CN106633863B - With active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption and preparation method thereof - Google Patents

With active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption and preparation method thereof Download PDF

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Publication number
CN106633863B
CN106633863B CN201611016550.8A CN201611016550A CN106633863B CN 106633863 B CN106633863 B CN 106633863B CN 201611016550 A CN201611016550 A CN 201611016550A CN 106633863 B CN106633863 B CN 106633863B
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polyaniline
oil absorption
compound oil
absorption material
active
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CN106633863A (en
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孙剑辉
谭露
董淑英
禹崇菲
王竞侦
陈露
郭淑杰
牛颖
王萌萌
高梦晗
徐苑
张静雯
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Henan Normal University
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Henan Normal University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/32Materials not provided for elsewhere for absorbing liquids to remove pollution, e.g. oil, gasoline, fat
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/02Polyamines

Abstract

The invention discloses one kind to have active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption and preparation method thereof, belongs to the synthesis technical field of aeroge compound oil absorption material.Technical solution of the present invention main points are as follows: graphene oxide and polyaniline are added to the water and ultrasonic disperse uniformly obtains solution A, the solution A is placed in hydrothermal reaction kettle in 150 DEG C of hydro-thermal reactions for 24 hours again, 12h is freezed after taking out sample, freeze-drying 48h in freeze drier is subsequently placed in and obtains with the active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption.The present invention uses one kettle way to prepare the polyaniline with the active 3D network structure of efficient absorption/graphene aerogel compound oil absorption material for the first time, synthesis technology is simple and low in cost, and aeroge compound oil absorption material obtained has the characteristic of efficient absorption oily substance at normal temperature.

Description

With the active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption And preparation method thereof
Technical field
The invention belongs to the synthesis technical fields of aeroge oil absorption material, and in particular to one kind has efficient absorption active 3D polyaniline/graphene aerogel compound oil absorption material and preparation method thereof.
Background technique
Water pollution has seriously threatened the health of the mankind, and in recent years, the method for purifying waste water has very much, including precipitating, biology Degradation, absorption and photocatalytic oxidation degradation etc..But conventional removal effect is often not satisfactory and may cause secondary dirt Dye.For aerogel material since its three-dimensional (3D) structure has good absorption property, most of aeroge has good conduction Property, thermal stability and the physical strength performances such as preferably, can be used for water-oil separating, biomimetic material and electric material etc..3D net The aeroge of shape structure can solve the indeterminable absorption saturation degree of simple adsorbent material now as the nano material of support Problem.Ideal electrode material of the polyaniline (PANI) as supercapacitor has preparation process simple, low in cost, reversible Property it is good, specific capacity is high and can be carried out quickly doping and goes the series of advantages such as doping process, therefore by extensive concern.But by During prolonged charge and discharge cycles its structure easily occur being swollen and Shrinkage behavior, cause its cyclical stability poor, Its further application is limited, compound with carbon-based material is one of the optimal path for alleviating this defect.And as novel carbon materials The graphene of material has good structural stability, strong electric conductivity and bigger serface, it is considered to be for overcoming PANI structure One of instable best carbon material.But it also has good adsorption function, uses stone other than being used as supercapacitor Black alkene has good adsorption function due to its special structure with the compound aeroge compound oil absorption material come out of polyaniline, However the still not no relevant report of this aspect at present.
Summary of the invention
The active with efficient absorption of waste oil can be effectively adsorbed the technical problem to be solved by the present invention is to provide a kind of 3D polyaniline/graphene aerogel compound oil absorption material and preparation method thereof.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, have the active 3D polyaniline of efficient absorption/ The preparation method of graphene aerogel compound oil absorption material, it is characterised in that specific steps are as follows: by graphene oxide and polyaniline It is added to the water and ultrasonic disperse uniformly obtains solution A, wherein the mass ratio of graphene oxide and polyaniline is 6:1-6, then will The solution A is placed in hydrothermal reaction kettle in 150 DEG C of hydro-thermal reactions for 24 hours, is freezed 12h after taking out sample, is subsequently placed in freeze-drying 48h is freeze-dried in machine to obtain with the active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption.
Further preferably, the mass ratio of the graphene oxide and polyaniline is preferably 3:2, and 3D polyaniline obtained/ After graphene aerogel compound oil absorption material adsorbs discarded pumping fluid the weight gain of aeroge compound oil absorption material compare for 5.6 × 103%。
It is of the present invention that there is the active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption, spy Sign is that the above method was prepared.
The invention has the following advantages: prepared using one kettle way has the active 3D network of efficient absorption for the first time The polyaniline of structure/graphene aerogel compound oil absorption material, synthesis technology is simple and low in cost, and aeroge obtained is compound Oil absorption material has the characteristic of efficient absorption oily substance at normal temperature.
Detailed description of the invention
Fig. 1 is the polyaniline of 3D made from the embodiment of the present invention 4/graphene aerogel compound oil absorption material XRD spectrum;
Fig. 2 is the polyaniline of 3D made from the embodiment of the present invention 4/graphene aerogel compound oil absorption material FT-IR map.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair Bright range.
Embodiment 1
0.18g graphene oxide (GO) and 0.03g polyaniline (PANI) are added in 60mL water and ultrasonic disperse is uniform Solution A is obtained, then the solution A is placed in hydrothermal reaction kettle in 150 DEG C of hydro-thermal reactions for 24 hours, freezes 12h after taking out sample, so Be placed in freeze drier be freeze-dried 48h obtain it is compound with the active 3D polyaniline/graphene aerogel of efficient absorption Oil absorption material (GOP).By the adsorption test to discarded pumping fluid, the mass weight gain of the aeroge compound oil absorption material is found Than being 1.7 × 103%。
Embodiment 2
0.18g graphene oxide (GO) and 0.06g polyaniline (PANI) are added in 60mL water and ultrasonic disperse is uniform Solution A is obtained, then the solution A is placed in hydrothermal reaction kettle in 150 DEG C of hydro-thermal reactions for 24 hours, freezes 12h after taking out sample, so Be placed in freeze drier be freeze-dried 48h obtain it is compound with the active 3D polyaniline/graphene aerogel of efficient absorption Oil absorption material (GOP).By the adsorption test to discarded pumping fluid, the mass weight gain of the aeroge compound oil absorption material is found Than being 2.2 × 103%。
Embodiment 3
0.18g graphene oxide (GO) and 0.09g polyaniline (PANI) are added in 60mL water and ultrasonic disperse is uniform Solution A is obtained, then the solution A is placed in hydrothermal reaction kettle in 150 DEG C of hydro-thermal reactions for 24 hours, freezes 12h after taking out sample, so Be placed in freeze drier be freeze-dried 48h obtain it is compound with the active 3D polyaniline/graphene aerogel of efficient absorption Oil absorption material (GOP).By the adsorption test to discarded pumping fluid, the mass weight gain of the aeroge compound oil absorption material is found Than being 3.8 × 103%。
Embodiment 4
0.18g graphene oxide (GO) and 0.12g polyaniline (PANI) are added in 60mL water and ultrasonic disperse is uniform Solution A is obtained, then the solution A is placed in hydrothermal reaction kettle in 150 DEG C of hydro-thermal reactions for 24 hours, freezes 12h after taking out sample, so Be placed in freeze drier be freeze-dried 48h obtain it is compound with the active 3D polyaniline/graphene aerogel of efficient absorption Oil absorption material (GOP).By the adsorption test to discarded pumping fluid, the mass weight gain of the aeroge compound oil absorption material is found Than being 5.6 × 103%。
Fig. 1 is the polyaniline of 3D made from the present embodiment/graphene aerogel compound oil absorption material XRD spectrum, can by figure Know, RGO has a wide diffraction maximum in 2 θ=26o, is the standard diffraction peak of graphene.The XRD spectrum of GOP illustrates that polyaniline is multiple It has a certain impact after closing reduced graphene to the crystal form of graphene, reduces the diffraction maximum of graphene and polyaniline occur Crystal form.
Fig. 2 is the polyaniline of 3D made from the present embodiment/graphene aerogel compound oil absorption material FT-IR map, by scheming It is found that the part oxygen-containing functional group of graphene oxide is reduced, polyphenyl amine content is less, and diffraction maximum is overlapped with graphene, because This, GOP infared spectrum is compared with RGO infared spectrum, no significant difference.
Embodiment 5
0.18g graphene oxide (GO) and 0.15g polyaniline (PANI) are added in 60mL water and ultrasonic disperse is uniform Solution A is obtained, then the solution A is placed in hydrothermal reaction kettle in 150 DEG C of hydro-thermal reactions for 24 hours, freezes 12h after taking out sample, so Be placed in freeze drier be freeze-dried 48h obtain it is compound with the active 3D polyaniline/graphene aerogel of efficient absorption Oil absorption material (GOP).By the adsorption test to discarded pumping fluid, the mass weight gain of the aeroge compound oil absorption material is found Than being 4.8 × 103%。
Embodiment 6
0.18g graphene oxide (GO) and 0.18g polyaniline (PANI) are added in 60mL water and ultrasonic disperse is uniform Solution A is obtained, then the solution A is placed in hydrothermal reaction kettle in 150 DEG C of hydro-thermal reactions for 24 hours, freezes 12h after taking out sample, so Be placed in freeze drier be freeze-dried 48h obtain it is compound with the active 3D polyaniline/graphene aerogel of efficient absorption Oil absorption material (GOP).By the adsorption test to discarded pumping fluid, the mass weight gain of the aeroge compound oil absorption material is found Than being 4.4 × 103%。
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within In the scope of protection of the invention.

Claims (3)

1. the preparation method with the active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption, feature exist In specific steps are as follows: graphene oxide and polyaniline are added to the water and ultrasonic disperse uniformly obtains solution A, wherein aoxidizing stone The mass ratio of black alkene and polyaniline is 6:1-6, then the solution A is placed in hydrothermal reaction kettle in 150 DEG C of hydro-thermal reactions for 24 hours, is taken 12h is freezed after sample out, freeze-drying 48h in freeze drier is subsequently placed in and obtains with the active 3D polyphenyl of efficient absorption Amine/graphene aerogel compound oil absorption material.
2. according to claim 1 have the active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption Preparation method, it is characterised in that: the mass ratio of the graphene oxide and polyaniline is preferably 3:2,3D polyphenyl obtained The weight gain of aeroge compound oil absorption material, which is compared, after amine/graphene aerogel compound oil absorption material adsorbs discarded pumping fluid is 5.6×103%。
3. one kind have the active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption, it is characterised in that be by What method of any of claims 1 or 2 was prepared.
CN201611016550.8A 2016-11-18 2016-11-18 With active 3D polyaniline/graphene aerogel compound oil absorption material of efficient absorption and preparation method thereof Active CN106633863B (en)

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CN108530889B (en) * 2017-08-30 2020-10-13 北京化工大学 MXene/conductive polymer composite aerogel and preparation method thereof
CN109126868A (en) * 2018-08-01 2019-01-04 河南师范大学 A kind of g-C for terramycin wastewater of degrading3N4The preparation method of-PANI composite photocatalyst material
CN108997576B (en) * 2018-08-10 2020-11-17 西安工业大学 Covalent bond combined polyaniline nanorod-graphene aerogel wave-absorbing material and preparation method thereof
CN110358137B (en) * 2019-07-16 2022-03-04 沈阳大学 Preparation method of graphene/polyaniline composite xerogel with porous network structure
CN110711564B (en) * 2019-09-23 2021-06-22 济南大学 Preparation and application of polyaniline/silicon dioxide/graphene oxide aerogel composite material
CN113416414B (en) * 2021-07-30 2022-04-22 湖南大学 Preparation method and application of aramid nanofiber/porous graphene/polyaniline composition, hydrogel and film with high mechanical strength

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CN104559176A (en) * 2015-01-27 2015-04-29 西南科技大学 Preparation method of three-dimensional reduced graphene oxide/polyaniline composite material
CN104658764A (en) * 2015-02-06 2015-05-27 浙江大学 Graphene aerogel three-component compound electrode material of supercapacitor as well as preparation and application
CN104998589A (en) * 2015-05-21 2015-10-28 西南石油大学 Preparation method for efficient oil absorption carbon aerogel material
CN106046401A (en) * 2016-07-07 2016-10-26 北京化工大学 Preparation method of graphene polyaniline aerogel thermoelectric material

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CN104559176A (en) * 2015-01-27 2015-04-29 西南科技大学 Preparation method of three-dimensional reduced graphene oxide/polyaniline composite material
CN104658764A (en) * 2015-02-06 2015-05-27 浙江大学 Graphene aerogel three-component compound electrode material of supercapacitor as well as preparation and application
CN104998589A (en) * 2015-05-21 2015-10-28 西南石油大学 Preparation method for efficient oil absorption carbon aerogel material
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