CN104689798A - Method for preparing composite mesoporous material - Google Patents

Method for preparing composite mesoporous material Download PDF

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CN104689798A
CN104689798A CN201510016052.2A CN201510016052A CN104689798A CN 104689798 A CN104689798 A CN 104689798A CN 201510016052 A CN201510016052 A CN 201510016052A CN 104689798 A CN104689798 A CN 104689798A
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graphite
insulation
mass ratio
warming
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冯云
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Abstract

The invention discloses a method for preparing a composite mesoporous material. The method comprises the steps of preparing graphite oxide, loading hollow FeO4 nanoparticles to the surfaces of graphene flake layers by a solvothermal method, then, coating the surfaces of the hollow nano Fe3O4 loaded graphene flake layers with polyaniline so as to prepare a graphene/hollow Fe3O4/polyaniline nano composite material, and finally, carrying out high-temperature carbonizing treatment, thereby preparing the mesoporous material. The method disclosed by the invention is convenient and fast, and the material can serve as an electromagnetic wave absorbing material and can also be used as an environmental adsorption material.

Description

A kind of preparation method of complex mesoporous material
Technical field
The present invention relates to absorbing material field, in particular a kind of preparation method of complex mesoporous material.
Background technology
Along with science and technology and the development of electronics industry, increasing electromagenetic wave radiation is present in around us, show through research, excessive electromagenetic wave radiation occurs, except obstacle, even may bring out the serious disease comprising all kinds of cancer except causing nervous system, immune system, reproductive system and blood circulation system etc.Be in for a long time in electromagnetic wave environment, damaged by electromagnetic wave in human body and the damage of the tissue of the self-regeneration that is not able to do in time and organ can become dynamic disease becomes because of long term accumulation, can threat to life time serious.
Graphene, the single layer structure due to its uniqueness makes it have the features such as ultralight density, large specific area, dielectric constant that electric conductivity is excellent and high, becomes a kind of novel wave-absorbing material.In addition, the chemical bond that oxidized graphenic surface exposes in a large number more easily produces the dielectric relaxor of outer-shell electron and attenuates electromagnetic waves under the effect of electromagnetic field, for Graphene is inhaling the applications expanding prospect in ripple field, at the hollow ferriferrous oxide nano-particle of graphenic surface carried magnetic, not only can improve magnetism of material energy, the magnetic loss of reinforced composite, be conducive to the impedance matching of composite, and ferriferrous oxide particles is again stacking in three-dimensional graphite structure in dry run as spacer medium minimizing Graphene, considerable effect is played to stable graphene film Rotating fields.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, provides a kind of preparation method of complex mesoporous material.
Technical scheme of the present invention is as follows:
A preparation method for complex mesoporous material, is characterized in that, its step is as follows:
Step one, the preparation of pre-oxidation graphite
By graphite powder, potassium peroxydisulfate and P 2o 5add in the concentrated sulfuric acid, form mixture, the pH value of the mixture formed is 1.5, and this mixture is stirred 1-2h at 60 DEG C, then 2-4h is stirred with at the ramp to 80 of 5 DEG C/min DEG C, finally be warming up to 87 DEG C with 2 DEG C/min and stir 1-2h, then adopt this mixture of distilled water diluting, the pH value of this mixture is diluted to 3.6, distilled water is adopted to filter after placing 36h, make mixture pH value be 6-7, after carry out drying at room temperature, described graphite powder, potassium peroxydisulfate, P 2o 5be 1-3: 1-2: 1-2: 5-10 with the mass ratio of the concentrated sulfuric acid;
Joined in red fuming nitric acid (RFNA) by dried mixture and stir 45-60min, make pH value be 2-4, the mass ratio of described dried mixture and red fuming nitric acid (RFNA) is 1-4: 50-100, and after stirring, at-8 DEG C, first time adds KMnO 4, stir 30min, at being cooled to-12 DEG C afterwards, second time adds KMnO 4, stir 30min, at being finally cooled to-15 DEG C, third time adds KMnO 4, stir 20min, obtain the graphite mixture of pre-oxidation, described first time adds KMnO 4, second time adds KMnO 4kMnO is added with third time 4mass ratio be 1: 2: 3, described dried mixture and total KMnO 4ratio be 1-2: 10-15.
Step 2, the preparation of surface-treated graphite oxide
The graphite mixture of pre-oxidation made for step one is put into incubator and is warmed up to 40 DEG C, reaction 3h, subsequently, add the first distilled water with the consistent amount of graphite mixture volume of pre-oxidation, then react 2.5h, by incubator temperature to 40 DEG C, again add after-fractionating water and H 2o 2reaction 10-60min, the amount of described after-fractionating water is 1-1.5 times of the first distilled water, after-fractionating water and H 2o 2volume ratio be 4-20: 1, reaction terminate after carry out centrifugation 10min, rotating speed 9500r/min, centrifugation afterproduct hydrochloric acid solution washs, the volume of this hydrochloric acid solution is 10-50 times of centrifugation afterproduct volume, and finally dialysis obtains graphite oxide in 7-8 days
Graphite oxide is put into purification liquid and obtains mixing material, carry out shaking dispersion and filter obtain purify after graphite oxide, described purification liquid is due to the concentrated sulfuric acid of 1.72g/ml and H 2o 2composition, the concentrated sulfuric acid and H 2o 2mass ratio be 1-2: 2-5;
Add N-hydroxysuccinimide after graphite oxide after purification is adopted methyl-sulfoxide ultrasonic dissolution and make surface conditioning agent by oneself and stir 2h at 35 DEG C, product carries out suction filtration, washing, oven dry, namely obtains surface-treated graphite oxide;
Step 3, dispersion
The ethylene glycol that the mixture (mass ratio of polymethylacrylic acid and polyacrylamide is 1: 1) be made up of polymethylacrylic acid and polyacrylamide with 1-10g PEO-PPOX-PEO triblock copolymer and 1g after surface-treated graphite oxide 1-2g step 2 obtained carries out lyophilization at-10-30 DEG C puts into 500ml in the lump carries out ultrasonic disperse, and then under ultraviolet irradiation, radiation 36h forms uniform first dispersion liquid;
Simultaneously by 4-15g by Fecl 36H 2o, Fecl 24H 2the mixture of O and acetyl acetone iron composition, 6 ~ 25g polyvinylpyrrolidone and 10 ~ 50g NH 4ac is dissolved in the ethylene glycol of 500-1000mL and forms the second dispersion liquid, by the first dispersion liquid and the second dispersion liquid mix and blend, and regulates with ammoniacal liquor, makes it to become the settled solution that pH value is 8-10, described Fecl 36H 2o, Fecl 24H 2the mass ratio of O and acetyl acetone iron is 1: 1: 0.5;
Step 4, the settled solution that 100ml step 3 obtains is put into reactor, after sealing, be heated to 150 DEG C, insulation 2h, 200 DEG C are warming up to afterwards with the heating rate of 2-4 DEG C/min, insulation 4h, 235 DEG C are warming up to afterwards with the heating rate of 3-6 DEG C/min, insulation 3h, then 200 DEG C of insulation 2h are cooled to the cooling rate of 5-7 DEG C/min, finally be warming up to 235 DEG C with the heating rate of 3-6 DEG C/min again, insulation 7h, after question response completes, reactor is taken out, make it cool to room temperature, described cooling rate is 3-6 DEG C/min, by the black powder centrifugation 10min of gained, rotating speed 8000 ~ 10000r/min, absolute ethyl alcohol and deionized water is adopted respectively to wash three times, at 50 ~ 70 DEG C of vacuum drying 24h, obtain the first product,
Be added in the solution of DBSA by 5g first product and 5-10g aniline monomer, ultrasonic disperse 65min, form the second product, the mass ratio of described first product and DBSA is 1-1.5: 8-15;
3g ammonium persulfate is dissolved in 80-120ml distilled water, slowly be added drop-wise in the second product, stirring reaction 15h, after reaction terminates, suction filtration, use distilled water, ethanol washed product colourless to filtrate respectively, 50 ~ 70 DEG C of vacuum drying 24 ~ 36h, obtain Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material;
Step 5, by Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material obtained in step 4, being positioned over place mat has in the ceramic crucible of potassium permanganate, and be placed in Muffle furnace and sinter, first 300 DEG C are warming up to the heating rate of 10 DEG C/min, insulation 30min, 600 DEG C are warming up to again with the heating rate of 12 DEG C/min, insulation 30min, then 500 DEG C are cooled to the rate of temperature fall of 15 DEG C/min, insulation 20min, finally be warming up to 950 DEG C of insulation 1-3h with the heating rate of 15 DEG C/min, obtain mesoporous material, the mass ratio of described Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material and potassium permanganate is 1: 3-5.
The particle diameter of described graphite powder is 15-30um.
The ratio of the g of graphite oxide described in step 2, methyl-sulfoxide ml, N-hydroxysuccinimide g and self-control surface conditioning agent g is 0.2-0.5: 20-25: 2-5: 0.1-05, described self-control surface conditioning agent is made up of dicyclohexylcarbodiimide, dodecyl sodium sulfate, kayexalate and polyacrylic acid, and described dicyclohexylcarbodiimide, dodecyl sodium sulfate, kayexalate and polyacrylic mass ratio are 1: 1: 2: 3.
In described described step 2, the concentration of hydrochloric acid is the hydrochloric acid solution of volume ratio 1: 10.
Described Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material is laminar nano composite wave-suction material, the ferroferric oxide nano granules homoepitaxial of hollow hemisphere structure is on two surfaces up and down of redox graphene sheet, the absorbing material of the multi-layer compound structure of a kind of nano thickness formed, on graphene sheet layer, load particle diameter is about hollow four iron oxide three particles of 20-50nm, and polyaniline-coated has the graphene sheet layer surface of hollow nano ferriferrous oxide in load.
The preparation method of absorbing material of the present invention is by the growth in situ of tri-iron tetroxide on graphene sheet layer and the in-situ polymerization of polyaniline on Graphene/ferriferrous oxide composite material surface, thus realize the wave-absorbing effect of material excellence, be 4.8-5.1GHz at the Absorber Bandwidth of below reflection loss-10dB;
The hole dimension of described mesoporous material is 5-30nm, and the suction ripple within the scope of 1-20Hz is-35-55dB.Have higher electrical conductivity, absorbing property within the scope of 1-20Hz is excellent, can be used for electromagnetic-wave absorbent, also can as environment adsorbing materials, for adsorbing the pollutants such as heavy metal in environment.The electric capacity of this mesoporous material under the current density of 200mA/g is 435-458F/g.
Applicant prepares pre-oxidation graphite through large quantity research step one of the present invention and adopts different heating rates to be warming up to required whipping temp, stirring stage by stage under different whipping temps, and adds KMnO at different temperature stage by stage 4contribute to the preparation of pre-oxidation graphite, make oxidation more thoroughly be higher than common disposable stirring and add KMnO 410-15%, and be conducive to the formation of later stage Graphene;
In step 2, further purification and surface treatment are done for graphite oxide, the purity adopting homemade purification liquid effectively can promote graphite reduces impurity, adopt homemade surface conditioning agent, the surperficial shortcoming low for metallic iron ion affinity of graphite oxide can be made up after adding, increase the load capacity of surperficial Fe ion, also make Fe ion below more even in the dispersion of graphite surface, the specific area of its graphite reaches 35-37m simultaneously 2/ g;
Dispersion effect in step 3 is good, and stability is high, is conducive to next step operation and the combination with iron ion;
During adopting different heating rates to be warming up to required temperature in step 4 of the present invention, through insulation of once lowering the temperature, more contribute to the formation of Graphene/hollow tri-iron tetroxide, make the absorbing property of the final absorbing material formed stronger, be better than the performance 5-15% of the absorbing material that commonsense method is formed, and the tri compound absorbing material performance formed is more stable;
The present invention without the need to using nitrogen or oxygen protection, without the need to hot conditions, can effectively reduce synthesis cost, and effectively raising the dispersing uniformity of nano particle in graphite, improve the performance of product in preparation process.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
A preparation method for complex mesoporous material, is characterized in that, its step is as follows:
Step one, the preparation of pre-oxidation graphite
By graphite powder, potassium peroxydisulfate and P 2o 5add in the concentrated sulfuric acid, form mixture, the pH value of the mixture formed is 1.5, and this mixture is stirred 1-2h at 60 DEG C, then 2-4h is stirred with at the ramp to 80 of 5 DEG C/min DEG C, finally be warming up to 87 DEG C with 2 DEG C/min and stir 1-2h, then adopt this mixture of distilled water diluting, the pH value of this mixture is diluted to 3.6, distilled water is adopted to filter after placing 36h, make mixture pH value be 6-7, after carry out drying at room temperature, described graphite powder, potassium peroxydisulfate, P 2o 5be 1-3: 1-2: 1-2: 5-10 with the mass ratio of the concentrated sulfuric acid;
Joined in red fuming nitric acid (RFNA) by dried mixture and stir 45-60min, make pH value be 2-4, the mass ratio of described dried mixture and red fuming nitric acid (RFNA) is 1-4: 50-100, and after stirring, at-8 DEG C, first time adds KMnO 4, stir 30min, at being cooled to-12 DEG C afterwards, second time adds KMnO 4, stir 30min, at being finally cooled to-15 DEG C, third time adds KMnO 4, stir 20min, obtain the graphite mixture of pre-oxidation, described first time adds KMnO 4, second time adds KMnO 4kMnO is added with third time 4mass ratio be 1: 2: 3, described dried mixture and total KMnO 4ratio be 1-2: 10-15.
Step 2, the preparation of surface-treated graphite oxide
The graphite mixture of pre-oxidation made for step one is put into incubator and is warmed up to 40 DEG C, reaction 3h, subsequently, add the first distilled water with the consistent amount of graphite mixture volume of pre-oxidation, then react 2.5h, by incubator temperature to 40 DEG C, again add after-fractionating water and H 2o 2reaction 10-60min, the amount of described after-fractionating water is 1-1.5 times of the first distilled water, after-fractionating water and H 2o 2volume ratio be 4-20: 1, reaction terminate after carry out centrifugation 10min, rotating speed 9500r/min, centrifugation afterproduct hydrochloric acid solution washs, the volume of this hydrochloric acid solution is 10-50 times of centrifugation afterproduct volume, and finally dialysis obtains graphite oxide in 7-8 days
Graphite oxide is put into purification liquid and obtains mixing material, carry out shaking dispersion and filter obtain purify after graphite oxide, described purification liquid is due to the concentrated sulfuric acid of 1.72g/ml and H 2o 2composition, the concentrated sulfuric acid and H 2o 2mass ratio be 1-2: 2-5;
Add N-hydroxysuccinimide after graphite oxide after purification is adopted methyl-sulfoxide ultrasonic dissolution and make surface conditioning agent by oneself and stir 2h at 35 DEG C, product carries out suction filtration, washing, oven dry, namely obtains surface-treated graphite oxide;
Step 3, dispersion
The ethylene glycol that the mixture (mass ratio of polymethylacrylic acid and polyacrylamide is 1: 1) be made up of polymethylacrylic acid and polyacrylamide with 1-10g PEO-PPOX-PEO triblock copolymer and 1g after surface-treated graphite oxide 1-2g step 2 obtained carries out lyophilization at-10-30 DEG C puts into 500ml in the lump carries out ultrasonic disperse, and then under ultraviolet irradiation, radiation 36h forms uniform first dispersion liquid;
Simultaneously by 4-15g by Fecl 36H 2o, Fecl 24H 2the mixture of O and acetyl acetone iron composition, 6 ~ 25g polyvinylpyrrolidone and 10 ~ 50g NH 4ac is dissolved in the ethylene glycol of 500-1000mL and forms the second dispersion liquid, by the first dispersion liquid and the second dispersion liquid mix and blend, and regulates with ammoniacal liquor, makes it to become the settled solution that pH value is 8-10, described Fecl 36H 2o, Fecl 24H 2the mass ratio of O and acetyl acetone iron is 1: 1: 0.5;
Step 4, the settled solution that 100ml step 3 obtains is put into reactor, after sealing, be heated to 150 DEG C, insulation 2h, 200 DEG C are warming up to afterwards with the heating rate of 2-4 DEG C/min, insulation 4h, 235 DEG C are warming up to afterwards with the heating rate of 3-6 DEG C/min, insulation 3h, then 200 DEG C of insulation 2h are cooled to the cooling rate of 5-7 DEG C/min, finally be warming up to 235 DEG C with the heating rate of 3-6 DEG C/min again, insulation 7h, after question response completes, reactor is taken out, make it cool to room temperature, described cooling rate is 3-6 DEG C/min, by the black powder centrifugation 10min of gained, rotating speed 8000 ~ 10000r/min, absolute ethyl alcohol and deionized water is adopted respectively to wash three times, at 50 ~ 70 DEG C of vacuum drying 24h, obtain the first product,
Be added in the solution of DBSA by 5g first product and 5-10g aniline monomer, ultrasonic disperse 65min, form the second product, the mass ratio of described first product and DBSA is 1-1.5: 8-15;
3g ammonium persulfate is dissolved in 80-120ml distilled water, slowly be added drop-wise in the second product, stirring reaction 15h, after reaction terminates, suction filtration, use distilled water, ethanol washed product colourless to filtrate respectively, 50 ~ 70 DEG C of vacuum drying 24 ~ 36h, obtain Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material;
Step 5, by Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material obtained in step 4, being positioned over place mat has in the ceramic crucible of potassium permanganate, and be placed in Muffle furnace and sinter, first 300 DEG C are warming up to the heating rate of 10 DEG C/min, insulation 30min, 600 DEG C are warming up to again with the heating rate of 12 DEG C/min, insulation 30min, then 500 DEG C are cooled to the rate of temperature fall of 15 DEG C/min, insulation 20min, finally be warming up to 950 DEG C of insulation 1-3h with the heating rate of 15 DEG C/min, obtain mesoporous material, the mass ratio of described Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material and potassium permanganate is 1: 3-5.
The particle diameter of described graphite powder is 15-30um.
The ratio of the g of graphite oxide described in step 2, methyl-sulfoxide ml, N-hydroxysuccinimide g and self-control surface conditioning agent g is 0.2-0.5: 20-25: 2-5: 0.1-05, described self-control surface conditioning agent is made up of dicyclohexylcarbodiimide, dodecyl sodium sulfate, kayexalate and polyacrylic acid, and described dicyclohexylcarbodiimide, dodecyl sodium sulfate, kayexalate and polyacrylic mass ratio are 1: 1: 2: 3.
In described described step 2, the concentration of hydrochloric acid is the hydrochloric acid solution of volume ratio 1: 10.
Described Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material is laminar nano composite wave-suction material, the ferroferric oxide nano granules homoepitaxial of hollow hemisphere structure is on two surfaces up and down of redox graphene sheet, the absorbing material of the multi-layer compound structure of a kind of nano thickness formed, on graphene sheet layer, load particle diameter is about hollow four iron oxide three particles of 20-50nm, and polyaniline-coated has the graphene sheet layer surface of hollow nano ferriferrous oxide in load.The hole dimension of described mesoporous material is 5-30nm, and the suction ripple within the scope of 1-20Hz is-35-55dB.Have higher electrical conductivity, absorbing property within the scope of 1-20Hz is excellent, can be used for electromagnetic-wave absorbent, also can as environment adsorbing materials, for adsorbing the pollutants such as heavy metal in environment.The electric capacity of this mesoporous material under the current density of 200mA/g is 435-458F/g.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.

Claims (5)

1. a preparation method for complex mesoporous material, is characterized in that, its step is as follows:
Step one, the preparation of pre-oxidation graphite
By graphite powder, potassium peroxydisulfate and P 2o 5add in the concentrated sulfuric acid, form mixture, the pH value of the mixture formed is 1.5, and this mixture is stirred 1-2h at 60 DEG C, then 2-4h is stirred with at the ramp to 80 of 5 DEG C/min DEG C, finally be warming up to 87 DEG C with 2 DEG C/min and stir 1-2h, then adopt this mixture of distilled water diluting, the pH value of this mixture is diluted to 3.6, distilled water is adopted to filter after placing 36h, make mixture pH value be 6-7, after carry out drying at room temperature, described graphite powder, potassium peroxydisulfate, P 2o 5be 1-3: 1-2: 1-2: 5-10 with the mass ratio of the concentrated sulfuric acid;
Joined in red fuming nitric acid (RFNA) by dried mixture and stir 45-60min, make pH value be 2-4, the mass ratio of described dried mixture and red fuming nitric acid (RFNA) is 1-4: 50-100, and after stirring, at-8 DEG C, first time adds KMnO 4, stir 30min, at being cooled to-12 DEG C afterwards, second time adds KMnO 4, stir 30min, at being finally cooled to-15 DEG C, third time adds KMnO 4, stir 20min, obtain the graphite mixture of pre-oxidation, described first time adds KMnO 4, second time adds KMnO 4kMnO is added with third time 4mass ratio be 1: 2: 3, described dried mixture and total KMnO 4ratio be 1-2: 10-15.
Step 2, the preparation of surface-treated graphite oxide
The graphite mixture of pre-oxidation made for step one is put into incubator and is warmed up to 40 DEG C, reaction 3h, subsequently, add the first distilled water with the consistent amount of graphite mixture volume of pre-oxidation, then react 2.5h, by incubator temperature to 40 DEG C, again add after-fractionating water and H 2o 2reaction 10-60min, the amount of described after-fractionating water is 1-1.5 times of the first distilled water, after-fractionating water and H 2o 2volume ratio be 4-20: 1, reaction terminate after carry out centrifugation 10min, rotating speed 9500r/min, centrifugation afterproduct hydrochloric acid solution washs, the volume of this hydrochloric acid solution is 10-50 times of centrifugation afterproduct volume, and finally dialysis obtains graphite oxide in 7-8 days
Graphite oxide is put into purification liquid and obtains mixing material, carry out shaking dispersion and filter obtain purify after graphite oxide, described purification liquid is due to the concentrated sulfuric acid of 1.72g/ml and H 2o 2composition, the concentrated sulfuric acid and H 2o 2mass ratio be 1-2: 2-5;
Add N-hydroxysuccinimide after graphite oxide after purification is adopted methyl-sulfoxide ultrasonic dissolution and make surface conditioning agent by oneself and stir 2h at 35 DEG C, product carries out suction filtration, washing, oven dry, namely obtains surface-treated graphite oxide;
Step 3, dispersion
The ethylene glycol that the mixture (mass ratio of polymethylacrylic acid and polyacrylamide is 1: 1) be made up of polymethylacrylic acid and polyacrylamide with 1-10g PEO-PPOX-PEO triblock copolymer and 1g after surface-treated graphite oxide 1-2g step 2 obtained carries out lyophilization at-10-30 DEG C puts into 500ml in the lump carries out ultrasonic disperse, and then under ultraviolet irradiation, radiation 36h forms uniform first dispersion liquid;
Simultaneously by 4-15g by Fecl 36H 2o, Fecl 24H 2the mixture of O and acetyl acetone iron composition, 6 ~ 25g polyvinylpyrrolidone and 10 ~ 50g NH 4ac is dissolved in the ethylene glycol of 500-1000mL and forms the second dispersion liquid, by the first dispersion liquid and the second dispersion liquid mix and blend, and regulates with ammoniacal liquor, makes it to become the settled solution that pH value is 8-10, described Fecl 36H 2o, Fecl 24H 2the mass ratio of O and acetyl acetone iron is 1: 1: 0.5;
Step 4, the settled solution that 100ml step 3 obtains is put into reactor, after sealing, be heated to 150 DEG C, insulation 2h, 200 DEG C are warming up to afterwards with the heating rate of 2-4 DEG C/min, insulation 4h, 235 DEG C are warming up to afterwards with the heating rate of 3-6 DEG C/min, insulation 3h, then 200 DEG C of insulation 2h are cooled to the cooling rate of 5-7 DEG C/min, finally be warming up to 235 DEG C with the heating rate of 3-6 DEG C/min again, insulation 7h, after question response completes, reactor is taken out, make it cool to room temperature, described cooling rate is 3-6 DEG C/min, by the black powder centrifugation 10min of gained, rotating speed 8000 ~ 10000r/min, absolute ethyl alcohol and deionized water is adopted respectively to wash three times, at 50 ~ 70 DEG C of vacuum drying 24h, obtain the first product,
Be added in the solution of DBSA by 5g first product and 5-10g aniline monomer, ultrasonic disperse 65min, form the second product, the mass ratio of described first product and DBSA is 1-1.5: 8-15;
3g ammonium persulfate is dissolved in 80-120ml distilled water, slowly be added drop-wise in the second product, stirring reaction 15h, after reaction terminates, suction filtration, use distilled water, ethanol washed product colourless to filtrate respectively, 50 ~ 70 DEG C of vacuum drying 24 ~ 36h, obtain Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material;
Step 5, by Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material obtained in step 4, being positioned over place mat has in the ceramic crucible of potassium permanganate, and be placed in Muffle furnace and sinter, first 300 DEG C are warming up to the heating rate of 10 DEG C/min, insulation 30min, 600 DEG C are warming up to again with the heating rate of 12 DEG C/min, insulation 30min, then 500 DEG C are cooled to the rate of temperature fall of 15 DEG C/min, insulation 20min, finally be warming up to 950 DEG C of insulation 1-3h with the heating rate of 15 DEG C/min, obtain mesoporous material, the mass ratio of described Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material and potassium permanganate is 1: 3-5.
2. preparation method according to claim 1, is characterized in that, the particle diameter of described graphite powder is 15-30um.
3. preparation method according to claim 1, it is characterized in that, the ratio of the g of graphite oxide described in step 2, methyl-sulfoxide ml, N-hydroxysuccinimide g and self-control surface conditioning agent g is 0.2-0.5: 20-25: 2-5: 0.1-05, described self-control surface conditioning agent is made up of dicyclohexylcarbodiimide, dodecyl sodium sulfate, kayexalate and polyacrylic acid, and described dicyclohexylcarbodiimide, dodecyl sodium sulfate, kayexalate and polyacrylic mass ratio are 1: 1: 2: 3.
4. preparation method according to claim 1, is characterized in that, in described described step 2, the concentration of hydrochloric acid is the hydrochloric acid solution of volume ratio 1: 10.
5. preparation method according to claim 1, it is characterized in that, described Graphene/hollow tri-iron tetroxide/polyaniline nano-composite material is laminar nano composite wave-suction material, the ferroferric oxide nano granules homoepitaxial of hollow hemisphere structure is on two surfaces up and down of redox graphene sheet, the absorbing material of the multi-layer compound structure of a kind of nano thickness formed, on graphene sheet layer, load particle diameter is about hollow four iron oxide three particles of 20-50nm, and polyaniline-coated has the graphene sheet layer surface of hollow nano ferriferrous oxide in load.
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CN105399088A (en) * 2015-12-11 2016-03-16 中国电子科技集团公司第十八研究所 Washing separation method of graphite oxide for graphene
CN105609305A (en) * 2016-01-19 2016-05-25 吉林大学 Preparation method of Fe<3>O<4>/graphene composite membrane
CN106400089A (en) * 2016-06-03 2017-02-15 安徽长青电子机械（集团）有限公司 Corrosion-resistant scaffolding composite electroplate liquid
CN106519222A (en) * 2016-10-15 2017-03-22 成都育芽科技有限公司 A graphene/magnetic particle/polyaniline composite porous wave-absorbing material and a preparing method thereof
CN108578703A (en) * 2018-05-25 2018-09-28 河北工业大学 A kind of preparation method of function medicine carrying material
CN111229164A (en) * 2020-02-21 2020-06-05 大连理工大学 Microporous carbon adsorbent for separating olefin and alkane and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103117175A (en) * 2013-02-25 2013-05-22 中国科学院过程工程研究所 Multi-element composite nano-material, preparation method thereof and application thereof
CN104163919A (en) * 2014-07-25 2014-11-26 北京科技大学 Polyaniline/oxidized graphene/ferriferrous oxide absorbing material and preparation method
CN104211058A (en) * 2014-09-22 2014-12-17 安徽理工大学 Method for preparing graphene from conducting polymer polyaniline

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103117175A (en) * 2013-02-25 2013-05-22 中国科学院过程工程研究所 Multi-element composite nano-material, preparation method thereof and application thereof
CN104163919A (en) * 2014-07-25 2014-11-26 北京科技大学 Polyaniline/oxidized graphene/ferriferrous oxide absorbing material and preparation method
CN104211058A (en) * 2014-09-22 2014-12-17 安徽理工大学 Method for preparing graphene from conducting polymer polyaniline

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
包莹: "石墨烯基磁性纳米复合物的制备及其性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105032375A (en) * 2015-06-24 2015-11-11 南京理工大学 Preparation method of magnetic graphite-based heavy metal adsorbing material
CN105032375B (en) * 2015-06-24 2017-05-17 南京理工大学 Preparation method of magnetic graphite-based heavy metal adsorbing material
CN105399088A (en) * 2015-12-11 2016-03-16 中国电子科技集团公司第十八研究所 Washing separation method of graphite oxide for graphene
CN105399088B (en) * 2015-12-11 2017-06-27 中国电子科技集团公司第十八研究所 A kind of washing separating method of Graphene graphite oxide
CN105609305A (en) * 2016-01-19 2016-05-25 吉林大学 Preparation method of Fe<3>O<4>/graphene composite membrane
CN106400089A (en) * 2016-06-03 2017-02-15 安徽长青电子机械（集团）有限公司 Corrosion-resistant scaffolding composite electroplate liquid
CN106519222A (en) * 2016-10-15 2017-03-22 成都育芽科技有限公司 A graphene/magnetic particle/polyaniline composite porous wave-absorbing material and a preparing method thereof
CN108578703A (en) * 2018-05-25 2018-09-28 河北工业大学 A kind of preparation method of function medicine carrying material
CN108578703B (en) * 2018-05-25 2020-07-28 河北工业大学 Preparation method of functional drug-loaded material
CN111229164A (en) * 2020-02-21 2020-06-05 大连理工大学 Microporous carbon adsorbent for separating olefin and alkane and preparation method and application thereof
CN111229164B (en) * 2020-02-21 2022-03-08 大连理工大学 Microporous carbon adsorbent for separating olefin and alkane and preparation method and application thereof

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