CN104497971A - Absorbing material - Google Patents
Absorbing material Download PDFInfo
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- CN104497971A CN104497971A CN201510016290.3A CN201510016290A CN104497971A CN 104497971 A CN104497971 A CN 104497971A CN 201510016290 A CN201510016290 A CN 201510016290A CN 104497971 A CN104497971 A CN 104497971A
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Abstract
The invention discloses an absorbing material. A method comprises the steps of preparing graphite oxide, dispersing, and successfully loading hollow ferrate nanoparticles to the surface of a grapheme slice layer. According to the method provided by the invention, the absorbing material with excellent absorbing material can be prepared conveniently.
Description
Technical field
The present invention relates to absorbing material field, in particular a kind of absorbing material.
Background technology
Along with science and technology and the development of electronic 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 neural system, immunity system, reproductive system and blood circulation etc.Be in for a long time in electromagnetic wave environment, damaged by hertzian 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 surface area, specific inductivity that 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 out-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 matrix material, and ferriferrous oxide particles is again stacking in three-dimensional graphite structure in drying process as spacer medium minimizing Graphene, considerable effect is played to stable graphene film Rotating fields.
Technical problem to be solved by this invention is for the deficiencies in the prior art, provides a kind of absorbing material.
Technical scheme of the present invention is as follows:
A kind of absorbing material, it is characterized in that this absorbing 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 ferric 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 this absorbing material is as described below:
Step one, the preparation of preoxidation graphite
By Graphite Powder 99, Potassium Persulphate and P
2o
5add in the vitriol oil, 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 99, Potassium Persulphate, P
2o
5be 1-3: 1-2: 1-2: 5-10 with the mass ratio of the vitriol oil;
Joined in concentrated nitric acid by dried mixture and stir 45-60min, make pH value be 2-4, the mass ratio of described dried mixture and concentrated nitric acid 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 preoxidation, 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 preoxidation made for step one is put into insulation can 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 preoxidation, then react 2.5h, by insulation can 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, centrifugation 10min is carried out after reaction terminates, rotating speed 9500r/min, centrifugation after product hydrochloric acid soln washs, the volume of this hydrochloric acid soln is 10-50 times of centrifugation after product volume, and finally dialysis obtains graphite oxide in 7-8 days, adds N-hydroxyl and at 35 DEG C, stir 2h in imide and self-control surface treatment agent after graphite oxide being adopted methyl-sulphoxide ultrasonic dissolution, product carries out suction filtration, washing, oven dry, namely obtains surface-treated graphite oxide;
Step 3, dispersion
Surface-treated graphite oxide 1-2g step 2 obtained puts into 500ml in the lump at-10-30 DEG C with 1-10g polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer ethylene glycol ultrasonic disperse after every trade frost drying 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 temperature rise rate of 2-4 DEG C/min, insulation 4h, 235 DEG C are warming up to afterwards with the temperature rise 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 temperature rise 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, dehydrated 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 Witco 1298 Soft Acid by 5g first product and 5-10g aniline monomer, ultrasonic disperse 65min, form the second product, the mass ratio of described first product and Witco 1298 Soft Acid is 1-1.5: 8-15;
Be dissolved in by 3g ammonium persulphate in 80-120ml distilled water, be slowly added drop-wise in the second product, stirring reaction 15h, after reaction terminates, suction filtration, use distilled water, washing with alcohol product colourless to filtrate respectively, 50 ~ 70 DEG C of vacuum-drying 24 ~ 36h, obtain absorbing material.
The particle diameter of described Graphite Powder 99 is 15-30um.
The ratio of the g of graphite oxide described in step 2, methyl-sulphoxide ml, N-hydroxysuccinimide g and self-control surface treatment agent g is 0.2-0.5: 20-25: 2-5: 0.1-05, described self-control surface treatment agent is made up of dicyclohexylcarbodiimide, sodium laurylsulfonate, sodium polystyrene sulfonate and polyacrylic acid, and described dicyclohexylcarbodiimide, sodium laurylsulfonate, sodium polystyrene sulfonate and polyacrylic mass ratio are 1: 1: 2: 3.
In described described step 2, the concentration of hydrochloric acid is the hydrochloric acid soln of volume ratio 1: 10.
The preparation method of absorbing material of the present invention is by the growth in situ of Z 250 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;
Applicant prepares preoxidation graphite through large quantity research step one of the present invention and adopts different temperature rise 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 preoxidation 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 surface treatment is done for graphite oxide, adopt homemade surface treatment agent, the surperficial shortcoming low for metallic iron ion avidity of graphite oxide enough can be made up after adding, increase the charge capacity of surperficial Fe ion, also make Fe ion below more even in the dispersion of graphite surface, the specific surface area of its graphite reaches 35-37m simultaneously
2/ g;
During adopting different temperature rise 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 Z 250, make the absorbing property of the final absorbing material formed stronger, be better than the performance 5-15% of the absorbing material that usual way 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.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
A kind of absorbing material, it is characterized in that this absorbing 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 ferric 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 this absorbing material is as described below:
Step one, the preparation of preoxidation graphite
By Graphite Powder 99, Potassium Persulphate and P
2o
5add in the vitriol oil, 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 99, Potassium Persulphate, P
2o
5be 1-3: 1-2: 1-2: 5-10 with the mass ratio of the vitriol oil;
Joined in concentrated nitric acid by dried mixture and stir 45-60min, make pH value be 2-4, the mass ratio of described dried mixture and concentrated nitric acid 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 preoxidation, 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 preoxidation made for step one is put into insulation can 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 preoxidation, then react 2.5h, by insulation can 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, centrifugation 10min is carried out after reaction terminates, rotating speed 9500r/min, centrifugation after product hydrochloric acid soln washs, the volume of this hydrochloric acid soln is 10-50 times of centrifugation after product volume, and finally dialysis obtains graphite oxide in 7-8 days, adds N-hydroxysuccinimide and makes surface treatment agent by oneself and stir 2h after graphite oxide being adopted methyl-sulphoxide ultrasonic dissolution at 35 DEG C, product carries out suction filtration, washing, oven dry, namely obtains surface-treated graphite oxide;
Step 3, dispersion
The ethylene glycol ultrasonic disperse putting into 500ml after surface-treated graphite oxide 1-2g step 2 obtained carries out frost drying at-10-30 DEG C with 1-10g polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer in the lump 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 temperature rise rate of 2-4 DEG C/min, insulation 4h, 235 DEG C are warming up to afterwards with the temperature rise 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 temperature rise 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, dehydrated 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 Witco 1298 Soft Acid by 5g first product and 5-10g aniline monomer, ultrasonic disperse 65min, form the second product, the mass ratio of described first product and Witco 1298 Soft Acid is 1-1.5: 8-15;
Be dissolved in by 3g ammonium persulphate in 80-120ml distilled water, be slowly added drop-wise in the second product, stirring reaction 15h, after reaction terminates, suction filtration, use distilled water, washing with alcohol product colourless to filtrate respectively, 50 ~ 70 DEG C of vacuum-drying 24 ~ 36h, obtain absorbing material.
The particle diameter of described Graphite Powder 99 is 15-30um.
The ratio of the g of graphite oxide described in step 2, methyl-sulphoxide ml, N-hydroxysuccinimide g and self-control surface treatment agent g is 0.2-0.5: 20-25: 2-5: 0.1-05, described self-control surface treatment agent is made up of dicyclohexylcarbodiimide, sodium laurylsulfonate, sodium polystyrene sulfonate and polyacrylic acid, and described dicyclohexylcarbodiimide, sodium laurylsulfonate, sodium polystyrene sulfonate and polyacrylic mass ratio are 1: 1: 2: 3.
In described described step 2, the concentration of hydrochloric acid is the hydrochloric acid soln of volume ratio 1: 10.
At the Absorber Bandwidth of below reflection loss-10dB up to 4.8-5.1GHz, and maximum reflection loss reaches-24dB.
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 (4)
1. an absorbing material, it is characterized in that this absorbing 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 ferric 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 this absorbing material is as described below:
Step one, the preparation of preoxidation graphite
By Graphite Powder 99, Potassium Persulphate and P
2o
5add in the vitriol oil, 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 99, Potassium Persulphate, P
2o
5be 1-3: 1-2: 1-2: 5-10 with the mass ratio of the vitriol oil;
Joined in concentrated nitric acid by dried mixture and stir 45-60min, make pH value be 2-4, the mass ratio of described dried mixture and concentrated nitric acid 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 preoxidation, 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 preoxidation made for step one is put into insulation can 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 preoxidation, then react 2.5h, by insulation can 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, centrifugation 10min is carried out after reaction terminates, rotating speed 9500r/min, centrifugation after product hydrochloric acid soln washs, the volume of this hydrochloric acid soln is 10-50 times of centrifugation after product volume, and finally dialysis obtains graphite oxide in 7-8 days, adds N-hydroxysuccinimide and makes surface treatment agent by oneself and stir 2h after graphite oxide being adopted methyl-sulphoxide ultrasonic dissolution at 35 DEG C, product carries out suction filtration, washing, oven dry, namely obtains surface-treated graphite oxide;
Step 3, dispersion
The ethylene glycol ultrasonic disperse putting into 500ml after surface-treated graphite oxide 1-2g step 2 obtained carries out frost drying at-10-30 DEG C with 1-10g polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer in the lump 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 NH4Ac are dissolved in the ethylene glycol of 500-1000mL and form the second dispersion liquid, by the first dispersion liquid and the second dispersion liquid mix and blend, and regulate with ammoniacal liquor, make 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 temperature rise rate of 2-4 DEG C/min, insulation 4h, 235 DEG C are warming up to afterwards with the temperature rise 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 temperature rise 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, dehydrated 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 Witco 1298 Soft Acid by 5g first product and 5-10g aniline monomer, ultrasonic disperse 65min, form the second product, the mass ratio of described first product and Witco 1298 Soft Acid is 1-1.5: 8-15;
Be dissolved in by 3g ammonium persulphate in 80-120ml distilled water, be slowly added drop-wise in the second product, stirring reaction 15h, after reaction terminates, suction filtration, use distilled water, washing with alcohol product colourless to filtrate respectively, 50 ~ 70 DEG C of vacuum-drying 24 ~ 36h, obtain absorbing material.
2. a kind of absorbing material according to claim 1, is characterized in that, the particle diameter of described Graphite Powder 99 is 15-30um.
3. a kind of absorbing material according to claim 1, it is characterized in that, the ratio of the g of graphite oxide described in step 2, methyl-sulphoxide ml, N-hydroxysuccinimide g and self-control surface treatment agent g is 0.2-0.5: 20-25: 2-5: 0.1-05, described self-control surface treatment agent is made up of dicyclohexylcarbodiimide, sodium laurylsulfonate, sodium polystyrene sulfonate and polyacrylic acid, and described dicyclohexylcarbodiimide, sodium laurylsulfonate, sodium polystyrene sulfonate and polyacrylic mass ratio are 1: 1: 2: 3.
4. a kind of absorbing material according to claim 1, is characterized in that, in described described step 2, the concentration of hydrochloric acid is the hydrochloric acid soln of volume ratio 1: 10.
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| CN201510016290.3A CN104497971A (en) | 2015-01-12 | 2015-01-12 | Absorbing material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105293468A (en) * | 2015-11-04 | 2016-02-03 | 上海应用技术学院 | Method for efficiently preparing sulphur-doped hollow carbon spheres |
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|---|---|---|---|---|
| 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 |
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2015
- 2015-01-12 CN CN201510016290.3A patent/CN104497971A/en active Pending
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| 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 |
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