CN106800293B - A kind of graphene of part of hydroxyl and preparation method thereof - Google Patents
A kind of graphene of part of hydroxyl and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of the graphene of part of hydroxyl, include the following steps: 1) in ice-water bath, 98% concentrated sulfuric acid is mixed with 30% hydrogen peroxide, stirs evenly, is cooled to room temperature, obtain reaction solution；2) reaction solution is added in ball grinder, and graphite nano plate is added thereto, 1~10h of ball milling obtains reaction product；3) reaction product is diluted in deionized water, neutralizes, using filter, washing, dialysis, drying, obtains hydroxylated graphene.This method simply operates well, is easy to industrializing implementation.
Description
Technical field
The present invention relates to technical field of nano material.More particularly, to the graphene and its system of a kind of part of hydroxyl
Preparation Method.
Background technique
Physicist Andrew Geim and Konstantin Novoselov of Univ Manchester UK etc. was in 2004
Graphene is successfully prepared using micromechanics stripping method, is all dodged from this in the fields such as either chemical, physics or material, electronics
A bright nova.Graphene is a kind of carbonaceous green wood with bi-dimensional cellular shape crystal structure being piled by single layer of carbon atom
Material, there are also the basic structural units of zero dimension fullerene, one-dimensional carbon nanotube and three-dimensional graphite for graphene, thus have many only
Special property.Such as large specific surface area, excellent conduction property, excellent mechanical performance and ultralight quality.Based on graphite
More than alkene various excellent properties, graphene become one of the research hotspot of 21st century each subject.
But if being widely applied it more, we also need to preferably utilize these characteristics of graphene
Its processing performance is improved, dispersibility such as dissolubility and in the base.And there are one in the dispersion process of graphene to ask
Topic, since the graphene of complete structure is made of the benzene hexatomic ring of stable keys, chemical stability is high, the inert state in surface, with
Other medium interactions are weaker, and there are very strong π-π to interact for each interlayer of graphite, cause lamella be stacked and
It is difficult to spread out, is difficult to be scattered in solvent, it more difficult to which equably compound with other organic or inorganic materials, this is to graphene
Further research and application have caused great difficulties, thus improve graphene dispersion by means such as the modifications of functional group
And its become extension graphene application field urgent problem to be solved with the compatibility of various solvents and material.
In early days, the graphene of part functional group is had using oxidation-reduction method preparation, but method is more complex, and it is existing special
In sharp document, has and graphene and highly basic are total to the research of ball milling, but the graphene defect generated in this way is more, to the property of graphene
Matter has some impact on.It can also be handled with nitration mixture, such as be restored with the mixed liquor graphene oxide of nitric acid and sulfuric acid,
Also the graphene of band part oxygen-containing group can be generated, but mixes some nitrogenous toxic gases of release in the method, in environment nocuousness.
In view of the above problems, needing to provide a kind of method of the graphene of new part of hydroxyl simple for process.
Summary of the invention
The first purpose of this invention is to provide a kind of preparation method of the graphene of part of hydroxyl, the preparation method
Simple process and environmental protection, and the degree of hydroxylation for the part of hydroxyl graphite alkene being prepared is 5~20%, the hydroxylating uniformity
It is good, and gained part of hydroxyl graphite alkene with a thickness of 0.35~10nm.
Second object of the present invention is to provide the hydroxyl that the preparation method of above-mentioned hydroxylated graphene is prepared
The graphene of change.
In order to achieve the above first purpose, the present invention adopts the following technical solutions:
A kind of preparation method of the graphene of part of hydroxyl, includes the following steps:
1) in ice-water bath, 98% concentrated sulfuric acid is mixed with 30% hydrogen peroxide, stirs evenly, is cooled to room temperature, obtain
Reaction solution；
2) reaction solution is added in ball grinder, and graphite nano plate is added thereto, 1~10h of ball milling must react production
Object；
3) reaction product is diluted in deionized water, neutralizes, using filter, washing, dialysis, drying, obtains part of hydroxyl
The graphene of change.
Preferably, in step 1), the volume ratio that hydrogen peroxide is mixed with the concentrated sulfuric acid is 1:1~30；It is highly preferred that hydrogen peroxide with
The volume ratio of concentrated sulfuric acid mixing is 1:1~10；Most preferably, the volume ratio that hydrogen peroxide is mixed with the concentrated sulfuric acid is 1:2~5, at this point,
Hydroxylated degree more it is high more evenly, and the thickness of obtained part of hydroxyl graphite alkene more it is small more evenly.
Preferably, in step 2), the graphite nano plate with a thickness of 10~100nm, preferably 30~100nm.
Preferably, in step 2), rotational speed of ball-mill is 50~300rpm；More preferably 100~200rpm, at this point, more helping
In obtaining, thickness is smaller and part of hydroxyl graphite alkene more evenly.
Preferably, in step 2), the time of ball-milling reaction is 3~6h；It is highly preferred that the time of ball-milling reaction is 3~4h,
Ball-milling reaction overlong time, the degree of hydroxylation and thickness dispersibility of graphene are poor, in nano cellulose composite film
Conductivity is also low；The ball-milling reaction time is too short, then the thickness of graphene is blocked up, bad dispersibility.
Preferably, in step 2), the additive amount ratio of the graphite nano plate and reaction solution is 0.8mg:1mL~1.2mg:
1mL, when the two additive amount ratio is excessive, then more difficult hydroxylating；The two additive amount ratio is too small, influences not on degree of hydroxylation
Greatly, but it will cause wastage of material.
Preferably, in step 3), it is described by reaction product be diluted to the extension rate in deionized water be 15~25 times.
Preferably, in step 3), the pH after neutralization is 7~12；It is highly preferred that the pH after neutralizing is 8~11.
Preferably, described to be filtered into suction filtration in step 3), filtering filtering filter membrane used is water system, and aperture is 0.1~0.4 μ
m；It is highly preferred that aperture is 0.1~0.2 μm.
Preferably, in step 3), when the dialysis, the molecular cut off of bag filter is 1000~14000 dalton.
Preferably, in step 3), the degree of hydroxylation of the hydroxylated graphene is 5~20%, preferably hydroxylating journey
Degree is 10~20%；With a thickness of 0.35~10nm.
The hydroxylated graphene that the present invention also protects the preparation method of above-mentioned hydroxylated graphene to be prepared.
The hydroxylated graphene is single layer (generally, it is considered that the graphene thickness of single layer is about 0.35nm thickness) or multilayer
Powder, with a thickness of 0.35~10nm.
The graphene for the part of hydroxyl that preparation method of the invention is prepared can be applied to compound with nano-cellulose
Composite membrane is prepared, in obtained composite membrane, when hydroxylated graphene content is up to 8% or more, which, which has, is led
Electrically, and conductivity is higher.
98% concentrated sulfuric acid refers to that conventional mass fraction is 98% sulfuric acid solution in the present invention；30% hydrogen peroxide is
Refer to that mass concentration is 30% hydrogen peroxide solution.In addition, unless otherwise specified, raw material used in the present invention can be by commercially available
Purchase obtains.
Beneficial effects of the present invention are as follows:
It is preparation method simple process of the invention, environmental protection, low in cost, and the graphene for the part of hydroxyl being prepared
Granularity is small, and epigranular, is easy to be dispersed in water, ethyl alcohol steadily in the long term, in n,N-Dimethylformamide equal solvent.In addition,
To the graphene of part of hydroxyl be easy to modify, can preferably be carried out with other basis materials compound, and compatibility is good, matrix
The performances such as the conduction of material can be improved preferably.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 shows the scanning electron microscope of raw graphite nanometer sheet used in 1 preparation method of the embodiment of the present invention
Photo (SEM).
The scanning electron microscope photograph of the graphene for the part of hydroxyl being prepared Fig. 2 shows the embodiment of the present invention 1
Piece (SEM).
Fig. 3 shows the atomic force microscopy of the graphene for the part of hydroxyl that embodiment 5 is prepared.
Fig. 4 shows the modified graphene (a) of hydroxylating in embodiment 5 and raw graphite nanometer sheet (b) in water
Dispersion, wherein A is the state being just dispersed in water, and B is to stand the state after 2h in water.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further below with reference to preferred embodiments and drawings
It is bright.Similar component is indicated in attached drawing with identical appended drawing reference.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
A kind of preparation method of the graphene of part of hydroxyl, steps are as follows:
It measures 30% hydrogen peroxide that volume ratio is 1:3 and 98% concentrated sulfuric acid will be above-mentioned then in ice water bath environment
Hydrogen peroxide is poured slowly into the concentrated sulfuric acid, and is constantly stirred to uniform, is then cooled to room temperature, is obtained reaction solution；It will reaction
Liquid is added in ball grinder, and the graphite nano plate being added thereto with a thickness of 10~100nm, wherein graphite nano plate and anti-
The mixed proportion for answering liquid is that 0.8mg graphite nano plate is added in every milliliter of reaction solution, carries out ball milling, rotational speed of ball-mill 100rpm, ball
Time consuming is 4h, obtains reaction product；Reaction product is poured slowly into a large amount of deionized water and is diluted, in the process constantly
It is stirred quickening heat dissipation, it is 8 that sodium hydroxide solution, which is then added, and is neutralized to pH value, stands 10min or so, uses vacuum circulated water
Pump carries out filtered off with suction, filter sizes are 0.45 μm, washing to neutrality, later in the dialysis that molecular cut off is 7000 dalton
It dialyses in bag, is finally freeze-dried (- 80 DEG C), obtains the graphene of part of hydroxyl.
Through EDS and AFM it is found that the degree of hydroxylation of the hydroxylated graphene of gained is 14%~17%, gained hydroxylating
Graphene with a thickness of 0.35~15nm, be uniformly dispersed in water, obtained hydroxylated graphene can be stood in water
6h keeps finely dispersed state.
Fig. 1 shows the electron scanning micrograph of raw graphite nanometer sheet used in preparation process, can from figure
Find out, graphite nano plate is thicker.
Fig. 2 shows the electron scanning micrographs for the hydroxylated graphene being prepared, it is seen that stone
Black alkene is relatively thin lamella.
The hydroxylated graphene being prepared is added in nano-cellulose and prepares composite membrane, when hydroxylating in composite membrane
Graphene content be 10% when, composite membrane is conductive, and conductivity reaches 0.9S/m；And will not have after the same method
Hydroxylated graphite nano plate is added in nano-cellulose and prepares composite membrane, and composite membrane does not have electric conductivity.
Embodiment 2
A kind of preparation method of the graphene of part of hydroxyl, steps are as follows:
It measures 30% hydrogen peroxide that volume ratio is 3:7 and 98% concentrated sulfuric acid will be above-mentioned then in ice water bath environment
The concentrated sulfuric acid is poured slowly into hydrogen peroxide, and is constantly stirred to uniform, is then cooled to room temperature, is obtained reaction solution；It will reaction
Liquid is added in ball grinder, and the graphite nano plate being added thereto with a thickness of 10~100nm, wherein graphite nano plate and anti-
The mixed proportion for answering liquid is that 0.9mg graphite nano plate is added in every milliliter of reaction solution, carries out ball milling, rotational speed of ball-mill 150rpm, ball
Time consuming is 4h, obtains reaction product；Reaction product is poured slowly into a large amount of deionized water and is diluted, in the process constantly
It is stirred quickening heat dissipation, it is 8 that sodium hydroxide solution, which is then added, and is neutralized to pH value, stands 10min or so, uses vacuum circulated water
Pump carries out filtered off with suction, filter sizes are 4 μm, washing to neutrality, later in the bag filter that molecular cut off is 7000 dalton
In dialyse, be finally freeze-dried (- 80 DEG C), obtain the graphene of part of hydroxyl.
Through EDS and AFM it is found that the degree of hydroxylation of the hydroxylated graphene of gained is 10~15%, gained is hydroxylated
Graphene with a thickness of 0.35~20nm, be uniformly dispersed in water, obtained hydroxylated graphene can stand in water 5h guarantor
Hold finely dispersed state.
The hydroxylated graphene being prepared is added in nano-cellulose and prepares composite membrane, when graphene in composite membrane
When content is 10%, composite membrane is conductive, and conductivity reaches 0.7S/m；And it after the same method will be not hydroxylated
Graphite nano plate is added in nano-cellulose and prepares composite membrane, and composite membrane does not have electric conductivity, and reason should be that graphite nano plate exists
Dispersion effect difference fails to form conductive path in nano-cellulose.
Embodiment 3
A kind of preparation method of the graphene of part of hydroxyl, steps are as follows:
It measures 30% hydrogen peroxide that volume ratio is 1:3 and 98% concentrated sulfuric acid will be above-mentioned then in ice water bath environment
The concentrated sulfuric acid is poured slowly into hydrogen peroxide, and is constantly stirred to uniform, is then cooled to room temperature, is obtained reaction solution；It will reaction
Liquid is added in ball grinder, and the graphite nano plate being added thereto with a thickness of 10~100nm, wherein graphite nano plate and anti-
The mixed proportion for answering liquid is that 1.0mg graphite nano plate is added in every milliliter of reaction solution, carries out ball milling, rotational speed of ball-mill 250rpm, ball
Time consuming is 4h, obtains reaction product；Reaction product is poured slowly into a large amount of deionized water and is diluted, in the process constantly
It is stirred quickening heat dissipation, it is 8 that sodium hydroxide solution, which is then added, and is neutralized to pH value, stands 10min or so, uses vacuum circulated water
Pump carries out filtered off with suction, filter sizes are 0.22 μm, washing to neutrality, later in the dialysis that molecular cut off is 7000 dalton
It dialyses in bag, is finally freeze-dried (- 80 DEG C), obtains the graphene of part of hydroxyl.
Through EDS and AFM it is found that the degree of hydroxylation of the hydroxylated graphene of gained is 12~16%, gained is hydroxylated
Graphene with a thickness of 0.35~14nm, be uniformly dispersed in water, obtained hydroxylated graphene can stand in water 6h guarantor
Hold finely dispersed state.
The hydroxylated graphene being prepared is added in nano-cellulose and prepares composite membrane, when hydroxylating in composite membrane
Graphene content be 10% when, composite membrane is conductive, and conductivity reaches 0.6S/m；And will not have after the same method
Hydroxylated graphite nano plate is added in nano-cellulose and prepares composite membrane, and composite membrane does not have electric conductivity.
Embodiment 4
A kind of preparation method of the graphene of part of hydroxyl, steps are as follows:
It measures 30% hydrogen peroxide that volume ratio is 1:3 and 98% concentrated sulfuric acid will be above-mentioned then in ice water bath environment
The concentrated sulfuric acid is poured slowly into hydrogen peroxide, and is constantly stirred to uniform, is then cooled to room temperature, is obtained reaction solution；It will reaction
Liquid is added in ball grinder, and the graphite nano plate being added thereto with a thickness of 10~100nm, wherein graphite nano plate and anti-
The mixed proportion for answering liquid is that 1.0mg graphite nano plate is added in every milliliter of reaction solution, carries out ball milling, rotational speed of ball-mill 150rpm, ball
Time consuming is 3h, obtains reaction product；Reaction product is poured slowly into a large amount of deionized water and is diluted, in the process constantly
It is stirred quickening heat dissipation, it is 8 that sodium hydroxide solution, which is then added, and is neutralized to pH value, stands 10min or so, uses vacuum circulated water
Pump carries out filtered off with suction, filter sizes are 0.2 μm, washing to neutrality, later in the dialysis that molecular cut off is 7000 dalton
It dialyses in bag, is finally freeze-dried (- 80 DEG C), obtains the graphene of part of hydroxyl.
EDS and AFM it is found that the hydroxylated graphene of gained degree of hydroxylation be 19~20%, the hydroxylated stone of gained
Black alkene with a thickness of 0.35~7nm, epigranular is uniformly dispersed in water, and obtained hydroxylated graphene is quiet in water
It can still be uniformly dispersed after setting 12h.
The hydroxylated graphene being prepared is added in nano-cellulose and prepares composite membrane, when hydroxylating in composite membrane
Graphene content be 8% when, composite membrane is conductive, and conductivity reaches 1.5S/m；And will not have after the same method
Hydroxylated graphite nano plate is added in nano-cellulose and prepares composite membrane, and composite membrane does not have electric conductivity.
Embodiment 5
A kind of preparation method of the graphene of part of hydroxyl, steps are as follows:
It measures 30% hydrogen peroxide that volume ratio is 3:7 and 98% concentrated sulfuric acid will be above-mentioned then in ice water bath environment
The concentrated sulfuric acid is poured slowly into hydrogen peroxide, and is constantly stirred to uniform, is then cooled to room temperature, is obtained reaction solution；It will reaction
Liquid is added in ball grinder, and the graphite nano plate being added thereto with a thickness of 10~100nm, wherein graphite nano plate and anti-
The mixed proportion for answering liquid is that 1.0mg graphite nano plate is added in every milliliter of reaction solution, carries out ball milling, rotational speed of ball-mill 200rpm, ball
Time consuming is 4h, obtains reaction product；Reaction product is poured slowly into a large amount of deionized water and is diluted, in the process constantly
It is stirred quickening heat dissipation, it is 8 that sodium hydroxide solution, which is then added, and is neutralized to pH value, stands 10min or so, uses vacuum circulated water
Pump carries out filtered off with suction, filter sizes are 0.22 μm, washing to neutrality, later in the dialysis that molecular cut off is 7000 dalton
It dialyses in bag, is finally freeze-dried (- 80 DEG C), obtains the graphene of part of hydroxyl.
Through EDS and AFM it is found that the degree of hydroxylation of the hydroxylated graphene of gained is 17~18%, gained is hydroxylated
Graphene with a thickness of 0.35~10.5nm, epigranular.
Fig. 3 shows the atomic force microscopy for the hydroxylated graphene that the present embodiment is prepared, can from figure
Find out, product has single layer and multi-layer graphene.
Fig. 4 shows the modified graphene (a) of the hydroxylating in the present embodiment and raw graphite nanometer sheet (b) in water
Dispersion.Wherein, A is the state being just dispersed in water, and B is the state stood after 2h.It can be seen from the figure that through this hair
The dispersion performance of bright modified graphene in water is excellent.Continue to stand 5h, is still able to maintain this dispersity.
The hydroxylated graphene being prepared is added in nano-cellulose and prepares composite membrane, when hydroxylating in composite membrane
Graphene content be 10% when, composite membrane is conductive, and conductivity reaches 0.9S/m；And will not have after the same method
Hydroxylated graphite nano plate is added in nano-cellulose and prepares composite membrane, and composite membrane does not have electric conductivity.
Embodiment 6
A kind of preparation method of the graphene of part of hydroxyl, steps are as follows:
It measures 30% hydrogen peroxide that volume ratio is 1:3 and 98% concentrated sulfuric acid will be above-mentioned then in ice water bath environment
The concentrated sulfuric acid is poured slowly into hydrogen peroxide, and is constantly stirred to uniform, is then cooled to room temperature, is obtained reaction solution；It will reaction
Liquid is added in ball grinder, and the graphite nano plate being added thereto with a thickness of 10~100nm, wherein graphite nano plate and anti-
The mixed proportion for answering liquid is that 1.0mg graphite nano plate is added in every milliliter of reaction solution, carries out ball milling, rotational speed of ball-mill 200rpm, ball
Time consuming is 3h, obtains reaction product；Reaction product is poured slowly into a large amount of deionized water and is diluted, in the process constantly
It is stirred quickening heat dissipation, it is 8 that sodium hydroxide solution, which is then added, and is neutralized to pH value, stands 10min or so, uses vacuum circulated water
Pump carries out filtered off with suction, filter sizes are 0.22 μm, washing to neutrality, later in the dialysis that molecular cut off is 7000 dalton
It dialyses in bag, is finally freeze-dried (- 80 DEG C), obtains the graphene of part of hydroxyl.
Through EDS and AFM it is found that the degree of hydroxylation of the hydroxylated graphene of gained is 12~14%, gained is hydroxylated
Graphene with a thickness of 0.35~20nm.
The hydroxylated graphene being prepared is added in nano-cellulose and prepares composite membrane, when hydroxylating in composite membrane
Graphene content be 10% when, composite membrane is conductive, and conductivity reaches 0.7S/m；And will not have after the same method
Hydroxylated graphite nano plate is added in nano-cellulose and prepares composite membrane, and composite membrane does not have electric conductivity.
Embodiment 7
A kind of preparation method of the graphene of part of hydroxyl, steps are as follows:
It measures 30% hydrogen peroxide that volume ratio is 1:15 and 98% concentrated sulfuric acid will be upper then in ice water bath environment
It states the concentrated sulfuric acid to be poured slowly into hydrogen peroxide, and is constantly stirred to uniform, then cool to room temperature, obtain reaction solution；It will be anti-
The graphite nano plate answered liquid to be added in ball grinder, and be added thereto with a thickness of 10~100nm, wherein graphite nano plate with
The mixed proportion of reaction solution is that 1.0mg graphite nano plate is added in every milliliter of reaction solution, carries out ball milling, rotational speed of ball-mill 150rpm,
Ball-milling Time is 3h, obtains reaction product；Back flow reaction product is poured slowly into a large amount of deionized water and is diluted, in the process
It is constantly stirred quickening heat dissipation, it is 8 that sodium hydroxide solution, which is then added, and is neutralized to pH value, stands 10min or so, uses vacuum
Water circulating pump carries out filtered off with suction, filter sizes are 0.22 μm, washing to neutrality, later in molecular cut off be 7000 dalton
Bag filter in dialyse, be finally freeze-dried (- 80 DEG C), obtain the graphene of part of hydroxyl.
Through EDS and AFM it is found that the degree of hydroxylation of the hydroxylated graphene of gained is 8~10%, the hydroxylated stone of gained
Black alkene with a thickness of 0.35~20nm.
The hydroxylated graphene being prepared is added in nano-cellulose and prepares composite membrane, when hydroxylating in composite membrane
Graphene content be 15% when, composite membrane is conductive, and conductivity reaches 0.6S/m；And will not have after the same method
Hydroxylated graphite nano plate is added in nano-cellulose and prepares composite membrane, and composite membrane does not have electric conductivity.
Comparative example 1
Embodiment 4 is repeated, difference is, changes rotational speed of ball-mill into 400rpm, remaining condition is constant, the hydroxyl being prepared
The degree of hydroxylation of the graphene of change differs between 3%~7%, the thickness of the hydroxylated graphene of gained 3.5~50nm it
Between, difference in thickness is larger.After obtained hydroxylated graphene is stood in water, it only can be uniformly dispersed 3h.
Composite membrane is prepared according to the method in embodiment 4, it is multiple when graphene content hydroxylated in composite membrane is to 15%
It closes film and just embodies electric conductivity, and conductivity only reaches 0.4S/m.
Comparative example 2
Embodiment 4 is repeated, difference is, changes rotational speed of ball-mill into 50rpm, remaining condition is constant, when Ball-milling Time is 3h,
The thickness of obtained graphene is in 30~80nm etc., and when Ball-milling Time extends to 8h, the thickness of graphene is still being dispersed in
Between 25~70nm.After obtained hydroxylated graphene is stood in water, it only can be uniformly dispersed 2h.
Comparative example 3
Embodiment 4 is repeated, difference is, Ball-milling Time is extended to 8h, remaining condition is constant, the hydroxylating being prepared
The degree of hydroxylation of graphene differed between 6%~15%, the thickness of the hydroxylated graphene of gained 3.5~30nm it
Between.After obtained hydroxylated graphene is stood in water, it only can be uniformly dispersed 4h.
Comparative example 4
Embodiment 4 is repeated, difference is, the additive amount of graphite nano plate is changed to 2mg/mL reaction solution, remaining condition is not
Become, the degree of hydroxylation for the hydroxylated graphene being prepared is only 2%~7%.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (2)
1. a kind of preparation method of the graphene of part of hydroxyl, which comprises the steps of:
1) in ice-water bath, 98% concentrated sulfuric acid is mixed with 30% hydrogen peroxide, stirs evenly, is cooled to room temperature, must react
Liquid；The volume ratio that hydrogen peroxide is mixed with the concentrated sulfuric acid is 1: 2~5；
2) reaction solution is added in ball grinder, and graphite nano plate is added thereto, 3~4h of ball milling obtains reaction product；Its
In, rotational speed of ball-mill is 100~200rpm；The additive amount of the graphite nano plate and reaction solution ratio is 0.8mg: 1mL~1.2mg:
1mL；The graphite nano plate with a thickness of 30~100nm；
3) reaction product is diluted in deionized water, neutralizes, using filter, washing, dialysis, drying, obtains part of hydroxyl
Graphene；It is 15~25 times that reaction product, which is diluted to the extension rate in deionized water, and the pH after neutralization is 8~11；Filtering filter
The aperture of film is 0.1~0.2 μm；When dialysis, the molecular cut off of bag filter is 1000~14000 dalton；The hydroxylating
Graphene degree of hydroxylation be 10~20%, with a thickness of 0.35~10nm.
2. the graphene for the part of hydroxyl that preparation method as described in claim 1 is prepared.
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| CN110773142A (en) * | 2019-11-14 | 2020-02-11 | 嘉兴烯成新材料有限公司 | Preparation and application of reduced hydroxylated graphene composite semiconductor catalyst |
| CN113173580A (en) * | 2021-05-19 | 2021-07-27 | 湖北省黄麦岭磷化工有限责任公司 | Preparation method of graphene |
| CN114590805A (en) * | 2022-03-31 | 2022-06-07 | 昆明云天墨睿科技有限公司 | Method for macroscopic preparation of hydroxyl-rich epoxy graphene oxide |
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| CN102225759A (en) * | 2011-04-14 | 2011-10-26 | 温州医学院 | Low-temperature preparation method of hydroxy-functionalized graphene |
| CN103788413A (en) * | 2014-01-24 | 2014-05-14 | 济南大学 | Method for chemically modifying inorganic filler with graphene oxide, product and application |
| CN104591117A (en) * | 2014-12-26 | 2015-05-06 | 江南大学 | Three-dimensional carbon nanometer tube/graphene hybrid material and preparation method thereof |
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