: the preparation method of described graphene oxide organic solution comprises:
Get 1 ~ 1.5 parts by weight of graphite powder to mix with the vitriol oil and 2 ~ 3 weight part potassium permanganate as graphite raw material, be placed in closed reaction vessel, stirring reaction 4 ~ 6h under 40 ~ 80 DEG C of condition of water bath heating, through decompression, suction filtration, after washing, by overanxious thing vacuum-drying, grinding, by the product ultrasonic disperse after drying and grinding in deionized water, adding hydrochloric acid regulates PH to be less than 3, add 1 ~ 3 weight part potassium permanganate in 0 ~ 10 DEG C of stirring reaction 4 ~ 6h, add hydrogen peroxide, be warming up to 20 ~ 30 DEG C of stirring in water bath reaction 2 ~ 4h, under room temperature, suspension liquid is carried out centrifugal settling, remove supernatant liquid, add deionized water in sediment and carry out centrifugal settling after stirring, remove supernatant liquid, get sediment and add dehydrated alcohol, after stirring, carry out centrifugal settling, get sediment absolute ethanol washing, by sediment drying treatment, be scattered in spraying dry in deionized water and namely obtain graphene oxide,
Add graphene oxide in deionized water, ultrasonic disperse, then add methyl-sulphoxide, stir, underpressure distillation centrifugal treating, obtain graphene oxide organic solution.
3. the preparation method of graphene oxide according to claim 1/polyether-type benzoglyoxaline matrix material, is characterized in that: polyether-type benzoglyoxaline is dissolved in graphene oxide organic solution, and the content of graphene oxide is 0.1 ~ 0.7wt%.
4. the preparation method of graphene oxide according to claim 3/polyether-type benzoglyoxaline matrix material, is characterized in that: polyether-type benzoglyoxaline is dissolved in graphene oxide organic solution, and the content of graphene oxide is 0.35wt%.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731783A (en) * | 2012-07-13 | 2012-10-17 | 厦门大学 | Polybenzimidazole resin containing pyridine rings and flexible ether bonds and preparation method thereof |
| US20140224124A1 (en) * | 2013-02-12 | 2014-08-14 | Korea Institute Of Science And Technology | Cardo copolybenzimidazoles, gas separation membranes and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731783A (en) * | 2012-07-13 | 2012-10-17 | 厦门大学 | Polybenzimidazole resin containing pyridine rings and flexible ether bonds and preparation method thereof |
| US20140224124A1 (en) * | 2013-02-12 | 2014-08-14 | Korea Institute Of Science And Technology | Cardo copolybenzimidazoles, gas separation membranes and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| NINA I. KOVTYUKHOVA ET AL: "Layer-by-Layer Assembly of Ultrathin Composite Films from Micron-Sized Graphite Oxide Sheets and Polycations", 《CHEMISTRY OF MATERIALS》 * |
| YAN WANG ET AL: "Graphene oxide/polybenzimidazole composites fabricated by a solvent-exchange method", 《CARBON》 * |
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