CN105985140A - Graphene and ceramic composite film and preparation method thereof - Google Patents
Graphene and ceramic composite film and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of filtering film preparation and particularly relates to a preparation method of a ceramic filtering film combined with graphene. The preparation method comprises the steps that graphite serves as the raw material, graphene oxide is prepared through sufficient intercalation oxidation, and a graphene oxide solution is prepared; the graphene oxide solution is sprayed to the surface of microporous ceramic; reduction is carried out under the conditions of a high temperature and an inert atmosphere, and the ceramic filtering film combined with graphene is obtained. According to the preparation method, the graphene oxide solution is attached to the surface of a ceramic filtering film in a spraying mode, graphene oxide is reduced under the conditions of a high temperature and an inert atmosphere, and thus the ceramic filtering film combined with graphene is formed, so that the binding force between graphene and the ceramic filtering film is improved, and the service life of the ceramic filtering film combined with graphene is prolonged; the prepared ceramic filtering film combined with graphene is long in service life, the filtration and separation effects are remarkably improved, the preparation method is simple, industrial production is easy, and the ceramic filtering film combined with graphene can be widely applied to the technical field of seawater desalination or wastewater treatment.
Description
Technical field
The present invention relates to the preparation method of the ceramic filter membrane of a kind of composite graphite alkene, belong to filtration membrane preparing technical field.
Background technology
Water resource is the base substance that the mankind depend on for existence; but with the industrialized development in the whole world and progress; the phenomenon of water resource pollution is increasingly severe; the crisis of facing mankind water resource has become the fact that can not argue; particularly China is populous; distribution of water resources is uneven, and lack of water is day by day serious.Although government has increased the input to environmental protection and sewage disposal, but China's water pollution situation is still very severe, and every gross contamination emission is very big, and pollution level is still at a relatively high level.Therefore, emphasis and the focus that water resource is research at present all the time how is efficiently utilized.
At present, for the method for sewage disposal, generally using ceramic membrane to carry out filtration treatment, ceramic membrane is because its intensity is high and resistance to chemical attack, cleaning and regeneration performance is good, has both and has high efficiency filter to have particularly important application in desalinization and sewage disposal with the two-fold advantage of secondary filter.But during ceramic membrane processes sewage, frangible mechanical strength does not still reach requirement, and service life is short.
Graphene, as new a member of material with carbon element, just causes the very big of scientific research personnel after 2004 are successfully prepared and pays close attention to because of its various excellent characteristic showing.Graphene is as the highest a member of specific surface area in material with carbon element, and its specific surface area is about 2630m2/g, adds that the chemical stability of its brilliance and the mechanical strength of superelevation make it have great potentiality in terms of adsorption filtration field.Therefore, how Graphene is combined with ceramic membrane and is applied to water treatment field by research, and the effect improving ceramic membrane process sewage is highly important problem.
For solving above-mentioned technical problem, Chinese patent literature CN 102908908 discloses a kind of method using graphene oxide modification ceramic micro filter film, prepare graphene oxide with graphite for raw material, graphene oxide is dispersed into the aqueous solution that solid content is 0.01 ~ 0.1wt%, ceramic micro filter film vacuum impregnation is in graphene oxide solution, drying is to graphene oxide modification ceramic micro filter film, this invention is by being immersed in ceramic filtration membrane by graphene oxide and being dried, the performance utilizing graphene oxide improves ceramic micro filter membrane separation efficiency, extend the service life of ceramic filtration membrane.
Graphene oxide modification ceramic micro filter film disclosed in above-mentioned patent document, after the graphene oxide being immersed in ceramic filtration membrane is dried, when crossing drainage, water is continuously applied to certain impulsive force to ceramic filtration membrane, ceramic membrane and the graphene oxide on it are only combined by the power between molecule, inevitably easily coming off, and graphene oxide being easily dissolved in aqueous medium, the filter efficiency causing ceramic filtration membrane is still very low；Additionally, during preparation method, graphene oxide is by being immersed in ceramic filtration membrane, and impregnation method easily blocks the micropore in ceramic filtration membrane..
Content of the invention
Therefore, invent technical problem to be solved be to overcome in prior art graphene oxide to modify ceramic filtration membrane filter efficiency is low, adhesion therebetween is low and the susceptible to plugging defect of ceramic filtration membrane micropore, thus provide the multiple Graphene that a kind of filter efficiency is high to close ceramic filtration membrane.
To this end, the present invention provides the preparation method of the ceramic filter membrane of a kind of composite graphite alkene, comprise the following steps:
With graphite as raw material, prepare graphene oxide by sufficient intercalation oxidation, and configure graphene oxide solution；
Graphene oxide solution is coated on the surface of micropore ceramic filter film, forms graphene oxide film layer；
Carry out reducing under high temperature, inert atmosphere conditions or electronation obtains the ceramic filter membrane of composite graphite alkene.
In the preparation method of the ceramic filter membrane of above-mentioned composite graphite alkene, the size of described graphene oxide is 2～10um.
In the preparation method of the ceramic filter membrane of above-mentioned composite graphite alkene, the concentration of described graphene oxide solution is 0.5～10mg/ml.
In the preparation method of the ceramic filter membrane of above-mentioned composite graphite alkene, graphene oxide is prepared in described intercalation oxidation, first by lyophilized for the graphene oxide solid oxidation Graphene that obtains, then dissolves solid oxidation Graphene in a solvent, forms graphene oxide solution.
In the preparation method of the ceramic filter membrane of above-mentioned composite graphite alkene, described solvent is alcohol solution, alkanes solution, any one or three kinds of mixed liquors coordinating with arbitrary proportion in the aqueous solution.
In the preparation method of the ceramic filter membrane of above-mentioned composite graphite alkene, described alcohol solution is methyl alcohol, ethanol, propyl alcohol, any one in butanol；Described alkanes solution is methane, ethane, propane, butane, any one in n-butanol methane.
In the preparation method of the ceramic filter membrane of above-mentioned composite graphite alkene, described graphene oxide is coated in micropore ceramics surface method be spraying process, sedimentation, in czochralski method any one, it is attached to described graphene oxide solution on ceramic filter membrane, and form graphene oxide layer.
In the preparation method of the ceramic filter membrane of above-mentioned composite graphite alkene, the inert atmosphere of described graphene oxide high temperature reduction is nitrogen, argon gas, any one in neon；The temperature of described graphene oxide reduction is 1200～1500 DEG C, and the recovery time is 24～48h.
In the preparation method of the ceramic filter membrane of above-mentioned composite graphite alkene, the flow velocity of described inert gas is 10～60mL/min；Described graphene oxide reduction temperature is 1350～1450 DEG C；Reduction temperature heating rate is 2～8 DEG C/min, and the described recovery time is 30～44h.
In the preparation method of the ceramic filter membrane of above-mentioned composite graphite alkene, described electronation uses reduces in reductant solution, or reduces at the steam of reducing agent；Described chemical reducing agent is hydrazine hydrate, hydroiodic acid, any one in sodium borohydride；The temperature of described reducing agent steam reduction is 50
~ 90 DEG C, the recovery time is 12 ~ 72h；The time of described reductant solution reduction is 1 ~ 5h.
The preparation method of the ceramic filter membrane of a kind of composite graphite alkene of the present invention has the advantage that
1. the preparation method of the ceramic filter membrane of a kind of composite graphite alkene of the present invention, by being first lyophilized graphene oxide, it is dissolved into solution again, and it is ultrasonically formed homodisperse graphene oxide solution, replace impregnation method of the prior art by spraying method, graphene oxide solution is attached on the surface of ceramic filter film, and form graphene oxide thin layer, avoid the micropore of impregnation method blocking ceramic filter membrane in prior art, thus improve the filtration separative efficiency of ceramic filter film.
2. the preparation method of the ceramic filter membrane of a kind of composite graphite alkene of the present invention, carry out reduction treatment by will be attached to the graphene oxide on ceramic filter membrane surface under high temperature, inert conditions or with chemical reducing agent, graphene oxide is reduced into Graphene, form the ceramic filter membrane of composite graphite alkene, improve Graphene and ceramic filter membrane adhesion between the two, improve the service life of Graphene composite ceramics filter membrane；Simultaneously by control reduction temperature, carry out redox graphene, reduction temperature can not be too high, too high meeting causes ceramic filter membrane frangible, temperature can not be too low, the too low meeting of temperature causes graphene oxide cannot be reduced into Graphene, and and ceramic filter membrane between adhesion insecure, thus affect the serviceability of ceramic filter membrane.Therefore, the preparation method of the ceramic filter membrane of the composite graphite alkene that the present invention provides, the composite graphite alkene ceramic filter membrane length in service life prepared, filter separating effect and significantly improve and preparation method is simple and is easy to industrialized production, can be widely applied to desalinization or technical field of sewage.
Brief description
Fig. 1 is pottery (left) and graphene oxide composite ceramics filter membrane (right) pictorial diagram of embodiment 1 offer.
Fig. 2 is the pictorial diagram of the composite graphite alkene ceramic filter membrane that embodiment 1 provides.
Fig. 3 is the SEM collection of illustrative plates of the uncoated Graphene ceramic filter membrane that embodiment 1 provides.
Fig. 4 is the Graphene composite ceramics filter membrane through high temperature reduction that embodiment 1 provides.
Detailed description of the invention
Embodiment 1
The preparation of graphene oxide: the expansible graphite of microwave treatment 100 mesh in advance, then successively add the concentrated sulfuric acid and permanganic acid respectively 30 DEG C, 60 DEG C, fully react under 90 DEG C of temperature conditionss, abundant intercalation obtains graphene oxide, and the hydrochloric acid solution high speed centrifuge washing in deionized water, 1mol/ml prepares graphene oxide colloidal sol respectively, freeze-dried 3 days again, prepare solid-state like graphene oxide；With the mixed liquor of the first alcohol and water that volume ratio is 3:1 as solvent, compound concentration is the graphene oxide solution of 1.5mg/ml, and ultrasonic 40min in ultrasonic wave, is sufficiently formed finely dispersed graphene oxide solution.
The ceramic filter membrane of spraying graphene oxide: utilize spray gun and connect nitrogen, the graphene oxide solution of the 1.5mg/ml having configured is uniformly sprayed on ceramic filter membrane inner surface, first spray one layer, next layer is sprayed again after to be dried, regulated the thickness of graphene oxide solution by the number of plies of control spraying graphene oxide, spray the graphene oxide of different-thickness according to demand, after being dried, obtain spraying the ceramic filter membrane of graphene oxide layer.
The ceramic filter membrane of composite graphite alkene: the ceramic filter membrane of above-mentioned spraying graphene oxide layer is put in tube furnace, being passed through flow velocity in tube furnace in quartz ampoule is 10mL/min nitrogen, heating rate be 2 DEG C/min by quartz ampoule in temperature rise to 1200 DEG C, reductase 12 4h graphene oxide under constant temperature, finally obtains the ceramic filter membrane of composite graphite alkene.
The present embodiment is by the ceramic filter membrane pictorial diagram of ceramic coated for graphene oxide filter membrane, composite graphite alkene respectively as depicted in figs. 1 and 2, and SEM electron microscope scanning analysis is carried out respectively to the ceramic filter membrane of non-graphite spraying alkene, the ceramic filter membrane of composite graphite alkene, its result is respectively as shown in Figure 3 and Figure 4, Fig. 3 can be learnt that pore channel is more flourishing, but aperture is bigger, filter effect is poor, particularly can not cross the various harmful metal impurities ion in drainage；Fig. 4 is the ceramic membrane SEM collection of illustrative plates being coated with Graphene, with Fig. 3 contrast this it appears that, surface covers a layer graphene layer, the aperture gathered is invisible, owing to Graphene has excellent adsorption filtration ability to some harmful metal ions, therefore, when ceramic membrane surface is coated with graphene layer, the harmful ion in water can directly be removed very easily.
Embodiment 2
The preparation of graphene oxide: the expansible graphite of microwave treatment 100 mesh in advance, then successively add the concentrated sulfuric acid and permanganic acid respectively 40 DEG C, 70 DEG C, fully react under 90 DEG C of temperature conditionss, abundant intercalation obtains graphene oxide, and the hydrochloric acid solution high speed centrifuge washing in deionized water, 0.8mol/ml prepares graphene oxide colloidal sol respectively, freeze-dried 2 days again, prepare solid-state like graphene oxide；With the mixed liquor of the second alcohol and water that volume ratio is 4:1 as solvent, compound concentration is the graphene oxide solution of 5mg/ml, and passes through the ultrasonic 90min of ultrasonic cell-break machine, is sufficiently formed finely dispersed graphene oxide solution.
Ceramic filter membrane by czochralski method spraying graphene oxide: the graphene oxide solution that concentration is 5mg/ml is uniformly and quickly flow through ceramic filter membrane inwall, the flow velocity of control liquid, thus on ceramic filter membrane inwall, it is evenly coated with one layer of graphene oxide layer, natural air drying, repeat the above steps, apply multilayer continuously at ceramic filter membrane inwall, form multilayer oxygen functionalized graphene and be dried.
The ceramic filter membrane of composite graphite alkene: the ceramic filter membrane of above-mentioned coating graphene oxide is placed on tube furnace, it is passed through the argon gas that flow is 25ml/min in the quartz ampoule of tube furnace, keep the inert atmosphere in reduction process, and temperature in pipe is risen to 1300 DEG C with the speed of 6 DEG C/min, reduction 44h, the ceramic filter membrane of the composite graphite alkene of preparation under constant temperature.
Embodiment 3
The preparation of graphene oxide: the expansible graphite of microwave treatment 100 mesh in advance, then successively add the concentrated sulfuric acid and permanganic acid respectively 35 DEG C, 65 DEG C, fully react under 80 DEG C of temperature conditionss, abundant intercalation obtains graphene oxide, and the hydrochloric acid solution high speed centrifuge washing in deionized water, 0.75mol/ml prepares graphene oxide colloidal sol respectively, freeze-dried 4 days again, prepare solid-state like graphene oxide；With the mixed liquor of the n-butanol methane that volume ratio is 2:1 and water as solvent, compound concentration is the graphene oxide solution of 15mg/ml, and passes through the ultrasonic 120min of ultrasonic cell-break machine, is sufficiently formed finely dispersed graphene oxide solution.
Ceramic filter membrane by sedimentation spraying graphene oxide: first ceramic filter membrane is placed on container bottom as substrate, deionized water is injected in container, the graphene oxide solution of the 15mg/ml of dispersed one layer of configuration on deionized water surface, then the liquid flowing outlet that container bottom is arranged is opened, slowly deionized water is released from outlet at bottom, graphene oxide liquid level slowly declines, last deionized water is discharged, graphene oxide layer is just deposited on ceramic filter membrane surface, redeposited next layer of graphene oxide solution after drying, until reaching expected graphene oxide layer thickness, it is finally dried to obtain the ceramic filter membrane of coating graphene oxide.
The ceramic filter membrane of composite graphite alkene: the ceramic filter membrane of above-mentioned coating graphene oxide is placed on tube furnace, it is passed through the argon gas that flow is 60mL/min in the quartz ampoule of tube furnace, keep the inert atmosphere in reduction process, and temperature in pipe is risen to 1500 DEG C with the speed of 8 DEG C/min, reduction 40h, the ceramic filter membrane of the composite graphite alkene of preparation under constant temperature.
Embodiment 4
The preparation of graphene oxide: the expansible graphite of microwave treatment 200 mesh in advance, then successively add the concentrated sulfuric acid and permanganic acid respectively 40 DEG C, 70 DEG C, fully react under 95 DEG C of temperature conditionss, abundant intercalation obtains graphene oxide, and the hydrochloric acid solution high speed centrifuge washing in deionized water, 1.1mol/ml prepares graphene oxide colloidal sol respectively, freeze-dried 2 days again, prepare solid-state like graphene oxide；With the mixed liquor of the propane that volume ratio is 4:1 and water as solvent, compound concentration is the graphene oxide solution of 10mg/ml, carrys out dispersed graphene oxide by the ultrasonic 65min of ultrasonic cell-break machine.
Ceramic filter membrane by sedimentation spraying graphene oxide: first ceramic filter membrane is placed on container bottom as substrate, deionized water is injected in container, the graphene oxide solution of the 10mg/ml of dispersed one layer of configuration on deionized water surface, then the liquid flowing outlet that container bottom is arranged is opened, slowly deionized water is released from outlet at bottom, graphene oxide liquid level slowly declines, last deionized water is discharged, graphene oxide layer is just deposited on ceramic filter membrane surface, redeposited next layer of graphene oxide solution after drying, until reaching expected graphene oxide layer thickness, it is finally dried to obtain the ceramic filter membrane of coating graphene oxide.
The ceramic filter membrane of composite graphite alkene: the ceramic filter membrane of above-mentioned coating graphene oxide is placed on tube furnace, it is passed through the argon gas that flow is 30mL/min in the quartz ampoule of tube furnace, keep the inert atmosphere in reduction process, and temperature in pipe is risen to 1450 DEG C with the speed of 4 DEG C/min, reduction 30h, the ceramic filter membrane of the composite graphite alkene of preparation under constant temperature.
Embodiment 5
The preparation of graphene oxide: the expansible graphite of microwave treatment 200 mesh in advance, then successively add the concentrated sulfuric acid and permanganic acid respectively 37 DEG C, 72 DEG C, fully react under 93 DEG C of temperature conditionss, abundant intercalation obtains graphene oxide, and the hydrochloric acid solution high speed centrifuge washing in deionized water, 0.95mol/ml prepares graphene oxide colloidal sol respectively, freeze-dried 2 days again, prepare solid-state like graphene oxide；With the mixed liquor of the butane that volume ratio is 5:1 and water as solvent, compound concentration is the graphene oxide solution of 2.5mg/ml, carrys out dispersed graphene oxide by the ultrasonic 25min of ultrasonic cell-break machine.
The ceramic filter membrane of spraying graphene oxide: utilize spray gun and connect nitrogen, the graphene oxide solution of the 2.5mg/ml having configured is uniformly sprayed on ceramic filter membrane inner surface, first spray one layer, next layer is sprayed again after to be dried, regulated the thickness of graphene oxide solution by the number of plies of control spraying graphene oxide, spray the graphene oxide of different-thickness according to demand, after being dried, obtain spraying the ceramic filter membrane of graphene oxide layer.
The ceramic filter membrane of composite graphite alkene: the ceramic filter membrane of above-mentioned coating graphene oxide is placed on tube furnace, it is passed through the neon that flow is 15mL/min in the quartz ampoule of tube furnace, keep the inert atmosphere in reduction process, and temperature in pipe is risen to 1350 DEG C with the speed of 3 DEG C/min, reduction 36h, the ceramic filter membrane of the composite graphite alkene of preparation under constant temperature.
Embodiment 6
The preparation of graphene oxide: the expansible graphite of microwave treatment 200 mesh in advance, then successively add the concentrated sulfuric acid and permanganic acid respectively 37 DEG C, 72 DEG C, fully react under 93 DEG C of temperature conditionss, abundant intercalation obtains graphene oxide, and the hydrochloric acid solution high speed centrifuge washing in deionized water, 0.95mol/ml prepares graphene oxide colloidal sol respectively, freeze-dried 2 days again, prepare solid-state like graphene oxide；With the mixed liquor of the ethane that volume ratio is 5:1 and water as solvent, compound concentration is the graphene oxide solution of 7.5mg/ml, carrys out dispersed graphene oxide by the ultrasonic 45min of ultrasonic cell-break machine.
Ceramic filter membrane by sedimentation spraying graphene oxide: first ceramic filter membrane is placed on container bottom as substrate, deionized water is injected in container, the graphene oxide solution of the 7.5mg/ml of dispersed one layer of configuration on deionized water surface, then the liquid flowing outlet that container bottom is arranged is opened, slowly deionized water is released from outlet at bottom, graphene oxide liquid level slowly declines, last deionized water is discharged, graphene oxide layer is just deposited on ceramic filter membrane surface, redeposited next layer of graphene oxide solution after drying, until reaching expected graphene oxide layer thickness, it is finally dried to obtain the ceramic filter membrane of coating graphene oxide.
The ceramic filter membrane of composite graphite alkene: insert the ceramic filter membrane of above-mentioned coating graphene oxide in airtight hydroiodic acid vapor vessel, and it is heated to 60 DEG C of slow reduction 72h, i.e. can get the ceramic filter membrane of composite graphite alkene.
Embodiment 7
The preparation of graphene oxide: in advance the expansible graphite of 100 mesh is placed in spheroidal graphite 48h in planetary ball mill, the graphite tentatively peeled off, then it is placed on microwave 10min in micro-wave oven and obtain expanded graphite, then successively add the concentrated sulfuric acid and permanganic acid respectively at 0 DEG C, 90 DEG C, fully reacting under 60 DEG C of temperature conditionss, abundant intercalation obtains graphene oxide, it is placed on ultrasonic 30min in ultrasonic cell-break machine, obtain the less graphene oxide solution of the number of plies;And the hydrochloric acid solution high speed centrifuge washing in deionized water, 0.95mol/ml prepares graphene oxide colloidal sol, more freeze-dried 4 days respectively, prepares solid-state like graphene oxide；With the mixed liquor of the methane that volume ratio is 2:1 and water as solvent, compound concentration is the graphene oxide solution of 3mg/ml, carrys out dispersed graphene oxide by the ultrasonic 40min of ultrasonic cell-break machine.
Ceramic filter membrane by czochralski method spraying graphene oxide: the graphene oxide solution that concentration is 3mg/ml is uniformly and quickly flow through ceramic filter membrane inwall, the flow velocity of control liquid, thus on ceramic filter membrane inwall, it is evenly coated with one layer of graphene oxide layer, natural air drying, repeat the above steps, apply multilayer continuously at ceramic filter membrane inwall, form multilayer oxygen functionalized graphene and be dried.
The ceramic filter membrane of composite graphite alkene: insert the ceramic filter membrane of above-mentioned coating graphene oxide in airtight hydrazine hydrate vapor vessel, and it is heated to 50 DEG C of slow reduction 12h, i.e. can get the ceramic filter membrane of composite graphite alkene.
Embodiment 8
The preparation method of the ceramic filter membrane of the composite graphite alkene that the present embodiment provides, different from embodiment 7 is: insert in airtight sodium borohydride vapor vessel by the ceramic filter membrane of coating graphene oxide, and it is heated to 90 DEG C of slow reduction 48h, i.e. can get the ceramic filter membrane of composite graphite alkene.
Embodiment 9
The preparation of graphene oxide: in advance the expansible graphite of 100 mesh is placed in spheroidal graphite 48h in planetary ball mill, the graphite tentatively peeled off, then it is placed on microwave 10min in micro-wave oven and obtain expanded graphite, then successively add the concentrated sulfuric acid and permanganic acid respectively at 10 DEG C, 80 DEG C, fully reacting under 50 DEG C of temperature conditionss, abundant intercalation obtains graphene oxide, it is placed on ultrasonic 40min in ultrasonic cell-break machine, obtain the less graphene oxide solution of the number of plies;And the hydrochloric acid solution high speed centrifuge washing in deionized water, 0.85mol/ml prepares graphene oxide colloidal sol, more freeze-dried 4 days respectively, prepares solid-state like graphene oxide；With the mixed liquor of the fourth alcohol and water that volume ratio is 3:1 as solvent, compound concentration is the graphene oxide solution of 12.5mg/ml, carrys out dispersed graphene oxide by the ultrasonic 60min of ultrasonic cell-break machine.
Ceramic filter membrane by czochralski method spraying graphene oxide: the graphene oxide solution that concentration is 12.5mg/ml is uniformly and quickly flow through ceramic filter membrane inwall, the flow velocity of control liquid, thus on ceramic filter membrane inwall, it is evenly coated with one layer of graphene oxide layer, natural air drying, repeat the above steps, apply multilayer continuously at ceramic filter membrane inwall, form multilayer oxygen functionalized graphene and be dried.
The ceramic filter membrane of composite graphite alkene: the ceramic filter membrane of above-mentioned coating graphene oxide is inserted in sodium borohydride solution, reduction 1h, it is dried to obtain the ceramic filter membrane of composite graphite alkene.
Embodiment 10
The preparation method of the ceramic filter membrane of the composite graphite alkene that the present embodiment provides, different from embodiment 9 is: insert in hydrazine hydrate solution by the ceramic filter membrane of coating graphene oxide, and reduction 3h is dried to obtain the ceramic filter membrane of composite graphite alkene.
Embodiment 11
The preparation method of the ceramic filter membrane of the composite graphite alkene that the present embodiment provides, different from embodiment 9 is: insert in hydroiodic acid solution by the ceramic filter membrane of coating graphene oxide, and reduction 5h is dried to obtain the ceramic filter membrane of composite graphite alkene.
Claims (10)
1. a preparation method for the ceramic filter membrane of composite graphite alkene, comprises the following steps:
With graphite as raw material, prepare graphene oxide by sufficient intercalation oxidation, and configure graphene oxide solution；Graphene oxide solution is coated on the surface of micropore ceramic filter film, forms graphene oxide film layer；Carry out reducing under high temperature, inert atmosphere conditions or electronation obtains the ceramic filter membrane of composite graphite alkene.
2. the preparation method of the ceramic filter membrane of composite graphite alkene according to claim 1, it is characterised in that: the size of described graphene oxide is 2～10um.
3. the preparation method of the ceramic filter membrane of composite graphite alkene according to claim 1 and 2, it is characterised in that: the concentration of described graphene oxide solution is 0.5～10mg/ml.
4. the preparation method of the ceramic filter membrane of the composite graphite alkene according to claim 1-3 is arbitrary, it is characterized in that: graphene oxide is prepared in described intercalation oxidation, first obtain solid oxidation Graphene by lyophilized for graphene oxide, again solid oxidation Graphene is dissolved in a solvent, form graphene oxide solution.
5. the preparation method of the ceramic filter membrane of composite graphite alkene according to claim 4, it is characterised in that: described solvent is alcohol solution, alkanes solution, any one or three kinds of mixed liquors coordinating with arbitrary proportion in the aqueous solution.
6. the preparation method of the ceramic filter membrane of composite graphite alkene according to claim 5, it is characterised in that: described alcohol solution is methyl alcohol, ethanol, propyl alcohol, any one in butanol；Described alkanes solution is methane, ethane, propane, butane, any one in n-butanol methane.
7. the preparation method of the ceramic filter membrane of the composite graphite alkene according to claim 1-6 is arbitrary, it is characterized in that: described graphene oxide is coated in micropore ceramics surface method be spraying process, sedimentation, in czochralski method any one, it is attached to described graphene oxide solution on ceramic filter membrane, and form graphene oxide layer.
8. the preparation method of the ceramic filter membrane of the composite graphite alkene according to claim 1-7 is arbitrary, it is characterised in that: the inert atmosphere of described graphene oxide high temperature reduction is nitrogen, argon gas, any one in neon；The temperature of described graphene oxide reduction is 1200～1500 DEG C, and the recovery time is 24～48h.
9. the preparation method of the ceramic filter membrane of composite graphite alkene according to claim 9, it is characterised in that: the flow velocity of described inert gas is 10～60mL/min；Described graphene oxide reduction temperature is 1350～1450 DEG C；Reduction temperature heating rate is 2～8 DEG C/min, and the described recovery time is 30～44h.
10. the preparation method of the ceramic filter membrane of the composite graphite alkene according to claim 1-7 is arbitrary, it is characterised in that: described electronation uses reduces in reductant solution, or reduces at the steam of reducing agent；Described chemical reducing agent is hydrazine hydrate, hydroiodic acid, any one in sodium borohydride；The temperature of described reducing agent steam reduction is 50 ~ 90 DEG C, and the recovery time is 12～72h；The time of described reductant solution reduction is 1～5h.
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