CN108190870A - A kind of preparation method of mesoporous grapheme material - Google Patents
A kind of preparation method of mesoporous grapheme material Download PDFInfo
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- CN108190870A CN108190870A CN201810203569.6A CN201810203569A CN108190870A CN 108190870 A CN108190870 A CN 108190870A CN 201810203569 A CN201810203569 A CN 201810203569A CN 108190870 A CN108190870 A CN 108190870A
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Abstract
The invention discloses a kind of preparation methods of mesoporous grapheme material, step 1, add graphene oxide into deionized water, then add in poly, and ultrasonic agitation obtains graphene oxide dispersion uniformly to being completely dispersed；Step 2, sodium chloride is added in and is stirred into graphene oxide dispersion to being completely dissolved, then microwave reaction 2h, obtain the second dispersion liquid；Step 3, the second dispersion liquid is added in into vacuum distillation reaction kettle reaction 4h, viscous fluid is obtained after cooling；Step 4, viscous fluid is added in into mold heating reaction 2h, obtains isothermal curing mold；Step 5, isothermal curing mold is put into hermetic electrolyte in absolute methanol and reacts 5h, added in deionized water sealing reflux cell reaction 2h, obtain mesoporous graphene oxide composite material；Step 6, by mesoporous graphene oxide composite material reduction reaction 3h, mesoporous grapheme material is obtained.The present invention solves the problems, such as that mesoporous graphene degree of graphitization is non-uniform.
Description
Technical field
The invention belongs to grapheme material technical fields, and in particular to a kind of preparation method of mesoporous grapheme material.
Background technology
Mesoporous ordered graphene material has due to having the degree of graphitization of height, high structurally ordered degree
Extremely excellent electric conductivity is very beneficial for the transmission of electronics and ion, makes it in energy storage field such as lithium battery and solar energy
The new energy materials such as battery field has boundless application prospect.Moreover, since mesoporous ordered graphene material has
There are huge specific surface area and pore volume so that it has very strong adsorption capacity, therefore equally has in absorbent fields
Very important status, and but also it has very important application in catalyst, hydrogen storage material, pharmaceutical carrier etc.
Prospect.In addition, order mesoporous grapheme material also has many advantages, such as that high temperature resistant, acid and alkali-resistance, intensity are high, conductivity of heat is high.
Order mesoporous grapheme material is not easy to directly at present due to the limitation of the specificity and preparation method of its structure
It is prepared, generally is further graphitized to obtain by preparing ordered mesopore carbon.Current main preparation methods have：(1) it is situated between
Hole carbon high-temp graphitization method.I.e. first using hard template method (mesoporous silicon makees template) or soft template method (block copolymer induction volatilization
Self assembly) ordered mesoporous carbon material is prepared.Then meso-porous carbon material is calcined at a high temperature of more than 2500 DEG C, with
Obtain the material of high graphitization degree.This method needs to carry out at very high temperatures, and since calcination temperature is excessively high, have
The skeleton of sequence mesoporous carbon is easy to occur to collapse on a large scale, and structurally ordered degree is also destroyed, and leads to the mesoporous graphite finally obtained
The decline of alkene material specific surface area is very big, loses its value for preparing and applying；(2) transition metal-catalyzed graphitization method.It is this
Method mixes after ordered mesopore carbon is prepared, by transition metal with meso-porous carbon material, then calcines.With former
Method is compared, and this method can just obtain high-graphitized carbon material at a lower temperature.But due to transition metal with
The mixing of the impossible substantially uniformity of mesoporous carbon, therefore the degree of graphitization of mesoporous grapheme material different location being prepared is non-
It is often uneven, it is unfavorable for its practical application.
Accordingly, it is desirable to provide a kind of new technical solution solves the above problems.
Invention content
For the problems of the prior art, the present invention provides
For realization more than technical purpose, the technical scheme is that：
A kind of preparation method of mesoporous grapheme material, includes the following steps：
Step 1, it adds graphene oxide into deionized water, then adds in poly, ultrasonic agitation is uniformly to complete
Full dispersion, obtains graphene oxide dispersion；
Step 2, sodium chloride is added in and is stirred into graphene oxide dispersion to being completely dissolved, then microwave reaction 1-
3h obtains the second dispersion liquid；
Step 3, the second dispersion liquid is added in into vacuum distillation reaction kettle reaction 3-5h, viscous fluid is obtained after cooling；
Step 4, viscous fluid is added in into mold heating reaction 1-2h, obtains isothermal curing mold；
Step 5, isothermal curing mold is put into hermetic electrolyte in absolute methanol and reacts 3-6h, added in deionized water and seal back
Cell reaction 1-2h is flowed, obtains mesoporous graphene oxide composite material；
Step 6, by mesoporous graphene oxide composite material reduction reaction 2-4h, mesoporous grapheme material is obtained.
The mass concentration of graphene oxide in deionized water in the step 1 is 30-50g/L, the poly
Addition be graphene oxide 40-60%.
The supersonic frequency of ultrasonic agitation in the step 1 is 10-15kHz, and temperature is 40-60 DEG C.
The addition of sodium chloride in the step 2 is the 60-80% of graphene oxide quality, and the stirring of the stirring is fast
It spends for 1000-1500r/min.
The power of microwave reaction in the step 2 is 500-800W, and the temperature of the microwave reaction is 60-70 DEG C.
The reaction temperature of vacuum distillation reaction kettle in the step 3 is 100-120 DEG C, and pressure is the 50- of atmospheric pressure
70%, the volume of the viscous fluid is the 10-15% of the second dispersion liquid volume.
The temperature of heating reaction in the step 4 is 110-150 DEG C, and the thermostat temperature of the isothermal curing mold is
70-90℃。
The addition of absolute methanol in the step 5 is the 70-80% of graphene oxide quality, and the hermetic electrolyte is anti-
The decomposition voltage answered is 10-15V, and electric current 0.2-0.8A, the temperature of the hermetic electrolyte reaction is 40-50 DEG C, and pressure is
0.2-0.4MPa。
The addition of deionized water in the step 5 is the 30-40% of absolute methanol quality, the sealing reflux electrolysis
The reaction temperature of reaction is 70-90 DEG C, pressure 0.3-0.5MPa, decomposition voltage 20-25V, electric current 1.1-1.5A.
For reduction reaction in the step 6 using hydrogen reduction method, the reaction temperature of the hydrogen reduction method is 350-400
℃。
Step 1 is added graphene oxide into deionized water, is then added in poly and is formed good dispersion,
Obtain graphene oxide dispersion；Graphene oxide adds in deionized water and forms suspension, and graphene oxide at this time is formed
Graininess is reunited；The addition of poly can form good dispersibility, and during ultrasonic agitation, ultrasonic clutch energy
The graphene oxide of reunion is disperseed, and promotes poly Molecular Adsorption in surface of graphene oxide, in water formation point
Granular media system.
Sodium chloride is dissolved in dispersion liquid by step 2, and is dissolved by churned mechanically mode, forms graphene oxide
Sodium chloride solution；The connecting key of poly and graphene oxide is opened by the way of microwave reaction, sodium chloride is embedding
Enter, form poly mosaic texture, obtain the mixed liquor of dispersion.
Deionized water is removed the second dispersion liquid by step 3 by way of vacuum distillation, forms sticky system, is gathered simultaneously
The thermoset structure of maleic acid re-forms graphene oxide and sodium chloride solidification, formation frame structure after cooling down
Sticky liquid.
Step 4 adds in viscous fluid in mold, and poly is formed consolidated structures in a heated condition, ensures whole
Curing, by graphene oxide and sodium chloride solidification in a mold, removal distilled water form stable consolidated structures, obtain constant temperature and consolidate
Change mold.
Isothermal curing mold is put into cell reaction in absolute methanol by step 5, is formed using the electric conductivity of methanol stable
Liquid conduction system by poly initial breakdown, and by the exposed appearance of sodium chloride, forms preliminary meso-hole structure；Addition go from
Sub- water can dissolve sodium chloride, form stable sodium chloride electrolyte；And it under the conditions of sealing flows back cell reaction, is protecting
While holding poly and be formed by curing stable framework, sodium chloride electrolyte plays good degradation system, by poly- Malaysia
Acid degradation；Sealing reflux system can cool down methanol gas to form liquid, form methanol/sodium chloride degradation system, carry significantly
Whole degradation effect has been risen, has formed mesoporous graphene oxide.
Step 6 restores mesoporous graphene oxide to form mesoporous grapheme material.
From the above, it can be seen that the present invention has advantages below：
1. the present invention solves the problems, such as that mesoporous graphene degree of graphitization is non-uniform, the mesoporous grapheme material hole of preparation
Gap is uniform, and specific surface is big.
2. preparation method provided by the invention, not only solving prior art preparation method needs temperature controlled problem,
Also solves the influence of other impurities simultaneously.
3. the present invention can not only prepare the meso-hole structure of various specifications, and can weigh using mold-dissolving removal method
Again using sodium chloride, cost, while entire preparation method energy conservation and environmental protection are greatly reduced, meets the requirement of national energy-saving emission reduction.
Specific embodiment
The present invention will be described in detail in conjunction with the embodiments, but does not do any restriction to the claim of the present invention.
Embodiment 1
A kind of preparation method of mesoporous grapheme material, includes the following steps：
Step 1, it adds graphene oxide into deionized water, then adds in poly, ultrasonic agitation is uniformly to complete
Full dispersion, obtains graphene oxide dispersion；
Step 2, sodium chloride is added in and is stirred into graphene oxide dispersion to being completely dissolved, then microwave reaction 1h,
Obtain the second dispersion liquid；
Step 3, the second dispersion liquid is added in into vacuum distillation reaction kettle reaction 3h, viscous fluid is obtained after cooling；
Step 4, viscous fluid is added in into mold heating reaction 1h, obtains isothermal curing mold；
Step 5, isothermal curing mold is put into hermetic electrolyte in absolute methanol and reacts 3h, add in deionized water sealing reflux
Cell reaction 1h obtains mesoporous graphene oxide composite material；
Step 6, by mesoporous graphene oxide composite material reduction reaction 2h, mesoporous grapheme material is obtained.
The mass concentration of graphene oxide in deionized water in the step 1 is 30g/L, and the poly adds
Enter amount is graphene oxide 40%.
The supersonic frequency of ultrasonic agitation in the step 1 is 10kHz, and temperature is 40 DEG C.
The addition of sodium chloride in the step 2 is the 60% of graphene oxide quality, the mixing speed of the stirring
For 1000r/min.
The power of microwave reaction in the step 2 is 500W, and the temperature of the microwave reaction is 60 DEG C.
The reaction temperature of vacuum distillation reaction kettle in the step 3 is 100 DEG C, and pressure is the 50% of atmospheric pressure, described
The volume of viscous fluid is the 10% of the second dispersion liquid volume.
The temperature of heating reaction in the step 4 is 110 DEG C, and the thermostat temperature of the isothermal curing mold is 70 DEG C.
The addition of absolute methanol in the step 5 is the 70% of graphene oxide quality, the hermetic electrolyte reaction
Decomposition voltage for 10V, electric current 0.2A, the temperature of the hermetic electrolyte reaction is 40 DEG C, pressure 0.2MPa.
The addition of deionized water in the step 5 is the 30% of absolute methanol quality, and the sealing reflux electrolysis is anti-
The reaction temperature answered is 70 DEG C, pressure 0.3MPa, decomposition voltage 20V, electric current 1.1A.
For reduction reaction in the step 6 using hydrogen reduction method, the reaction temperature of the hydrogen reduction method is 350 DEG C.
Embodiment 2
A kind of preparation method of mesoporous grapheme material, includes the following steps：
Step 1, it adds graphene oxide into deionized water, then adds in poly, ultrasonic agitation is uniformly to complete
Full dispersion, obtains graphene oxide dispersion；
Step 2, sodium chloride is added in and is stirred into graphene oxide dispersion to being completely dissolved, then microwave reaction 3h,
Obtain the second dispersion liquid；
Step 3, the second dispersion liquid is added in into vacuum distillation reaction kettle reaction 5h, viscous fluid is obtained after cooling；
Step 4, viscous fluid is added in into mold heating reaction 2h, obtains isothermal curing mold；
Step 5, isothermal curing mold is put into hermetic electrolyte in absolute methanol and reacts 6h, add in deionized water sealing reflux
Cell reaction 2h obtains mesoporous graphene oxide composite material；
Step 6, by mesoporous graphene oxide composite material reduction reaction 4h, mesoporous grapheme material is obtained.
The mass concentration of graphene oxide in deionized water in the step 1 is 50g/L, and the poly adds
Enter amount is graphene oxide 60%.
The supersonic frequency of ultrasonic agitation in the step 1 is 15kHz, and temperature is 60 DEG C.
The addition of sodium chloride in the step 2 is the 80% of graphene oxide quality, the mixing speed of the stirring
For 1500r/min.
The power of microwave reaction in the step 2 is 800W, and the temperature of the microwave reaction is 70 DEG C.
The reaction temperature of vacuum distillation reaction kettle in the step 3 is 120 DEG C, and pressure is the 70% of atmospheric pressure, described
The volume of viscous fluid is the 15% of the second dispersion liquid volume.
The temperature of heating reaction in the step 4 is 150 DEG C, and the thermostat temperature of the isothermal curing mold is 90 DEG C.
The addition of absolute methanol in the step 5 is the 80% of graphene oxide quality, the hermetic electrolyte reaction
Decomposition voltage for 15V, electric current 0.8A, the temperature of the hermetic electrolyte reaction is 50 DEG C, pressure 0.4MPa.
The addition of deionized water in the step 5 is the 40% of absolute methanol quality, and the sealing reflux electrolysis is anti-
The reaction temperature answered is 90 DEG C, pressure 0.5MPa, decomposition voltage 25V, electric current 1.1-1.5A.
For reduction reaction in the step 6 using hydrogen reduction method, the reaction temperature of the hydrogen reduction method is 400 DEG C.
Embodiment 3
A kind of preparation method of mesoporous grapheme material, includes the following steps：
Step 1, it adds graphene oxide into deionized water, then adds in poly, ultrasonic agitation is uniformly to complete
Full dispersion, obtains graphene oxide dispersion；
Step 2, sodium chloride is added in and is stirred into graphene oxide dispersion to being completely dissolved, then microwave reaction 2h,
Obtain the second dispersion liquid；
Step 3, the second dispersion liquid is added in into vacuum distillation reaction kettle reaction 4h, viscous fluid is obtained after cooling；
Step 4, viscous fluid is added in into mold heating reaction 2h, obtains isothermal curing mold；
Step 5, isothermal curing mold is put into hermetic electrolyte in absolute methanol and reacts 5h, add in deionized water sealing reflux
Cell reaction 2h obtains mesoporous graphene oxide composite material；
Step 6, by mesoporous graphene oxide composite material reduction reaction 3h, mesoporous grapheme material is obtained.
The mass concentration of graphene oxide in deionized water in the step 1 is 40g/L, and the poly adds
Enter amount is graphene oxide 50%.
The supersonic frequency of ultrasonic agitation in the step 1 is 13kHz, and temperature is 50 DEG C.
The addition of sodium chloride in the step 2 is the 70% of graphene oxide quality, the mixing speed of the stirring
For 1300r/min.
The power of microwave reaction in the step 2 is 600W, and the temperature of the microwave reaction is 65 DEG C.
The reaction temperature of vacuum distillation reaction kettle in the step 3 is 110 DEG C, and pressure is the 60% of atmospheric pressure, described
The volume of viscous fluid is the 13% of the second dispersion liquid volume.
The temperature of heating reaction in the step 4 is 130 DEG C, and the thermostat temperature of the isothermal curing mold is 80 DEG C.
The addition of absolute methanol in the step 5 is the 75% of graphene oxide quality, the hermetic electrolyte reaction
Decomposition voltage for 13V, electric current 0.6A, the temperature of the hermetic electrolyte reaction is 45 DEG C, pressure 0.3MPa.
The addition of deionized water in the step 5 is the 35% of absolute methanol quality, and the sealing reflux electrolysis is anti-
The reaction temperature answered is 80 DEG C, pressure 0.4MPa, decomposition voltage 23V, electric current 1.3A.
For reduction reaction in the step 6 using hydrogen reduction method, the reaction temperature of the hydrogen reduction method is 380 DEG C.
In conclusion the present invention has the following advantages：
1. the present invention solves the problems, such as that mesoporous graphene degree of graphitization is non-uniform, the mesoporous grapheme material hole of preparation
Gap is uniform, and specific surface is big.
2. preparation method provided by the invention, not only solving prior art preparation method needs temperature controlled problem,
Also solves the influence of other impurities simultaneously.
3. the present invention can not only prepare the meso-hole structure of various specifications, and can weigh using mold-dissolving removal method
Again using sodium chloride, cost, while entire preparation method energy conservation and environmental protection are greatly reduced, meets the requirement of national energy-saving emission reduction.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
The described technical solution of inventive embodiments.It will be understood by those of ordinary skill in the art that still the present invention can be carried out
Modification or equivalent replacement, to reach identical technique effect；As long as meeting using needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of preparation method of mesoporous grapheme material, it is characterised in that：Include the following steps：
Step 1, it adds graphene oxide into deionized water, then adds in poly, ultrasonic agitation uniformly to dividing completely
It dissipates, obtains graphene oxide dispersion；
Step 2, sodium chloride is added in and is stirred into graphene oxide dispersion to being completely dissolved, then microwave reaction 1-3h, obtains
To the second dispersion liquid；
Step 3, the second dispersion liquid is added in into vacuum distillation reaction kettle reaction 3-5h, viscous fluid is obtained after cooling；
Step 4, viscous fluid is added in into mold heating reaction 1-2h, obtains isothermal curing mold；
Step 5, isothermal curing mold is put into hermetic electrolyte in absolute methanol and reacts 3-6h, add in deionized water sealing reflux electricity
Solution reaction 1-2h, obtains mesoporous graphene oxide composite material；
Step 6, by mesoporous graphene oxide composite material reduction reaction 2-4h, mesoporous grapheme material is obtained.
2. a kind of preparation method of mesoporous grapheme material according to claim 1, it is characterised in that：In the step 1
Graphene oxide mass concentration in deionized water be 30-50g/L, the addition of the poly is graphene oxide
40-60%.
3. a kind of preparation method of mesoporous grapheme material according to claim 1, it is characterised in that：In the step 1
Ultrasonic agitation supersonic frequency for 10-15kHz, temperature is 40-60 DEG C.
4. a kind of preparation method of mesoporous grapheme material according to claim 1, it is characterised in that：In the step 2
Sodium chloride addition be graphene oxide quality 60-80%, the mixing speed of the stirring is 1000-1500r/min.
5. a kind of preparation method of mesoporous grapheme material according to claim 1, it is characterised in that：In the step 2
Microwave reaction power for 500-800W, the temperature of the microwave reaction is 60-70 DEG C.
6. a kind of preparation method of mesoporous grapheme material according to claim 1, it is characterised in that：In the step 3
Vacuum distillation reaction kettle reaction temperature for 100-120 DEG C, pressure is the 50-70% of atmospheric pressure, the volume of the viscous fluid
It is the 10-15% of the second dispersion liquid volume.
7. a kind of preparation method of mesoporous grapheme material according to claim 1, it is characterised in that：In the step 4
Heating reaction temperature for 110-150 DEG C, the thermostat temperature of the isothermal curing mold is 70-90 DEG C.
8. a kind of preparation method of mesoporous grapheme material according to claim 1, it is characterised in that：In the step 5
Absolute methanol addition be graphene oxide quality 70-80%, the decomposition voltage of hermetic electrolyte reaction is 10-
15V, electric current 0.2-0.8A, the temperature of the hermetic electrolyte reaction is 40-50 DEG C, pressure 0.2-0.4MPa.
9. a kind of preparation method of mesoporous grapheme material according to claim 1, it is characterised in that：In the step 5
Deionized water addition be absolute methanol quality 30-40%, it is described sealing reflux cell reaction reaction temperature be 70-
90 DEG C, pressure 0.3-0.5MPa, decomposition voltage 20-25V, electric current 1.1-1.5A.
10. a kind of preparation method of mesoporous grapheme material according to claim 1, it is characterised in that：In the step 6
Reduction reaction using hydrogen reduction method, the reaction temperature of the hydrogen reduction method is 350-400 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110759335A (en) * | 2019-12-10 | 2020-02-07 | 齐鲁工业大学 | Porous graphene electrode and preparation method thereof |
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| CN104591172A (en) * | 2015-01-22 | 2015-05-06 | 南京理工大学 | Preparation method for graphene |
| CN105449213A (en) * | 2015-12-29 | 2016-03-30 | 哈尔滨工业大学 | Porous graphene-coated modified lithium ion battery cathode material and preparation method thereof |
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| US20120034442A1 (en) * | 2010-08-06 | 2012-02-09 | Lawrence Livermore National Security, Llc | Graphene aerogels |
| KR20130015013A (en) * | 2013-01-14 | 2013-02-12 | 한국화학연구원 | Porous organic-inorganic hybrid materials, method for preparing thereof, adsorbant comprising them and application thereof |
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| CN110759335A (en) * | 2019-12-10 | 2020-02-07 | 齐鲁工业大学 | Porous graphene electrode and preparation method thereof |
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