CN107603225B - A kind of the graphene anti-corrosion film and preparation method of Pasting - Google Patents
A kind of the graphene anti-corrosion film and preparation method of Pasting Download PDFInfo
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Abstract
The invention belongs to the technical fields of anti-corrosion film preparation, provide a kind of the graphene anti-corrosion film and preparation method of Pasting.This method is first using graphite powder as raw material, in N, the dispersion liquid of graphene is made in ultrasound stripping in dinethylformamide, then it is mixed with self-crosslinking organic silicon emulsion, dispersant and stabilizer, spray-dried obtained composite particles, again through calendering film forming and sided corona treatment, the graphene anti-corrosion film of Pasting is obtained.Compared with conventional method, graphene anti-corrosion film prepared by the present invention, adhesion is good, has strict anticorrosion, waterproof, gas-tight and other effects, while whole preparation process is simple, easy to operate, cost is relatively low, easy for construction, it can be achieved that industrialized production.
Description
Technical field
The invention belongs to the technical fields of anti-corrosion film preparation, provide a kind of the graphene anti-corrosion film and system of Pasting
Preparation Method.
Background technology
The two-dimentional carbon material for only one layer of atomic thickness that graphene is made of carbon atom.2004, Britain Man Chesi
Graphene is isolated in especially big physicist An Deliegaimu and the success of Constantine's Nuo Woxiao loves from graphite, it was demonstrated that it
Can be with individualism, therefore two people also obtain Nobel Prize in physics in 2010 jointly.Most as presently found most thin, intensity
Greatly, a kind of strongest novel nano-material of electrical and thermal conductivity --- graphene is referred to as " dark fund ", is " king of new material ".Science
Family even foretells that graphene will start the subversiveness new technology to have swept the globe, a new industrial revolution.
Emerging strategic material of the graphene as forefront, receives the concern of global scientist, multinational all to fight for
The leading position of graphene research and development.Graphene has high-specific surface area, Quick conductive, excellent chemical stability, dashes forward simultaneously
The performances such as the mechanical property, the high-termal conductivity that go out, application range is extremely extensive, from supercomputer to ultracapacitor, arrives compound
Material arrives paint field, and graphene all fully develops talents, and applies most fast possibility just in paint field, is applied including conduction
Material, anticorrosive paint, anti-flaming dope, heat-conductive coating and high intensity coating etc..
Graphene is used to that in coating pure graphene coating and graphene composite coating can be prepared, the former is primarily referred to as pure graphite
Functional coating of alkene the effects that metal surface plays anticorrosion, conduction；The latter be primarily referred to as graphene first with polymer
Then resin compounded prepares functional coating with composite material, graphene can be obviously improved the performance of resin, therefore graphene is multiple
Closing coating becomes the important application research field of graphene.It is the stone of solid phase that current universal technique, which prepares graphene anticorrosive paint,
Black alkene powder is mixed with coating, and graphene substantially has 3 kinds with coating polymer resin compounded method：Melt blending, solution are total
Mixed, in-situ polymerization.Although graphene has excellent anti-corrosion barrier property, current graphene is in anticorrosive paint using presence
The layer for being difficult to the defect disperseed and graphene is easy to be overlapped the defect of aggregation again.In recent years, prepared by domestic and international researcher
Go out graphene film and to it in the expansion research of metal erosion protection field, the graphene film of such Pasting is solving stone
While black alkene reunion sex chromosome mosaicism, also there is advantageous characteristic anti-oxidant, in terms of resistant to liquid burn into antibiont corrosion.
At present certain effect has been achieved in terms of graphene anticorrosive paint, especially graphene anti-corrosion film both at home and abroad.
Its intermediate range is extensively expensive et al. to have invented a kind of method preparing graphene/silicon alkane laminated film in metal surface（Chinese invention patent
Application number 201310533443.2）, the method overcomes graphene film and the weak disadvantage of metal bond strength, there are two types of introducing contains
The silane coupling agent of different chemical functional groups produces a kind of composite membrane, but the preparation process of this method is multiple as transition film layer
It is miscellaneous and of high cost, while there are agglomeration traits for graphene.In addition, Zhao Chongjun et al. has invented a kind of graphene of anti-corrosion/lead
The preparation method of electric polypyrrole composite film（Chinese invention patent application number 201610252725.9）, the method is single using pyrroles
The volatility feature of body, allows the pyrrole monomer of vapor phase to be in contact with graphene oxide solution, to occur on two-phase interface
Redox reaction makes pyrrole monomer be oxidatively polymerized into polypyrrole, while graphene oxide is reduced to graphene, finally in gas
Liquid interface generates graphene/electric polypyrrole laminated film, but this method equally exists that cost is higher, preparation process is complicated asks
Topic, while graphene still remains the non-uniform problem of dispersion, is unfavorable for promoting.
As it can be seen that graphene exists in the prior art in anticorrosive paint using in the presence of defect and the graphite for being difficult to disperse
The layer of alkene is easy to be overlapped the defect of aggregation again, while general graphene film fitting is not close, and preparation process is complicated and cost
High problem.
Invention content
The object of the present invention is to provide the graphene anti-corrosion films and preparation method of a kind of Pasting, are original with graphite powder
Material, in n,N-Dimethylformamide ultrasound stripping be made graphene dispersion liquid, then with self-crosslinking organic silicon emulsion, dispersion
Agent and stabilizer mixing, spray-dried obtained composite particles, then through calendering film forming and sided corona treatment, obtain the graphite of Pasting
Alkene anti-corrosion film.Compared with conventional method, graphene anti-corrosion film prepared by the present invention, adhesion is good, has strict anti-corrosion
Erosion, waterproof, gas-tight and other effects, while whole preparation process is simple, easy to operate, cost is relatively low, easy for construction, it can be achieved that industrial
Metaplasia is produced, and can be solved graphene in conventional method and be applied defect and the graphene for existing and being difficult to disperse in anticorrosive paint
Layer be easy to be overlapped the defect of aggregation again, while solving that general graphene film fitting is not close, and in addition preparation process is multiple
Miscellaneous and of high cost problem.
Specific technical solution of the present invention is as follows：
A kind of preparation method of the graphene anti-corrosion film of Pasting, first using graphite powder as raw material, in N, N- dimethyl methyls
The dispersion liquid of graphene is made in ultrasound stripping in amide, is then mixed with self-crosslinking organic silicon emulsion, dispersant and stabilizer, passes through
Composite particles are made in spray drying, then through calendering film forming and sided corona treatment, obtain the graphene anti-corrosion film of Pasting；It prepares
It is as follows：
（1）The graphite powder of certain mass is added in glass container, the n,N-Dimethylformamide of certain mass is added,
After mixing, vessel port is sealed with preservative film, and container is placed in ice bath, then use ultrasonic cell disrupte machine to it
It is ultrasonically treated, the supernatant of mixture is taken after ultrasound, be added in centrifuge tube, high speed centrifugation, by the supernatant in centrifuge tube
It is transferred in clean container, obtains the dispersion liquid of graphene；
（2）To step（1）A certain amount of self-crosslinking organic silicon emulsion, dispersant and stabilization are added in the dispersion liquid of gained
Agent, strong stirring are uniformly mixed and slurry are made, then dried by spray dryer, obtain composite particles；
（3）Suitable calender is selected, roller rolling velocity and temperature are set, by step（2）Pressure is added in the particle of gained
The feed inlet for prolonging machine, during particle is downtrodden, organosilicon occurs self-crosslinking and forms tridimensional network and form a film, with dispersion
Graphene mutually cooperatively form complete covering, play strict anticorrosion, waterproof, gas-tight and other effects, then to film into
Row sided corona treatment promotes its surface adhesion, obtains the graphene anti-corrosion film of Pasting.
Preferably, step（1）The addition quality of the graphite powder is the 3~5% of n,N-Dimethylformamide quality.
Preferably, step（1）In the entire dispersion process, the temperature of dispersion liquid is no more than 30 DEG C.
Preferably, step（1）The ultrasound treatment patterns are ultrasound 2s, stop 2s, then ultrasound 2s, stop 2s, repeatedly,
It is ultrasonically treated 15~35min altogether.
Preferably, step（1）The rotating speed of the centrifugal treating is 400~600r/min, and centrifugation time is 10~20min.
Preferably, step（2）The dispersant is barium stearate, zinc stearate, magnesium stearate, copper stearate or stearic acid
At least one of calcium；The stabilizer is at least one of pentaerythrite, xylitol or mannitol.
Preferably, step（2）The addition of the self-crosslinking organic silicon emulsion is the 40~60% of dispersion liquid quality；It is described
The addition of dispersant is the 4~8% of dispersion liquid quality；The addition of the stabilizer is the 2~4% of dispersion liquid quality.
Preferably, step（2）The rotating speed of the spray dryer is 18000~25000r/min, spray disk a diameter of 50
~150mm, the dry powder rate of recovery are not less than 95%.
Preferably, step（3）The calender can be two-roll calendar, tri-roll press machine, four-roll calender or five roll-ins
Prolong machine.
Preferably, step（3）The draw ratio of the calender is 2~2.5, and rolling velocity is 50~90m/min, roller temperature
Degree is 100~140 DEG C.
Preferably, step（3）Film forming thickness after the calendering is 10~30 μm.
For how to improve the dispersion problem of graphene, there is a large amount of scientific research personnel to make a series of grind in this respect
Study carefully, method is concentrated mainly on, introducing foreign molecules modified to the surface of graphene, surfactant, introducing macromolecule is added
And doping aromatic series macromolecular etc., also have in the face using the graphene oxide restored or the electrostatic of edge oxygen-containing functional group is arranged
Reprimand effect achievees the purpose that stable dispersion to weaken piece interlayer Van der Waals force.The present invention is molten with n,N-Dimethylformamide
Agent, the method removed using intermittence ultrasound are directly removed with graphite powder and graphene are made, then be centrifuged, can be obtained
Stable graphene dispersing solution.
Spray dryer is a kind of device that can be completed at the same time drying and be granulated.Feed pump can be adjusted according to technological requirement
Pressure, the size of flow, spray orifice, obtain the spheric granules of a certain size required ratio.Spray dryer is that continous way is normal
The one kind for pressing drier makes it with hot air and is dried using special installation by liquid material atomisation.For drying certain
A little thermal sensitivity liquid, suspension or viscous liquid, it can also be used to drying fuel, intermediate, soap powder and inorganic salts etc..The present invention
Composite slurry spray drying is become into composite particles using this principle, in order to roll film forming.
Sided corona treatment is a kind of shock treatment, and the surface of stock can be made to have higher adhesion.Its principle is to utilize
High-frequency high voltage carries out corona discharge on processed stock surface, generates low temperature plasma, and stock surface is made to produce
For raw radical reaction to promote polymer to crosslink, surface is roughening and increases its wetability to polar solvent.Deng from
Daughter is by shocking by electricity and penetrating into stock surface breakdown its molecular structure, and then by the molecular oxidation on stock surface and pole
Change, plasma electric shock erosion surface, to increase the adhesive ability on stock surface.The present invention is using this principle to anti-corrosion film
Surface is handled, and increases its adhesion so that it can directly be bonded, be coated in material surfaces such as metals.
Anti-corrosion film produced by the present invention, with other methods（Such as it is hot bonding or is not used graphene dispersing solution）Anti-corrosion
Film is compared, indoor anticorrosive grade, outdoor anti-corrosion grade, and the peel strength with metallic copper, as shown in table 1.It can be seen that：
The preparation method of the present invention, can effectively improve the antiseptic property of film, and the adhesive strength of enhanced film and metal base.
Table 1
| Performance indicator | Peel strength（kN/m） | Indoor anticorrosive grade | Outdoor anti-corrosion grade |
| Graphene dispersing solution is not used | 3~4 | F1 | W |
| It is hot bonding | 1~1.5 | F2 | WF1~WF2 |
| The method of the present invention | 3~4 | F2 | WF2 |
The present invention provides the graphene anti-corrosion films and preparation method of a kind of Pasting, compared with prior art, dash forward
The characteristics of going out and excellent effect are：
1. graphene anti-corrosion film prepared by the present invention has strict anticorrosion, waterproof, gas-tight and other effects.
2. graphene anti-corrosion film prepared by the present invention, adhesion is good, can directly paste, be coated in the materials table such as metal
Face.
3. the preparation method of the present invention, process is simple, easy to operate, and cost is relatively low, and product is easy for construction, it can be achieved that work
Industry metaplasia is produced.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A kind of the graphene anti-corrosion film and preparation method of Pasting, the detailed process for preparing anti-corrosion film are as follows：
3kg graphite powders are added in glass container, 10kgN, dinethylformamide, after mixing, with guarantor are added
Fresh film seals vessel port, and container is placed in ice bath.Then use ultrasonic cell disrupte machine with the side of 2s on, 2s off
Formula is ultrasonically treated it, stops ultrasound after 35min.Then the supernatant of mixture is taken, is added in centrifuge tube, and centrifuging
With the speed centrifugal treating 10min of 600r/min in machine.Supernatant in centrifuge tube is transferred in clean container, graphite is obtained
The dispersion liquid of alkene；5.5kg self-crosslinkings organic silicon emulsion, 0.6kg barium stearates and 0.2kg sweet dews are added into 10kg dispersion liquids
Alcohol, strong stirring are uniformly mixed and slurry are made, and then by spray dryer, are dried, are answered with the rotating speed of 18000r/min
Close particle；Tri-roll press machine is selected, draw ratio 2.5, rolling velocity 50m/min, roller temperature is 140 DEG C, by compound
The feed inlet of grain addition calender, during particle is downtrodden, organosilicon occurs self-crosslinking formation tridimensional network and forms
Film mutually cooperatively forms complete covering with the graphene of dispersion, plays strict anticorrosion, waterproof, gas-tight and other effects.Then
Sided corona treatment is carried out to film, its surface adhesion is promoted, obtains the graphene anti-corrosion film of Pasting.
To the anti-corrosion film that embodiment 1 obtains, its indoor anticorrosive grade and outdoor anti-corrosion grade are tested, as shown in table 2.It will
It is pasted on metallic copper, is carried out L-type stripping afterwards for 24 hours, is tested its peel strength, as shown in table 2.
Embodiment 2
A kind of the graphene anti-corrosion film and preparation method of Pasting, the detailed process for preparing anti-corrosion film are as follows：
4kg graphite powders are added in glass container, 10kgN, dinethylformamide, after mixing, with guarantor are added
Fresh film seals vessel port, and container is placed in ice bath.Then use ultrasonic cell disrupte machine with the side of 2s on, 2s off
Formula is ultrasonically treated it, stops ultrasound after 35min.Then the supernatant of mixture is taken, is added in centrifuge tube, and centrifuging
With the speed centrifugal treating 12min of 500r/min in machine.Supernatant in centrifuge tube is transferred in clean container, graphite is obtained
The dispersion liquid of alkene；4.5kg self-crosslinkings organic silicon emulsion, 0.5kg calcium stearates and 0.3kg xyloses are added into 10kg dispersion liquids
Alcohol, strong stirring are uniformly mixed and slurry are made, and then by spray dryer, are dried, are answered with the rotating speed of 25000r/min
Close particle；Four-roll calender is selected, draw ratio 2, rolling velocity 50m/min, roller temperature is 100 DEG C, by composite particles
The feed inlet of calender is added, during particle is downtrodden, organosilicon occurs self-crosslinking and forms tridimensional network and form a film,
Complete covering is mutually cooperatively formed with the graphene of dispersion, plays strict anticorrosion, waterproof, gas-tight and other effects.Then right
Film carries out sided corona treatment, promotes its surface adhesion, obtains the graphene anti-corrosion film of Pasting.
To the anti-corrosion film that embodiment 2 obtains, its indoor anticorrosive grade and outdoor anti-corrosion grade are tested, as shown in table 2.It will
It is pasted on metallic copper, is carried out L-type stripping afterwards for 24 hours, is tested its peel strength, as shown in table 2.
Embodiment 3
A kind of the graphene anti-corrosion film and preparation method of Pasting, the detailed process for preparing anti-corrosion film are as follows：
5kg graphite powders are added in glass container, 10kgN, dinethylformamide, after mixing, with guarantor are added
Fresh film seals vessel port, and container is placed in ice bath.Then use ultrasonic cell disrupte machine with the side of 2s on, 2s off
Formula is ultrasonically treated it, stops ultrasound after 25min.Then the supernatant of mixture is taken, is added in centrifuge tube, and centrifuging
With the speed centrifugal treating 11min of 440r/min in machine.Supernatant in centrifuge tube is transferred in clean container, graphite is obtained
The dispersion liquid of alkene；4kg self-crosslinkings organic silicon emulsion, 0.4kg copper stearates and 0.4kg seasons penta 4 are added into 10kg dispersion liquids
Alcohol, strong stirring are uniformly mixed and slurry are made, and then by spray dryer, are dried, are obtained compound with the rotating speed of 1900r/min
Particle；Select five roll calendars, draw ratio 2, rolling velocity 60m/min, roller temperature is 120 DEG C, by composite particles plus
The feed inlet for entering calender, during particle is downtrodden, organosilicon occurs self-crosslinking and forms tridimensional network and form a film, with
The graphene of dispersion mutually cooperatively forms complete covering, plays strict anticorrosion, waterproof, gas-tight and other effects.Then to thin
Film carries out sided corona treatment, promotes its surface adhesion, obtains the graphene anti-corrosion film of Pasting.
To the anti-corrosion film that embodiment 3 obtains, its indoor anticorrosive grade and outdoor anti-corrosion grade are tested, as shown in table 2.It will
It is pasted on metallic copper, is carried out L-type stripping afterwards for 24 hours, is tested its peel strength, as shown in table 2.
Embodiment 4
A kind of the graphene anti-corrosion film and preparation method of Pasting, the detailed process for preparing anti-corrosion film are as follows：
3.5kg graphite powders are added in glass container, 10kgN is added, dinethylformamide is used after mixing
Preservative film seals vessel port, and container is placed in ice bath.Then use ultrasonic cell disrupte machine with 2s on, 2s off
Mode is ultrasonically treated it, stops ultrasound after 30min.Then take the supernatant of mixture, be added in centrifuge tube, and from
With the speed centrifugal treating 18min of 550r/min in scheming.Supernatant in centrifuge tube is transferred in clean container, stone is obtained
The dispersion liquid of black alkene；6kg self-crosslinkings organic silicon emulsion, 0.8kg magnesium stearates and 0.3kg sweet dews are added into 10kg dispersion liquids
Alcohol, strong stirring are uniformly mixed and slurry are made, and then by spray dryer, are dried, are answered with the rotating speed of 22000r/min
Close particle；Four-roll calender is selected, draw ratio 2, rolling velocity 70m/min, roller temperature is 130 DEG C, by composite particles
The feed inlet of calender is added, during particle is downtrodden, organosilicon occurs self-crosslinking and forms tridimensional network and form a film,
Complete covering is mutually cooperatively formed with the graphene of dispersion, plays strict anticorrosion, waterproof, gas-tight and other effects.Then right
Film carries out sided corona treatment, promotes its surface adhesion, obtains the graphene anti-corrosion film of Pasting.
To the anti-corrosion film that embodiment 4 obtains, its indoor anticorrosive grade and outdoor anti-corrosion grade are tested, as shown in table 2.It will
It is pasted on metallic copper, is carried out L-type stripping afterwards for 24 hours, is tested its peel strength, as shown in table 2.
Embodiment 5
A kind of the graphene anti-corrosion film and preparation method of Pasting, the detailed process for preparing anti-corrosion film are as follows：
4.5kg graphite powders are added in glass container, 10kgN is added, dinethylformamide is used after mixing
Preservative film seals vessel port, and container is placed in ice bath.Then use ultrasonic cell disrupte machine with 2s on, 2s off
Mode is ultrasonically treated it, stops ultrasound after 20min.Then take the supernatant of mixture, be added in centrifuge tube, and from
With the speed centrifugal treating 15min of 500r/min in scheming.Supernatant in centrifuge tube is transferred in clean container, stone is obtained
The dispersion liquid of black alkene；5kg self-crosslinkings organic silicon emulsion, 0.6kg zinc stearates and 0.4kg xyloses are added into 10kg dispersion liquids
Alcohol, strong stirring are uniformly mixed and slurry are made, and then by spray dryer, are dried, are answered with the rotating speed of 25000r/min
Close particle；Two-roll calendar is selected, draw ratio 2, rolling velocity 90m/min, roller temperature is 100 DEG C, by composite particles
The feed inlet of calender is added, during particle is downtrodden, organosilicon occurs self-crosslinking and forms tridimensional network and form a film,
Complete covering is mutually cooperatively formed with the graphene of dispersion, plays strict anticorrosion, waterproof, gas-tight and other effects.Then right
Film carries out sided corona treatment, promotes its surface adhesion, obtains the graphene anti-corrosion film of Pasting.
To the anti-corrosion film that embodiment 5 obtains, its indoor anticorrosive grade and outdoor anti-corrosion grade are tested, as shown in table 2.It will
It is pasted on metallic copper, is carried out L-type stripping afterwards for 24 hours, is tested its peel strength, as shown in table 2.
Embodiment 6
A kind of the graphene anti-corrosion film and preparation method of Pasting, the detailed process for preparing anti-corrosion film are as follows：
4kg graphite powders are added in glass container, 10kgN, dinethylformamide, after mixing, with guarantor are added
Fresh film seals vessel port, and container is placed in ice bath.Then use ultrasonic cell disrupte machine with the side of 2s on, 2s off
Formula is ultrasonically treated it, stops ultrasound after 35min.Then the supernatant of mixture is taken, is added in centrifuge tube, and centrifuging
With the speed centrifugal treating 10min of 400r/min in machine.Supernatant in centrifuge tube is transferred in clean container, graphite is obtained
The dispersion liquid of alkene；4.5kg self-crosslinkings organic silicon emulsion, 0.5kg barium stearates and 0.2kg seasons penta 4 are added into 10kg dispersion liquids
Alcohol, strong stirring are uniformly mixed and slurry are made, and then by spray dryer, are dried, are answered with the rotating speed of 18000r/min
Close particle；Tri-roll press machine is selected, draw ratio 2, rolling velocity 50m/min, roller temperature is 140 DEG C, by composite particles
The feed inlet of calender is added, during particle is downtrodden, organosilicon occurs self-crosslinking and forms tridimensional network and form a film,
Complete covering is mutually cooperatively formed with the graphene of dispersion, plays strict anticorrosion, waterproof, gas-tight and other effects.Then right
Film carries out sided corona treatment, promotes its surface adhesion, obtains the graphene anti-corrosion film of Pasting.
To the anti-corrosion film that embodiment 6 obtains, its indoor anticorrosive grade and outdoor anti-corrosion grade are tested, as shown in table 2.It will
It is pasted on metallic copper, is carried out L-type stripping afterwards for 24 hours, is tested its peel strength, as shown in table 2.
Comparative example 1
Graphene dispersing solution is not used, is directly made compound using self-crosslinking organic silicon emulsion, dispersant and stabilizer
Grain, then through calendering film forming and sided corona treatment, other preparation conditions are consistent with embodiment 6.
To the anti-corrosion film that comparative example 1 obtains, its indoor anticorrosive grade and outdoor anti-corrosion grade are tested, as shown in table 2.It will
It is pasted on metallic copper, is carried out L-type stripping afterwards for 24 hours, is tested its peel strength, as shown in table 2.
Comparative example 2
Sided corona treatment is not carried out, is directly hot bonding calendered film with by protection face, other preparation conditions and embodiment 6 one
It causes.
To the anti-corrosion film that comparative example 2 obtains, its indoor anticorrosive grade and outdoor anti-corrosion grade, wherein indoor anticorrosive are tested
Grade is divided into：Indoor anti-moderate corrosion type F1；Indoor resistant to strong corrosion type F2；Outdoor anti-corrosion grade is divided into：Prevent light corrosion type in open air
W；Outdoor anti-moderate corrosion type WF1；Outdoor resistant to strong corrosion type WF2, as shown in table 2.Itself and metallic copper are hot bonding, for 24 hours after
L-type stripping is carried out, tests its peel strength, as shown in table 2.
Table 2
| Performance indicator | Peel strength（kN/m） | Indoor anticorrosive grade | Outdoor anti-corrosion grade |
| Comparative example 1 | 3.45 | F1 | W |
| Comparative example 2 | 1.36 | F2 | WF2 |
| Embodiment 1 | 3.64 | F2 | WF2 |
| Embodiment 2 | 3.25 | F2 | WF2 |
| Embodiment 3 | 3.38 | F2 | WF2 |
| Embodiment 4 | 3.16 | F2 | WF2 |
| Embodiment 5 | 3.27 | F2 | WF2 |
| Embodiment 6 | 3.41 | F2 | WF2 |
Claims (10)
1. a kind of preparation method of the graphene anti-corrosion film of Pasting, which is characterized in that first using graphite powder as raw material, in N, N-
In dimethylformamide ultrasound stripping be made graphene dispersion liquid, then with self-crosslinking organic silicon emulsion, dispersant and stabilization
Agent mixes, spray-dried obtained composite particles, then simultaneously sided corona treatment, the graphene anti-corrosion for obtaining Pasting are thin through calendering film forming
Film, preparation are as follows：
（1）The graphite powder of certain mass is added in glass container, the n,N-Dimethylformamide of certain mass is added, is mixed
After uniformly, vessel port is sealed with preservative film, and container is placed in ice bath, then it is carried out using ultrasonic cell disrupte machine
It is ultrasonically treated, the supernatant of mixture is taken after ultrasound, be added in centrifuge tube, high speed centrifugation, the supernatant in centrifuge tube is shifted
Into clean container, the dispersion liquid of graphene is obtained；
（2）To step（1）A certain amount of self-crosslinking organic silicon emulsion, dispersant and stabilizer are added in the dispersion liquid of gained, by force
Power, which is uniformly mixed, is made slurry, is then dried by spray dryer, obtains composite particles；
（3）Suitable calender is selected, roller rolling velocity and temperature are set, by step（2）Pressure is added in the composite particles of gained
Prolong machine, be pressed into film, sided corona treatment then is carried out to get the graphene anti-corrosion film of Pasting to film.
2. the preparation method of the graphene anti-corrosion film of a kind of Pasting according to claim 1, it is characterised in that：Step
（1）The addition quality of the graphite powder is the 3~5% of n,N-Dimethylformamide quality.
3. the preparation method of the graphene anti-corrosion film of a kind of Pasting according to claim 1, it is characterised in that：Step
（1）In the entire dispersion process, temperature≤30 DEG C of dispersion liquid.
4. the preparation method of the graphene anti-corrosion film of a kind of Pasting according to claim 1, it is characterised in that：Step
（1）The ultrasound treatment patterns are ultrasound 2s, stop 2s, then ultrasound 2s, stop 2s, repeatedly, 15~35min of supersound process altogether.
5. the preparation method of the graphene anti-corrosion film of a kind of Pasting according to claim 1, it is characterised in that：Step
（1）The rotating speed of the high speed centrifugation processing is 400~600r/min, and centrifugation time is 10~20min.
6. the preparation method of the graphene anti-corrosion film of a kind of Pasting according to claim 1, it is characterised in that：Step
（2）The dispersant is at least one of barium stearate, zinc stearate, magnesium stearate, copper stearate or calcium stearate；It is described
Stabilizer is at least one of pentaerythrite, xylitol or mannitol；The addition of the self-crosslinking organic silicon emulsion is point
The 40~60% of dispersion liquid quality；The addition of the dispersant is the 4~8% of dispersion liquid quality；The addition of the stabilizer is
The 2~4% of dispersion liquid quality.
7. the preparation method of the graphene anti-corrosion film of a kind of Pasting according to claim 1, it is characterised in that：Step
（2）The rotating speed of the spray dryer be 18000~25000r/min, a diameter of 50~150mm of spray disk, the dry powder rate of recovery >=
95%。
8. the preparation method of the graphene anti-corrosion film of a kind of Pasting according to claim 1, it is characterised in that：Step
（3）The calender is two-roll calendar, tri-roll press machine, four-roll calender or five roll calendars；The draw ratio of calender is 2
~2.5, rolling velocity is 50~90m/min, and roller temperature is 100~140 DEG C.
9. according to a kind of preparation method of the graphene anti-corrosion film of Pasting of claim 1 or 8, it is characterised in that：Step
Suddenly（3）Film forming thickness after the calendering is 10~30 μm.
10. using the graphene anti-corrosion film for the Pasting that any one of claim 1~9 preparation method is prepared.
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| CN103172062A (en) * | 2013-04-17 | 2013-06-26 | 东南大学 | Preparation method of graphene film for dye-sensitized solar cell counter electrodes |
| CN104118869A (en) * | 2014-07-07 | 2014-10-29 | 苏州世优佳电子科技有限公司 | Preparation method of graphene thin films |
| JP2015229618A (en) * | 2014-06-05 | 2015-12-21 | 国立大学法人北陸先端科学技術大学院大学 | Graphene release agent for chemical release graphene film production and production method of graphene film |
| CN105253878A (en) * | 2015-11-18 | 2016-01-20 | 复旦大学 | Method for directly preparing expanded graphite or graphene under normal temperature and normal pressure |
| CN105860065A (en) * | 2016-04-22 | 2016-08-17 | 华东理工大学 | Preparation method of anti-corrosion graphene/conductive polypyrrole composite thin film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172062A (en) * | 2013-04-17 | 2013-06-26 | 东南大学 | Preparation method of graphene film for dye-sensitized solar cell counter electrodes |
| JP2015229618A (en) * | 2014-06-05 | 2015-12-21 | 国立大学法人北陸先端科学技術大学院大学 | Graphene release agent for chemical release graphene film production and production method of graphene film |
| CN104118869A (en) * | 2014-07-07 | 2014-10-29 | 苏州世优佳电子科技有限公司 | Preparation method of graphene thin films |
| CN105253878A (en) * | 2015-11-18 | 2016-01-20 | 复旦大学 | Method for directly preparing expanded graphite or graphene under normal temperature and normal pressure |
| CN105860065A (en) * | 2016-04-22 | 2016-08-17 | 华东理工大学 | Preparation method of anti-corrosion graphene/conductive polypyrrole composite thin film |
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