CN104971703A - Preparation method of polypyrrole coated magnetic reduced graphene nanometer material - Google Patents

Preparation method of polypyrrole coated magnetic reduced graphene nanometer material Download PDF

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Publication number
CN104971703A
CN104971703A CN201510344900.2A CN201510344900A CN104971703A CN 104971703 A CN104971703 A CN 104971703A CN 201510344900 A CN201510344900 A CN 201510344900A CN 104971703 A CN104971703 A CN 104971703A
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rgo
nano material
preparation
solution
naoh
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唐祝兴
彭剑
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Shenyang Ligong University
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Shenyang Ligong University
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Abstract

The invention relates to a preparation method of a polypyrrole coated magnetic reduced graphene nanometer material. The preparation method comprises the following steps: firstly, manufacturing a mixed solution of oxidized graphene, ferrous sulfate, sodium hydroxide and ammonia water, and reacting in a polytetrafluoroethylene reaction kettle, washing the product, and drying to obtain a Fe3O4/RGO nanometer material; and secondly, dispersing the Fe3O4/RGO nanometer material prepared in the first step in deionized water, then adding pyrrole (PY) monomers, mechanically stirring for 30 min in an ice-water bath, adding sodium persulfate solid (APS) after the pyrrole monomers are completely dispersed, continuing to mechanically stir for 30 min in the ice-water bath until the solution gradually becomes clear from muddy through observation, finally washing the product, and drying to obtain a PPY/Fe3O4/RGO material. The method is simple in operation, the particles are uniform, the dispersion is good, and the adsorption capacity is high. The manufacturing process is environment-friendly and free of pollution.

Description

A kind of preparation method of polypyrrole coated magnetic reduced graphene nano material
                                
Technical field
The invention belongs to the preparation method field of magnetic nanometer composite material, particularly a kind of polypyrrole coated magnetic reduced graphene nano material (PPY/Fe 3o 4/ RGO) preparation method.
Background technology
The synthetic method of magnetic Nano material can be divided into physical method and chemical method two class, the former comprises organic polishing, the organic thermal decomposition method of metal, electrolysis, vacuum vapour deposition, and the latter is mainly divided into solvent-thermal method, coprecipitation, microemulsion method, sol-gel process etc.But the magnetic nano-particle size distribution adopting physical method obtained is wider, and be not suitable for the relatively high field application of the particle size scale requirement such as Chemical Decomposition, biology, medical science, the general chemical method that adopts prepares magnetic Nano material.
(1) solvent-thermal method
Solvent-thermal method is referred to as hydrothermal method again, belongs to the category of liquid phase chemical.The method prepares the method for nano material in water or other hot solvent under referring to high pressure-temperature.At present, existing much about employing water heat transfer Fe 3o 4the report of nano particle and superfines.The particle that solvent-thermal method is prepared seldom is reunited, product particle size size distribution all hooks, crystalline form has the complete advantage of growth, and hydro-thermal reaction raw material is also relatively more cheap, and production cost is lower.
(2) coprecipitation
Coprecipitation is the most economical method preparing nanoscale magnetic bead, refers to use Fe under room temperature or high temperature inert gas protection 2+and Fe 3+salt in the basic conditions mix and blend obtains superparamagnetism Fe 3o 4the method of crystal settling.
This method is simple to operate, economical, be easy to industrialization, but the dimensional controllability of the magnetic nanoparticle prepared and homogeneity poor, to be improved.
(3) microemulsion method
Microemulsion refers to two kinds of originally immiscible liquid, under Action of Surfactant, and the Thermodynamically stable of formation, isotropism, appearance transparent or translucent " oil-in-water " dispersion.Adopt micro-emulsion method for preparing nano Fe 30 4, each micro emulsion drop can regard a microreactor as, has the protection of micro emulsion drop just can effectively avoid reuniting, thus can obtain the spherical nanostructure of morphology controllable, uniform particle diameter between particle.
Although microemulsion method can control the pattern of magnetic nano-particle effectively, lower with the productive rate of the method synthesizing nano-particle, and need synthetic, the synthetic material of higher cost, and be not suitable for actual production.
(4) sol-gel process
Sol-gel process refers to the organic or inorganic salt of iron for raw material, through the first obtained colloidal sol of the chemical reactions such as hydrolysis and polycondensation under saturation conditions, then is converted into gel, then obtains the method for oxide or solid chemical compound through heating or freeze drying calcining.
Summary of the invention
The object of this invention is to provide a kind of preparation method of polypyrrole coated magnetic reduced graphene nano material, the coated nanometer Fe of polypyrrole can be prepared by this method 30 4ball is attached to the nano composite material of stratiform reduced graphene.
The technical scheme adopted is:
A kind of polypyrrole coated magnetic reduced graphene nano material (PPY/Fe 3o 4/ RGO) preparation method, comprise the following steps:
One, Fe 3o 4the preparation of/RGO nano material
1.1, the graphene oxide (GO) taking 0.08g is dispersed in the distilled water of 30ml, carries out the ultrasonic of 1h, makes Graphene completely soluble in water.
1.2, the FeSO of 1.39g is successively taken 47H 2o is dissolved in the water of 20ml, and the NaOH of 0.4g is dissolved in the water of 5ml, is added in the graphene solution of 1.1 successively, and obtained mass ratio is GO:FeSO 47H 2the aqueous solution of O:NaOH=1:17.375:5, carries out the magnetic agitation of 1h.
1.3, the N of 20ml is measured 2h 4h 2o solution is (containing N 2h 4h 2the quality of O is 16g) add in above-mentioned 1.2 solution, obtained mass ratio is GO:FeSO 47H 2o:NaOH:N 2h 4h 2the solution of O=1:17.375:5:200, is transferred to its mixed solution in polytetrafluoroethylene (PTFE) reactor, temperature 180 DEG C of isothermal reaction 8h.
1.4, reaction is cooled to room temperature after terminating, and by the product distilled water ultrasonic cleaning be separated with magnet, then with EtOH Sonicate cleaning, the alternately cleaning step repeating above distilled water and EtOH Sonicate cleaning repeatedly, obtains Fe 3o 4/ RGO nano material.
1.5, by Fe 3o 4/ RGO nano material puts into baking oven, and 60 DEG C of condition 6 h are dried, and obtains dry Fe 3o 4/ RGO nano material, Fe 3o 4the diameter of nano particle is 20-50 nanometer, is spherical shape.
Two, polypyrrole coated magnetic reduced graphene nano material (PPY/Fe 3o 4/ RGO) preparation.
2.1, the Fe of 10mg is taken 3o 4/ RGO nano material is dispersed in the water of 40ml, ultrasonic 30min, makes it soluble in water.
2.2, measure 0.104ml(100mg) pyrrole monomer (PY) be dissolved in the solution of 2.1, mechanical agitation 30min in ice-water bath, makes it mix completely.
2.3, the ammonium persulfate (APS) taking 0.34g is dissolved in 10ml distilled water, is added in the solution of 2.2, and finally obtaining mass ratio is Fe 3o 4the solution of/RGO:PY:APS=1:10:34, mechanical agitation 30min in ice-water bath, solution becomes muddy by clarification gradually.
2.4, after reaction terminates, the mixture obtained with distilled water and ethanol alternate repetition cleaning 2.3 3 times, then suction filtration is carried out to it, the material obtained is put into baking oven, and under 60 DEG C of conditions, 6h is dried, and obtains dry PPY/Fe 3o 4/ RGO nano material.
Its advantage is:
The present invention is simple to operate, and cost is low, prepared PPY/Fe 3o 4/ RGO magnetic Nano material particle diameter is in Nano grade, uniform particles, good dispersion, high adsorption capacity.Can not environmental pollution be caused when preparation, harmless to the health of operating personnel.
Detailed description of the invention
A kind of polypyrrole coated magnetic reduced graphene nano material (PPY/Fe 3o 4/ RGO) preparation method, comprise the following steps:
One, Fe 3o 4the preparation of/RGO nano material.
1.1, take the graphene oxide (GO) of 0.08g in the beaker of 250ml drying, the distilled water getting 30ml with graduated cylinder adds in beaker, carries out ultrasonic (electric power is the ultrasonic cleaner of 150W) of 1h, makes Graphene completely soluble in water.
1.2, the FeSO of 1.39g is successively taken 47H 2o is dissolved in the water of 20ml, and the NaOH of 0.4g is dissolved in the water of 5ml, is added in the graphene solution of 1.1 successively, and obtained mass ratio is GO:FeSO 47H 2the aqueous solution of O:NaOH=1:17.375:5, carries out the magnetic agitation (rotating speed is 200rpm) of 1h.
1.3, the N of 20ml is measured 2h 4h 2o solution is (containing N 2h 4h 2the quality of O is 16g) add in above-mentioned 1.2 solution, obtained mass ratio is GO:FeSO 47H 2o:NaOH:N 2h 4h 2the solution of O=1:17.375:5:200, is transferred to its mixed solution in polytetrafluoroethylene (PTFE) reactor, temperature 180 DEG C of isothermal reaction 8h.
1.4, reaction is cooled to room temperature after terminating, and by the product distilled water ultrasonic cleaning is separated with magnet, then with EtOH Sonicate cleaning, that repeats that above distilled water and EtOH Sonicate clean replaces cleaning step 3-6 time, obtains Fe 3o 4/ RGO nano material.
1.5, by Fe 3o 4/ RGO nano material puts into baking oven, and 60 DEG C of condition 6 h are dried, and obtains dry Fe 3o 4/ RGO nano material, Fe 3o 4the diameter of nano particle is 20-50 nanometer, is spherical shape.
Two, polypyrrole coated magnetic reduced graphene nano material (PPY/Fe 3o 4/ RGO) preparation.
2.1, the Fe of 10mg is taken 3o 4/ RGO nano material is dispersed in the water of 40ml, ultrasonic 30min, makes it soluble in water.
2.2, measure 0.104ml(100mg) pyrrole monomer (PY) be dissolved in the solution of 2.1, in ice-water bath, mechanical agitation 30min(rotating speed is 200rpm), make it mix completely.
2.3, the ammonium persulfate (APS) taking 0.34g is dissolved in 10ml distilled water, is added in the solution of 2.2, and finally obtaining mass ratio is Fe 3o 4the solution of/RGO:PY:APS=1:10:34, mechanical agitation 30min in ice-water bath (0-4 DEG C), solution becomes muddy by clarification gradually.
2.4, after reaction terminates, the mixture obtained with distilled water and ethanol alternate repetition cleaning 2.3 3 times, then suction filtration is carried out to it, the material obtained is put into baking oven, and under 60 DEG C of conditions, 6h is dried, and obtains dry PPY/Fe 3o 4/ RGO nano material.

Claims (2)

1. a polypyrrole coated magnetic reduced graphene nano material (PPY/Fe 3o 4/ RGO) preparation method, it is characterized in that comprising the following steps:
One, Fe 3o 4the preparation of/RGO nano material
1.1, be GO:FeSO according to mass ratio 47H 2the ratio of O:NaOH=1:17.375:5 gets GO, FeSO 47H 2o, NaOH powder, preparation GO, FeSO47H 2the mixed solution of O, NaOH;
1.2, the mixed solution using the continuous magnetic agitation of magnetic stirring apparatus above-mentioned 1.1 to obtain, rotating speed is 200rpm, 1 hour time;
1.3, measure the N of certain content 2h 4h 2o solution adds in above-mentioned 1.2 solution, and obtained mass ratio is GO:FeSO 47H 2o:NaOH:N 2h 4h 2the solution of O=1:17.375:5:200, is transferred to its mixed solution in polytetrafluoroethylene (PTFE) reactor, temperature 180 DEG C of isothermal reaction 8h;
1.4, reaction is cooled to room temperature after terminating, and by the product distilled water ultrasonic cleaning is separated with magnet, then with EtOH Sonicate cleaning, that repeats that above distilled water and EtOH Sonicate clean replaces cleaning step 3-6 time, obtains Fe 3o 4/ RGO nano material;
1.5, by Fe 3o 4/ RGO nano material puts into baking oven, and 60 DEG C of condition 6 h are dried, and obtains dry Fe 3o 4/ RGO nano material, Fe 3o 4the diameter of nano particle is 20-50 nanometer, is spherical shape;
Two, polypyrrole coated magnetic reduced graphene nano material (PPY/Fe 3o 4/ RGO) preparation
2.1, be Fe according to mass ratio 3o 4the Fe that the first step is prepared by the ratio of/RGO:PY:APS=1:10:34 3o 4/ RGO nano material is scattered in deionized water, then add pyrrole monomer (PY), mechanical agitation 30min in ice-water bath, after it disperses completely, add sodium peroxydisulfate solid (APS), continue mechanical agitation 30min in ice-water bath, finally can observe solution and become muddy by clarification gradually;
2.2, after reaction terminates, the mixture obtained with distilled water and ethanol alternate repetition cleaning 2.1 3 times, then suction filtration is carried out to it, the material obtained is put into baking oven, and under 60 DEG C of conditions, 6h is dried, and obtains dry PPY/Fe 3o 4/ RGO nano material.
2. the preparation method of polypyrrole coated magnetic reduced graphene nano material according to claim 1, is characterized in that:
In the described first step, graphene oxide (GO) is 0.08 g, FeSO 47H 2o quality is that 1.39g, NaOH quality is for being 0.4 g, N 2h 4h 2o solution is 20ml;
Fe in described second step 3o 4/ RGO nano material is 10mg, and pyrrole monomer (PY) is 0.104ml(100mg), ammonium persulfate (APS) quality is 0.34g.
CN201510344900.2A 2015-06-23 2015-06-23 Preparation method of polypyrrole coated magnetic reduced graphene nanometer material Pending CN104971703A (en)

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Publication number Priority date Publication date Assignee Title
CN106479349A (en) * 2016-11-10 2017-03-08 无锡市明盛强力风机有限公司 A kind of electromagnetic screen coating
CN107519846A (en) * 2017-07-31 2017-12-29 华南理工大学 A kind of graphene/silicon dioxide Pt/Polypyrrole composite material and preparation method and application
CN108201883A (en) * 2018-03-12 2018-06-26 中国科学院合肥物质科学研究院 It is a kind of for magnetic Nano material of hexavalent chromium and preparation method thereof in water body of degrading
CN111087627A (en) * 2019-12-27 2020-05-01 太原理工大学 Composite hydrogel and preparation method and application thereof
CN111220743A (en) * 2019-10-28 2020-06-02 中国计量科学研究院 Application of MrGOPA composite adsorbent in pesticide residue detection and pesticide residue detection method

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CN104190385A (en) * 2014-08-29 2014-12-10 湖南大学 Polypyrrole/Fe3O4/graphene composite material, and preparation method and application thereof
CN104694072A (en) * 2015-01-12 2015-06-10 冯云 Composite mesoporous material

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106479349A (en) * 2016-11-10 2017-03-08 无锡市明盛强力风机有限公司 A kind of electromagnetic screen coating
CN107519846A (en) * 2017-07-31 2017-12-29 华南理工大学 A kind of graphene/silicon dioxide Pt/Polypyrrole composite material and preparation method and application
CN108201883A (en) * 2018-03-12 2018-06-26 中国科学院合肥物质科学研究院 It is a kind of for magnetic Nano material of hexavalent chromium and preparation method thereof in water body of degrading
CN111220743A (en) * 2019-10-28 2020-06-02 中国计量科学研究院 Application of MrGOPA composite adsorbent in pesticide residue detection and pesticide residue detection method
CN111220743B (en) * 2019-10-28 2021-06-08 中国计量科学研究院 Application of MrGOPA composite adsorbent in pesticide residue detection and pesticide residue detection method
CN111087627A (en) * 2019-12-27 2020-05-01 太原理工大学 Composite hydrogel and preparation method and application thereof

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