CN107934952A - A kind of preparation method of the graphene oxide with absorbing property - Google Patents
A kind of preparation method of the graphene oxide with absorbing property Download PDFInfo
- Publication number
- CN107934952A CN107934952A CN201711472587.6A CN201711472587A CN107934952A CN 107934952 A CN107934952 A CN 107934952A CN 201711472587 A CN201711472587 A CN 201711472587A CN 107934952 A CN107934952 A CN 107934952A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- absorbing property
- preparation
- sulfuric acid
- concentrated sulfuric
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
Abstract
A kind of preparation method of the graphene oxide with absorbing property, belongs to nano wave-absorbing material manufacturing field.Method is：1) after the concentrated sulfuric acid that natural flake graphite, potassium peroxydisulfate, phosphorus pentoxide and mass fraction are 98% is mixed, under agitation, reacted in water bath with thermostatic control；Neutrality is washed, vacuum pump is filtered, ground after drying, to pre-oxidation graphite presoma；2) first the concentrated sulfuric acid for pre-oxidizing graphite presoma with mass fraction is 98% is mixed in ice-water bath, is slowly added to potassium permanganate and potassium bichromate, obtains mixture；In isoperibol, 2~4h of reaction obtains blackish green viscous liquid；Cl is passed through during temperature≤45 DEG C2, deionized water for a period of time after, then ionized water and hydrogen peroxide, are made bright yellow solution；By bright yellow solution, filter and washed with dilute hydrochloric acid, be washed with deionized to PH=6.8~7.2, obtain mixed liquor；Ground after drying, graphene oxide is made.
Description
Technical field
The invention belongs to nano wave-absorbing material manufacturing field, more particularly to a kind of system with absorbing property graphene oxide
Preparation Method.
Background technology
Graphene oxide has and graphene as oxidation, the important intermediate of two stages " forming a connecting link " of reduction
Similar two-dimensional structure, and oxygen-containing functional group has stronger reactivity in structure sheaf, easily with other organic or inorganic materials
Compound is formed, thus is received significant attention.
The existing main method for preparing graphene oxide has：Hummers methods, improve Hummers methods.The present invention, which uses, to be changed
Into Hummers methods, manufacturing cost is cheap and easy to implement, and can prepare stable graphene oxide suspension, solves
It is not easy the problem of scattered.Oxidizing process, which refers to react native graphite and strong acid and oxidizing species, generates graphite oxide (GO),
The defects of being prepared into graphene oxide (mono-layer graphite oxide) by ultrasonic disperse, being produced in oxidizing process can produce defect
Dielectric relaxor and group's electronics dipole relaxation, these can all increase the infiltration and absorption of electromagnetic wave, shortcoming cleverly is become excellent
Point.This method is simple, cost is low, reaction condition is gently easy to control.
At present, tend to graphene oxide for most of the study of radar absorbing property of graphene oxide to carry out with other materials
It is compound, such as ferrite etc..So that the absorbing material production cost prepared is very high, it is unfavorable for commercial introduction in daily life.And
The present invention probes into the absorbing property of graphene oxide itself, and between 14~18GHz, maximum reflectivity reaches -34.28dB.Can
The features such as to meet for absorbing material " light weight, thickness are thin ", beneficial to the production and application of the modern life.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation side of the graphene oxide with absorbing property
Method.Absorbing property of the graphene oxide in high frequency band is realized, is that a kind of method is simple, cost is low, reaction condition is easily-controllable,
The preparation method of the good graphene oxide of high frequency band (14~18GHz) absorbing property.
The preparation method of the graphene oxide with absorbing property of the present invention, comprises the following steps：
Step 1, graphite presoma is pre-oxidized to prepare：
(1) in mass ratio, natural flake graphite (C): potassium peroxydisulfate (K2S2O8): phosphorus pentoxide (P2O5): mass fraction
For 98% concentrated sulfuric acid (H25O4)=(1~3): (1~5): (1~4): (8~10), weigh above-mentioned 4 kinds of raw materials respectively；
(2) after 4 kinds of raw materials are mixed, under agitation, 50~90 DEG C of water bath with thermostatic control is placed in, reacts 6~8h；
(3) diluted with deionized water and wash neutrality, vacuum pump filters, and is ground after drying at room temperature, to pre- oxygen
Graphite presoma；
Step 2, secondary oxidation prepares graphene oxide：
(1) by pre-oxidation graphite presoma (g): mass fraction is 98% concentrated sulfuric acid (mL): potassium permanganate (g): weight chromium
Sour potassium (g)=(1~4): (13~23): (4~8): (1~3), measures or take respectively above-mentioned 4 kinds of raw materials, will first pre-oxidize stone
The concentrated sulfuric acid that black presoma and mass fraction are 98% mixes in ice-water bath, stirring be respectively added slowly at the same time potassium permanganate and
Potassium bichromate, obtains mixture；
(2) mixture is placed in 30~40 DEG C of isoperibol, fully reacts 2~4h, be made blackish green thick
Liquid；
(3) by volume, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid: first part of deionized water=(1
~3): (2~4), measure first part of deionized water, the material quality fraction in step 2 (1) is 98% dense sulphur by volume
Acid：Second part of deionized water: hydrogen peroxide=(28~30): (1~3), measures second part of deionized water and hydrogen peroxide；
Temperature≤45 DEG C of blackish green viscous liquid are controlled, Cl is continually fed into blackish green viscous liquid2,
First part of deionized water is added, after 12~18min, second part of deionized water and hydrogen peroxide is added, bright yellow solution is made, this
When stop be passed through Cl2；
(3) by bright yellow solution, filter and washed with dilute hydrochloric acid, be washed with deionized to PH=6.8~7.2, obtain mixed
Close liquid；
(4) by mixed liquor, ground after drying, graphene oxide is made.
The preparation method of the above-mentioned graphene oxide with absorbing property, wherein：
In the step 1 (1), potassium peroxydisulfate, phosphorus pentoxide, the concentrated sulfuric acid are that analysis is pure, and graphite powder used is natural
Crystalline flake graphite, purity 99.5%.
In the step 1 (2), raw material electric stirring in thermostatted water, makes the concentrated sulfuric acid be come into full contact with graphite, by graphite linings
Between expand, make its carry out pre-oxidation.
In the step 1 (2), mixing speed is 150~270r/min.
In the step 1 (2), react and carried out in four-hole boiling flask.
It is that potassium permanganate is exploded by thermal decomposition in order to prevent using ice-water bath in the step 2 (1).
In the step 2 (1), the speed being slowly added to is 0.5~1.2g/min.
In the step 2 (2), isoperibol is water bath with thermostatic control.The water bath with thermostatic control carries out in thermostat water bath.
In the step 2 (2), the method fully reacted is auxiliary electric stirring mixture.
In the step 2 (2), the flow control of chlorine is 0.1~10m3/h。
In the step 2 (3), the mass concentration of dilute hydrochloric acid is 5~15%.
In the step 2 (3), metal ion is washed away using dilute hydrochloric acid.
In the step 2 (4), dried using air dry oven.
Graphene oxide with absorbing property prepared by the method for the present invention, its interlamellar spacing are 0.82~.0.91nm, the oxygen
Graphite alkene is 0.96~1.77 in the magnetic conductivity real part of 17.83GHz Frequency points, and imaginary part is 0.02~0.96；Dielectric constant is real
Portion is 6.18, and imaginary part is 11.42~2.87.
The preparation method of the graphene oxide with absorbing property of the present invention, compared with prior art, of the invention is excellent
Point is：
The graphene oxide layer structure of the present invention is greatly improved in the case where keeping its maximum integrality
Graphene oxide obtains the good stannic oxide/graphene nano material of electromagnetic performance, the system from the absorbing property in high band
Preparation Method is simple, and cost is low, and reaction condition is easily-controllable, and product quality is light, and dielectric loss and magnetic hystersis loss are provided with and well, are applicable in
In industrialized production.
Brief description of the drawings
The process flow chart of the preparation method of the graphene oxide with absorbing property of Fig. 1 embodiment of the present invention 1~5；
The scanning electron microscopic picture of graphene oxide with absorbing property prepared by Fig. 2 embodiment of the present invention 1；
The scanning electron microscopic picture of graphene oxide with absorbing property prepared by Fig. 3 embodiment of the present invention 2；
The scanning electron microscopic picture of graphene oxide with absorbing property prepared by Fig. 4 embodiment of the present invention 3；
The scanning electron microscopic picture of graphene oxide with absorbing property prepared by Fig. 5 embodiment of the present invention 4；
The scanning electron microscopic picture of graphene oxide with absorbing property prepared by Fig. 6 embodiment of the present invention 5；
The magnetic conductivity real part of graphene oxide with absorbing property prepared by Fig. 7 different embodiments of the invention, imaginary part and
Real part of permittivity, imaginary part contrast picture；
Fig. 8 invents the picture of the reflectance loss of the graphene oxide with absorbing property prepared by different embodiments.
Embodiment：
In following embodiments, the process flow chart of the preparation method of the graphene oxide with absorbing property is as shown in Figure 1.
In following embodiments, potassium peroxydisulfate, phosphorus pentoxide, mass fraction are 98% concentrated sulfuric acid, are that analysis is pure, used
Graphite powder is natural flake graphite, purity 99.5%.
Embodiment 1
A kind of preparation method of the graphene oxide with absorbing property, comprises the following steps：
Step 1, graphite presoma is pre-oxidized to prepare：
(1) in mass ratio, natural flake graphite (C): potassium peroxydisulfate (K2S2O8): phosphorus pentoxide (P2O5): mass fraction
For 98% concentrated sulfuric acid (H2SO4)=1: 1: 1: 8, weigh above-mentioned 4 kinds of raw materials respectively；
(2) after 4 kinds of raw materials are mixed in four-hole boiling flask, under agitation, 60 DEG C of water bath with thermostatic control is placed in, reacted
7h, mixing speed 150r/min；
(3) diluted with deionized water and wash neutrality, vacuum pump filters, and is ground after drying at room temperature, to pre- oxygen
Graphite presoma；
Step 2, secondary oxidation prepares graphene oxide：
(1) by pre-oxidation graphite presoma (g): mass fraction is 98% concentrated sulfuric acid (mL): potassium permanganate (g): weight chromium
Sour potassium (g)=1: 15: 2: 0.5, above-mentioned 4 kinds of raw materials are measured or take respectively, first will pre-oxidation graphite presoma and mass fraction
Mixed for 98% concentrated sulfuric acid in ice-water bath, stirring is slowly added to potassium permanganate and weight chromium with the speed of 1g/min respectively at the same time
Sour potassium, obtains mixture；
(2) during mixture is placed in 35 DEG C of thermostat water bath, fully reaction 2h, is made blackish green under the conditions of electric stirring
The viscous liquid of color；
(3) by volume, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid: first part of deionized water=15
: 46, first part of deionized water 92mL is measured, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid by volume：The
Two parts of deionized waters: hydrogen peroxide=35: 1, measure second part of deionized water 280mL and hydrogen peroxide 8mL；
Temperature≤45 DEG C of blackish green viscous liquid are controlled, Cl is continually fed into blackish green viscous liquid2,
The flow control of chlorine is 5m3/ h, adds first part of deionized water, after 15min, adds second part of deionized water and peroxidating
Hydrogen, is made bright yellow solution, stops being passed through Cl at this time2；
(3) by bright yellow solution, filter and washed with the dilute hydrochloric acid that mass concentration is 10%, is washed with deionized to PH
=7, obtain mixed liquor；
(4) by mixed liquor, ground after being dried in air dry oven, graphene oxide is made.
Graphene oxide manufactured in the present embodiment with absorbing property, scanning electron microscopic picture are shown in attached drawing 2, and magnetic conductivity is real
Portion, imaginary part and real part of permittivity, imaginary part contrast picture are shown in attached drawing 7, its interlamellar spacing is 0.82nm, which exists
The magnetic conductivity real part of 17.83GHz Frequency points is 1, imaginary part 0.02；Real part of permittivity is 5.2, imaginary part 1.46；This implementation
The picture of the reflectance loss of graphene oxide with absorbing property prepared by example is shown in attached drawing 8.
Embodiment 2
A kind of preparation method of the graphene oxide with absorbing property, comprises the following steps：
Step 1, graphite presoma is pre-oxidized to prepare：
(1) in mass ratio, natural flake graphite (C): potassium peroxydisulfate (K2S2O8): phosphorus pentoxide (P2O5): mass fraction
For 98% concentrated sulfuric acid (H2SO4)=2: 2: 1: 9, weigh above-mentioned 4 kinds of raw materials respectively；
(2) after 4 kinds of raw materials are mixed in four-hole boiling flask, under agitation, 60 DEG C of water bath with thermostatic control is placed in, reacted
6h, mixing speed 270r/min；
(3) diluted with deionized water and wash neutrality, vacuum pump filters, and is ground after drying at room temperature, to pre- oxygen
Graphite presoma；
Step 2, secondary oxidation prepares graphene oxide：
(1) by pre-oxidation graphite presoma (g): mass fraction is 98% concentrated sulfuric acid (mL): potassium permanganate (g): weight chromium
Sour potassium (g)=1: 14: 3: 1, above-mentioned 4 kinds of raw materials are measured or taken respectively, are with mass fraction by pre-oxidation graphite presoma first
98% concentrated sulfuric acid mixes in ice-water bath, and stirring is slowly added to potassium permanganate and dichromic acid with the speed of 1g/min respectively at the same time
Potassium, obtains mixture；
(2) during mixture is placed in 35 DEG C of thermostat water bath, fully reaction 3h, is made blackish green under the conditions of electric stirring
The viscous liquid of color；
(3) by volume, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid: first part of deionized water=7:
23, first part of deionized water 92mL is measured, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid by volume：Second
Part deionized water: hydrogen peroxide=280: 9, measure second part of deionized water 280mL and hydrogen peroxide 9mL；
Temperature≤45 DEG C of blackish green viscous liquid are controlled, Cl is continually fed into blackish green viscous liquid2,
The flow control of chlorine is 5m3/ h, adds first part of deionized water, after 15min, adds second part of deionized water and peroxidating
Hydrogen, is made bright yellow solution, stops being passed through Cl at this time2；
(3) by bright yellow solution, filter and washed with the dilute hydrochloric acid that mass concentration is 10%, is washed with deionized to PH
=7, obtain mixed liquor；
(4) by mixed liquor, ground after being dried in air dry oven, graphene oxide is made.
Graphene oxide manufactured in the present embodiment with absorbing property, scanning electron microscopic picture are shown in attached drawing 3, and magnetic conductivity is real
Portion, imaginary part and real part of permittivity, imaginary part contrast picture are shown in attached drawing 7, its interlamellar spacing is 0.87nm, which exists
The magnetic conductivity real part of 17.83GHz Frequency points is 1.02, imaginary part 0.06；Real part of permittivity is 5.37, imaginary part 1.72；This
The picture of the reflectance loss of graphene oxide with absorbing property prepared by embodiment is shown in attached drawing 8.
Embodiment 3
A kind of preparation method of the graphene oxide with absorbing property, comprises the following steps：
Step 1, graphite presoma is pre-oxidized to prepare：
(1) in mass ratio, natural flake graphite (C): potassium peroxydisulfate (K2S2O8): phosphorus pentoxide (P2O5): mass fraction
For 98% concentrated sulfuric acid (H2SO4)=2: 1: 1: 10, weigh above-mentioned 4 kinds of raw materials respectively；
(2) after 4 kinds of raw materials are mixed in four-hole boiling flask, under agitation, 80 DEG C of water bath with thermostatic control is placed in, reacted
8h, mixing speed 180r/min；
(3) diluted with deionized water and wash neutrality, vacuum pump filters, and is ground after drying at room temperature, to pre- oxygen
Graphite presoma；
Step 2, secondary oxidation prepares graphene oxide：
(1) by pre-oxidation graphite presoma (g): mass fraction is 98% concentrated sulfuric acid (mL): potassium permanganate (g): weight chromium
Sour potassium (g)=1: 23: 3: 1.5, above-mentioned 4 kinds of raw materials are measured or take respectively, first will pre-oxidation graphite presoma and mass fraction
Mixed for 98% concentrated sulfuric acid in ice-water bath, stirring is slowly added to potassium permanganate and weight chromium with the speed of 1g/min respectively at the same time
Sour potassium, obtains mixture；
(2) during mixture is placed in 35 DEG C of thermostat water bath, fully reaction 2h, is made blackish green under the conditions of electric stirring
The viscous liquid of color；
(3) by volume, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid: first part of deionized water=1:
2, first part of deionized water 92mL is measured, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid by volume：Second
Part deionized water: hydrogen peroxide=28: 1, measure second part of deionized water 280mL and hydrogen peroxide 10mL；
Temperature≤45 DEG C of blackish green viscous liquid are controlled, Cl is continually fed into blackish green viscous liquid2,
The flow control of chlorine is 5m3/ h, adds first part of deionized water, after 15min, adds second part of deionized water and peroxidating
Hydrogen, is made bright yellow solution, stops being passed through Cl at this time2；
(3) by bright yellow solution, filter and washed with the dilute hydrochloric acid that mass concentration is 10%, is washed with deionized to PH
=7, obtain mixed liquor；
(4) by mixed liquor, ground after being dried in air dry oven, graphene oxide is made.
Graphene oxide manufactured in the present embodiment with absorbing property, scanning electron microscopic picture are shown in attached drawing 4, and magnetic conductivity is real
Portion, imaginary part and real part of permittivity, imaginary part contrast picture are shown in attached drawing 7, its interlamellar spacing is 0.91nm, which exists
The magnetic conductivity real part of 17.83GHz Frequency points is 1.77, imaginary part 0.96；Real part of permittivity is 6.18, imaginary part 1.98；This
The picture of the reflectance loss of graphene oxide with absorbing property prepared by embodiment is shown in attached drawing 8.
Embodiment 4
A kind of preparation method of the graphene oxide with absorbing property, comprises the following steps：
Step 1, graphite presoma is pre-oxidized to prepare：
(1) in mass ratio, natural flake graphite (C): potassium peroxydisulfate (K2S2O8): phosphorus pentoxide (P2O5): mass fraction
For 98% concentrated sulfuric acid (H2SO4)=3: 1: 1: 10, weigh above-mentioned 4 kinds of raw materials respectively；
(2) after 4 kinds of raw materials are mixed in four-hole boiling flask, under agitation, 70 DEG C of water bath with thermostatic control is placed in, reacted
6h, mixing speed 150r/min；
(3) diluted with deionized water and wash neutrality, vacuum pump filters, and is ground after drying at room temperature, to pre- oxygen
Graphite presoma；
Step 2, secondary oxidation prepares graphene oxide：
(1) by pre-oxidation graphite presoma (g): mass fraction is 98% concentrated sulfuric acid (mL): potassium permanganate (g): weight chromium
Sour potassium (g)=1: 20: 2: 1.5, above-mentioned 4 kinds of raw materials are measured or take respectively, first will pre-oxidation graphite presoma and mass fraction
Mixed for 98% concentrated sulfuric acid in ice-water bath, stirring is slowly added to potassium permanganate and weight chromium with the speed of 1g/min respectively at the same time
Sour potassium, obtains mixture；
(2) during mixture is placed in 35 DEG C of thermostat water bath, fully reaction 2h, is made blackish green under the conditions of electric stirring
The viscous liquid of color；
(3) by volume, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid: first part of deionized water=10
: 23, first part of deionized water 92mL is measured, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid by volume：The
Two parts of deionized waters: hydrogen peroxide=35: 1, measure second part of deionized water 280mL and hydrogen peroxide 8mL；
Temperature≤45 DEG C of blackish green viscous liquid are controlled, Cl is continually fed into blackish green viscous liquid2,
The flow control of chlorine is 5m3/ h, adds first part of deionized water, after 15min, adds second part of deionized water and peroxidating
Hydrogen, is made bright yellow solution, stops being passed through Cl at this time2；
(3) by bright yellow solution, filter and washed with the dilute hydrochloric acid that mass concentration is 10%, is washed with deionized to PH
=7, obtain mixed liquor；
(4) by mixed liquor, ground after being dried in air dry oven, graphene oxide is made.
Graphene oxide manufactured in the present embodiment with absorbing property, scanning electron microscopic picture are shown in attached drawing 5, and magnetic conductivity is real
Portion, imaginary part and real part of permittivity, imaginary part contrast picture are shown in attached drawing 7, its interlamellar spacing is 0.90nm, which exists
The magnetic conductivity real part of 17.83GHz Frequency points is 0.96, imaginary part 0.05；Real part of permittivity is 6.91, imaginary part 2.87；This
The picture of the reflectance loss of graphene oxide with absorbing property prepared by embodiment is shown in attached drawing 8.
Embodiment 5
A kind of preparation method of the graphene oxide with absorbing property, comprises the following steps：
Step 1, graphite presoma is pre-oxidized to prepare：
(1) in mass ratio, natural flake graphite (C): potassium peroxydisulfate (K2S2O8): phosphorus pentoxide (P2O5): mass fraction
For 98% concentrated sulfuric acid (H2SO4)=1: 2: 2: 10, weigh above-mentioned 4 kinds of raw materials respectively；
(2) after 4 kinds of raw materials are mixed in four-hole boiling flask, under agitation, 70 DEG C of water bath with thermostatic control is placed in, reacted
7h, mixing speed 270r/min；
(3) diluted with deionized water and wash neutrality, vacuum pump filters, and is ground after drying at room temperature, to pre- oxygen
Graphite presoma；
Step 2, secondary oxidation prepares graphene oxide：
(1) by pre-oxidation graphite presoma (g): mass fraction is 98% concentrated sulfuric acid (mL): potassium permanganate (g): weight chromium
Sour potassium (g)=2: 14: 1.5: 0.25, above-mentioned 4 kinds of raw materials are measured or take respectively, first will pre-oxidation graphite presoma and quality point
Number mixes for 98% concentrated sulfuric acid in ice-water bath, and stirring is slowly added to potassium permanganate and again with the speed of 1g/min respectively at the same time
Potassium chromate, obtains mixture；
(2) during mixture is placed in 35 DEG C of thermostat water bath, fully reaction 3h, is made blackish green under the conditions of electric stirring
The viscous liquid of color；
(3) by volume, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid: first part of deionized water=7:
23, first part of deionized water 92mL is measured, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid by volume：Second
Part deionized water: hydrogen peroxide=280: 9, measure second part of deionized water 280mL and hydrogen peroxide 9mL；
Temperature≤45 DEG C of blackish green viscous liquid are controlled, Cl is continually fed into blackish green viscous liquid2,
The flow control of chlorine is 5m3/ h, adds first part of deionized water, after 15min, adds second part of deionized water and peroxidating
Hydrogen, is made bright yellow solution, stops being passed through C1 at this time2；
(3) by bright yellow solution, filter and washed with the dilute hydrochloric acid that mass concentration is 10%, is washed with deionized to PH
=7, obtain mixed liquor；
(4) by mixed liquor, ground after being dried in air dry oven, graphene oxide is made.
Graphene oxide manufactured in the present embodiment with absorbing property, scanning electron microscopic picture are shown in attached drawing 6, and magnetic conductivity is real
Portion, imaginary part and real part of permittivity, imaginary part contrast picture are shown in attached drawing 7, its interlamellar spacing is 0.83nm, which exists
The magnetic conductivity real part of 17.83GHz Frequency points is 0.98, imaginary part 0.04；Real part of permittivity is 5.99, imaginary part 1.93；This
The picture of the reflectance loss of graphene oxide with absorbing property prepared by embodiment is shown in attached drawing 8.
Claims (10)
1. a kind of preparation method of the graphene oxide with absorbing property, it is characterised in that comprise the following steps：
Step 1, graphite presoma is pre-oxidized to prepare：
(1) in mass ratio, natural flake graphite (C): potassium peroxydisulfate (K2S2O8): phosphorus pentoxide (P2O5): mass fraction is
98% concentrated sulfuric acid (H2SO4)=(1~3): (1~5): (1~4): (8~10), weigh above-mentioned 4 kinds of raw materials respectively；
(2) after 4 kinds of raw materials are mixed, under agitation, 50~90 DEG C of water bath with thermostatic control is placed in, reacts 6~8h；
(3) diluted with deionized water and wash neutrality, vacuum pump filters, and is ground after drying at room temperature, to pre-oxidation stone
Black presoma；
Step 2, secondary oxidation prepares graphene oxide：
(1) by pre-oxidation graphite presoma (g): mass fraction is 98% concentrated sulfuric acid (mL): potassium permanganate (g): potassium bichromate
(g)=(1~4): (13~23): (4~8): (1~3), measures or take respectively above-mentioned 4 kinds of raw materials, before will first pre-oxidizing graphite
Drive body and mixed with the concentrated sulfuric acid that mass fraction is 98% in ice-water bath, stirring is respectively added slowly to potassium permanganate and weight chromium at the same time
Sour potassium, obtains mixture；
(2) mixture is placed in 30~40 DEG C of isoperibol, fully reacts 2~4h, blackish green viscous liquid is made；
(3) by volume, the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid: first part of deionized water=(1~3)
: (2~4), measure first part of deionized water, and the material quality fraction in step 2 (1) is 98% concentrated sulfuric acid by volume: the
Two parts of deionized waters: hydrogen peroxide=(28~30): (1~3), measures second part of deionized water and hydrogen peroxide；
Temperature≤45 DEG C of blackish green viscous liquid are controlled, Cl is continually fed into blackish green viscous liquid2, add
First part of deionized water, after 12~18min, adds second part of deionized water and hydrogen peroxide, bright yellow solution is made, stops at this time
Only it is passed through Cl2；
(3) by bright yellow solution, filter and washed with dilute hydrochloric acid, be washed with deionized to PH=6.8~7.2, obtain mixed liquor；
(4) by mixed liquor, ground after drying, graphene oxide is made.
2. the preparation method of the graphene oxide according to claim 1 with absorbing property, it is characterised in that the step
In rapid 1 (1), potassium peroxydisulfate, phosphorus pentoxide, the concentrated sulfuric acid are that analysis is pure, and graphite powder used is natural flake graphite, and purity is
99.5%.
3. the preparation method of the graphene oxide according to claim 1 with absorbing property, it is characterised in that the step
In rapid 1 (2), mixing speed is 150~270r/min.
4. the preparation method of the graphene oxide according to claim 1 with absorbing property, it is characterised in that the step
In rapid 1 (2), react and carried out in four-hole boiling flask.
5. the preparation method of the graphene oxide according to claim 1 with absorbing property, it is characterised in that the step
In rapid 2 (1), the speed being slowly added to is 0.5~1.2g/min.
6. the preparation method of the graphene oxide according to claim 1 with absorbing property, it is characterised in that the step
In rapid 2 (2), isoperibol is water bath with thermostatic control.
7. the preparation method of the graphene oxide according to claim 1 with absorbing property, it is characterised in that the step
In rapid 2 (2), the method fully reacted is auxiliary electric stirring mixture；In the step 2 (4), carried out using air dry oven
Drying.
8. the preparation method of the graphene oxide according to claim 1 with absorbing property, it is characterised in that the step
In rapid 2 (2), the flow control of chlorine is 0.1~10m3/h。
9. the preparation method of the graphene oxide according to claim 1 with absorbing property, it is characterised in that the step
In rapid 2 (3), the mass concentration of dilute hydrochloric acid is 5~15%.
10. the preparation method of the graphene oxide according to claim 1 with absorbing property, it is characterised in that described
Graphene oxide with absorbing property prepared by method, its interlamellar spacing is 0.82~.0.91nm, which exists
The magnetic conductivity real part of 17.83GHz Frequency points is 0.96~1.77, and imaginary part is 0.02~0.96；Real part of permittivity is 6.18, empty
Portion is 11.42~2.87.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711472587.6A CN107934952A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation method of the graphene oxide with absorbing property |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711472587.6A CN107934952A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation method of the graphene oxide with absorbing property |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107934952A true CN107934952A (en) | 2018-04-20 |
Family
ID=61936915
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711472587.6A Pending CN107934952A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation method of the graphene oxide with absorbing property |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107934952A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109612177A (en) * | 2018-12-25 | 2019-04-12 | 吉林大学 | A kind of two-dimensional confinement ice and preparation method thereof |
| CN111204753A (en) * | 2020-02-12 | 2020-05-29 | 西安工程大学 | Method for preparing graphene oxide by stripping graphite oxide |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502611A (en) * | 2011-11-15 | 2012-06-20 | 东南大学 | Method for rapidly preparing graphene in large quantities by utilizing graphite oxides |
| CN103910354A (en) * | 2014-03-25 | 2014-07-09 | 复旦大学 | Method for preparing graphene through large-scale aqueous phase |
| WO2014127218A1 (en) * | 2013-02-14 | 2014-08-21 | University Of South Carolina | Defect engineered multilayer epitaxial graphene growth |
| CN104386680A (en) * | 2014-11-14 | 2015-03-04 | 沙嫣 | Method for large-scale preparation of bulky graphene |
| CN105776189A (en) * | 2016-01-30 | 2016-07-20 | 山西大学 | Method for preparing high-purity small oxidized graphene |
| CN106044760A (en) * | 2016-07-28 | 2016-10-26 | 东华大学 | Method for preparing graphene oxide |
-
2017
- 2017-12-29 CN CN201711472587.6A patent/CN107934952A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502611A (en) * | 2011-11-15 | 2012-06-20 | 东南大学 | Method for rapidly preparing graphene in large quantities by utilizing graphite oxides |
| WO2014127218A1 (en) * | 2013-02-14 | 2014-08-21 | University Of South Carolina | Defect engineered multilayer epitaxial graphene growth |
| CN103910354A (en) * | 2014-03-25 | 2014-07-09 | 复旦大学 | Method for preparing graphene through large-scale aqueous phase |
| CN104386680A (en) * | 2014-11-14 | 2015-03-04 | 沙嫣 | Method for large-scale preparation of bulky graphene |
| CN105776189A (en) * | 2016-01-30 | 2016-07-20 | 山西大学 | Method for preparing high-purity small oxidized graphene |
| CN106044760A (en) * | 2016-07-28 | 2016-10-26 | 东华大学 | Method for preparing graphene oxide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109612177A (en) * | 2018-12-25 | 2019-04-12 | 吉林大学 | A kind of two-dimensional confinement ice and preparation method thereof |
| CN111204753A (en) * | 2020-02-12 | 2020-05-29 | 西安工程大学 | Method for preparing graphene oxide by stripping graphite oxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xu et al. | Electrochemical synthesis of ammonia using a cell with a Nafion membrane and SmFe 0.7 Cu 0.3− x Ni x O 3 (x= 0− 0.3) cathode at atmospheric pressure and lower temperature | |
| CN103241983B (en) | Preparation method of graphene oxide modified polycarboxylic acid type water-reducer | |
| CN106219528B (en) | A kind of method of controllable preparation graphene oxide and graphene oxide quantum dot | |
| CN107934952A (en) | A kind of preparation method of the graphene oxide with absorbing property | |
| CN110436508B (en) | Preparation method and application of flaky nano copper oxide | |
| CN104941543B (en) | A kind of preparation method of strong magnetic electricity performance graphene/ferrate composite nano-microsphere | |
| CN101597472A (en) | A kind of method of utilizing copper iron tailings relieving haperacidity burning slag to prepare ferriferrous oxide microwave adsorbing material | |
| CN102910683A (en) | Production method for synthesizing nanoscale oxide iron red through full-wet method | |
| CN1234614C (en) | Manufacture of granular hematite corpuscle | |
| CN105950109B (en) | Redox graphene, stannic oxide and ferric oxide composite material | |
| CN100355699C (en) | Process for making graphite powder with electromagnetic property | |
| CN103506620B (en) | Iron/barium titanate core-shell particles | |
| CN114340371B (en) | Graphene oxide-high-entropy alloy nanocomposite for electromagnetic wave shielding and preparation method and application thereof | |
| CN107454815B (en) | Cu2O/MWCNTs composite material, preparation method and electromagnetic wave absorption application | |
| CN104876274B (en) | A kind of preparation method of mangano-manganic oxide | |
| CN108083266A (en) | A kind of zinc powder reduction graphene oxide prepares the method with absorbing property graphene | |
| CN102442702A (en) | Holmium-doped bismuth ferric multiferroic material and preparation method thereof | |
| CN108539174A (en) | A kind of preparation method of ferrous phosphate lithium/carbon composite material | |
| CN110482540B (en) | Preparation method of graphene oxide powder with good dispersibility | |
| CN106430178B (en) | A kind of microwave chemical preparation method of fine scale sulphur-free expanded graphite | |
| CN106928239B (en) | Graphene-porphyrin type organic nano material and preparation method thereof | |
| CN102502865B (en) | Preparation method of iron oxide brown | |
| CN109231271B (en) | Preparation method of orthorhombic phase nano-belt-shaped molybdenum trioxide | |
| CN107487787A (en) | A kind of hollow KMnF3The preparation method of nanometer square particle | |
| CN114573036A (en) | Porous rod-shaped Fe2O3Preparation method and application of/Ag |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180420 |
|
| RJ01 | Rejection of invention patent application after publication |