CN107603485B - A kind of preparation method of the dedicated polymolecularity graphene masterbatch of anticorrosive paint - Google Patents
A kind of preparation method of the dedicated polymolecularity graphene masterbatch of anticorrosive paint Download PDFInfo
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- CN107603485B CN107603485B CN201711016744.2A CN201711016744A CN107603485B CN 107603485 B CN107603485 B CN 107603485B CN 201711016744 A CN201711016744 A CN 201711016744A CN 107603485 B CN107603485 B CN 107603485B
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Abstract
For current graphene using haveing the defects that be difficult to disperse and the easy defect for being overlapped aggregation again of the layer of graphene in anticorrosive paint.The present invention proposes a kind of preparation method of dedicated polymolecularity graphene masterbatch of anticorrosive paint; its technical point is first to promote its percent opening at cellular by hydrofluoric acid deep etching glass microballoon; plasma surface treatment is carried out again; inert gas is passed through to be protected; graphene is soldered in microballon hole using discharge plasma simultaneously, is granulated with vector resin through Screw Extrusion after cooling and polymolecularity masterbatch is made.Solve the problems, such as that graphene is easily overlapped reunion so that the graphene uniform with dynamic load disperses using the glass microballoon good fluidity that the masterbatch bring remarkable result is spherical surface.
Description
Technical field
The present invention relates to grapheme material fields, and in particular to a kind of dedicated polymolecularity graphene masterbatch of anticorrosive paint
Preparation method.
Background technique
Graphene be it is a kind of as thickness in monolayer carbon atom it is tightly packed made of bi-dimensional cellular shape crystalline material.Due to graphite
Alkene has unique physicochemical properties, such as high-specific surface area, good electric conductivity and mechanical performance, excellent optics and heating power
Performance etc. is learned, the focus of every field research is had become.Its energy storage, liquid crystal device, electronic device, biomaterial,
The fields such as sensing material and catalyst carrier have shown excellent performance, have broad application prospects.But due to graphite
The special construction of alkene crystal causes its chemical stability high, easily reunites there are Van der Waals force between lamella and lamella,
It is difficult to be dissolved in water or other organic solvents, which prevent the further research and developments of graphene.Therefore graphene is carried out
Functionalization is particularly important to improve the dispersibility of graphene in the base.
Chinese patent application " a kind of graphene conductive masterbatch and preparation method thereof ", application No. is CN201610918490.2
A kind of graphene conductive masterbatch and preparation method thereof is provided.The Strong shear screw extruder that the present invention has shearing tooth using one,
Graphite raw material is uniformly mixed with hot melt material, is acted on using the Strong shear of shearing tooth, by graphite removing at graphene, and will
Graphene is evenly spread out along screw rod direction of rotation, is obtained finely dispersed graphene fusant and is obtained finally by extruding pelletization
Obtain graphene conductive masterbatch.The invention provides the above method and overcomes in the prior art by using graphene dry powder as raw material
Preparing graphene conductive master batch leads to high production cost, big using risk, the dispersibility of graphene in the conducting masterbatch of preparation
Difference, the low technical problem of yield rate realize the dispersion that graphene is improved while production cost is greatly reduced in masterbatch
Property, it is easy to the technical effect of graphene efficiently utilized, further, raw material and product are easy to store, highly-safe.But the skill
The defect of art is also extremely obvious: on the one hand, when dispersing to graphene, which is mentioned using the method for hot melt material package
Therefore the dispersibility of high graphene often loses physically or chemically activity by the graphene that hot melt material wraps up, cannot play
The effect of itself.On the other hand, dispersed pretreatment is not carried out to graphene due to present invention extruding charging process, leads to stone
Agglomeration just has occurred in black alkene in charging or pressure process, and this agglomeration can not reverse.
Chinese patent application " a method of it is dispersed in a polymer matrix to improve graphene ", application No. is
CN201510916570.X provides a kind of method that raising graphene disperses in a polymer matrix, i.e., first by polymer, stone
Black alkene and lewis acid catalyst obtain polymer/graphene with 100 ︰, 3~10 ︰, 0.1~2 component proportion progress melting mixing
Composite masterbatch.Lewis acid is removed later, the masterbatch of preparation is obtained containing containing lower graphene with mixed with polymers
The nanocomposite of amount.Obtained polymer/graphene composite material with do not use lewis acid catalyst handle to obtain
Polymer/graphene composite material compare, graphene dispersion is more uniform in the former polymeric matrix, and aggregate obviously subtracts
Few, more uniform dispersion facilitates the thermal oxidation stability performance for further promoting composite material.The technology equally need to be to modified material
Material carries out hot melt processing, and graphene particles or powder report are fully wrapped around, loses materialization activity；Simultaneously as point of this method
The poor fluidity of graphene, causes the dispersion of graphene not fully uniform during dissipating.
In conclusion how to improve graphene dispersion, overcomes graphene overlapping or agglomeration is grapheme material fortune
Important key technology.Although having there is researcher's door to propose the method for improving graphene dispersion, but all exist
Various defects, more prominent disadvantage have at two.One, existing graphene dispersion technology mostly uses hot melt material packet
It wraps up in, prevent the mode dispersed graphite alkene to contact with each other between graphene, this method causes graphene to be wrapped up by hot melt material, from
And it loses physically or chemically active.Two, the poor fluidity of grapheme material, existing dispersion technology itself is to consider dispersing
Agglomeration in the process leads to occur irreversible agglomeration in dispersion process, so that there are lack for product
It falls into.
Summary of the invention
For above-mentioned existing graphene using easy again with the layer of graphene in the presence of being difficult to disperse in anticorrosive paint
To be overlapped in the defect and existing graphene dispersion technology of aggregation that there are graphene dispersions insufficient, materialization activity it is bad with
And the deficiencies of there are irreversible agglomerations in dispersion process, the present invention proposes a kind of dedicated polymolecularity stone of anticorrosive paint
The preparation method of black alkene masterbatch.
A kind of preparation method of the dedicated polymolecularity graphene masterbatch of anticorrosive paint, the technical solution of use includes following step
It is rapid:
Hf etching agent: being first configured to the solution of 0.15~0.25mol/L by step 1, and it is molten that this is added in glass microballoon
In liquid, 50~80 DEG C at a temperature of stir, etch 1~2 hour, until it forms pit shape or cellular to improve its aperture
Rate；
Step 2: the glass microballoon that completion is etched in step 1 is rinsed with clear water, until surface hydrofluoric acid is completely washed,
By glass microballoon aeration-drying；
Step 3: the glass microballoon after the completion of step 2 cleaning is put into plasma treatment instrument cavity, and stone is added
Black alkene powder empties the air in plasma treatment instrument cavity；It is passed through inert protective gas；
Step 4: will be brought rapidly up in plasma treatment instrument cavity, pressurize, be powered, and be kept for 6 ~ 25 minutes, graphene is burnt
Knot is fixed in glass microballoon hole；
Step 5: the glass microballoon of step 4 sintering is mixed evenly with a certain proportion of resin material, and utilizes spiral shell
Bar extrusion granulation obtains a kind of dedicated polymolecularity graphene masterbatch of anticorrosive paint.
Preferably, heretofore described glass microballoon granularity is 10 ~ 250 microns, 1 ~ 2 micron of wall thickness, density 0.42
~0.6g/cm3。
Preferably, the concentration of heretofore described hf etching agent is 0.18mol/L.
Preferably, heretofore described acid etch temperature is at 65 DEG C.
Further, glass microballoon described in step 3 and nanoscale graphite alkene powder are 1:0.5 ~ 1.2 by volume.
Further, step 4 can be replaced: glass microballoon is placed in plasma treatment instrument cavity, with 200 in cavity
DEG C/min speed be brought rapidly up to 1000 DEG C ~ 1500 DEG C while improving in inner body pressure to 0Pa ~ 40MPa, energization and adjusting
Discharge current is 200-800 A, 10 ~ 18V of power-on voltage, is kept for 6 ~ 25 minutes, graphene, which is sintered, is fixed on glass microballoon hole
In cave.
Further, it is temperature 1280 that graphene, which is sintered the more excellent temperature condition to this process in glass microballoon hole,
DEG C, pressure 24Mpa, discharge current 250A, voltage 15V.
Further, the volume ratio of glass microballoon and resin material described in step 5 is 1:3 ~ 8.
Preferably, inert protective gas described in step 3 refers to one of helium, argon gas, or both any ratio
Example mixture.
The present invention provides a kind of preparation method of dedicated polymolecularity graphene masterbatch of anticorrosive paint, with prior art phase
Than the feature and excellent effect protruded is:
(1) a kind of method for being prepared by glass microballoon carrying, dispersed graphite alkene material is provided；
(2) using the porous cave-shaped glass microballoon formed after etching, Graphene powder powder material point is being improved as far as possible
While cloth density, but can ensure that will not occur on a large scale be overlapped or reunite.
(3) using the glass microballoon of spherical shape as graphene carrier, its mobility can be greatly improved, makes its distribution more
Uniformly.
(4) method provided by the invention for preparing polymolecularity graphene masterbatch has raw material sources extensive, at low cost
The characteristics of honest and clean, production equipment is simple, strong operability, has significant market application value.
Detailed description of the invention
A kind of scanning electron microscopic picture of the dedicated polymolecularity graphene masterbatch of anticorrosive paint that Fig. 1 embodiment 4 obtains.
Specific embodiment
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 preparation method of the dedicated polymolecularity graphene masterbatch of anticorrosive paint, the technical solution of use includes following step
It is rapid:
Hf etching agent: being first configured to the solution of 0.15mol/L by step 1, and glass microballoon is added in this solution,
50 DEG C at a temperature of stir, etch 1 hour, until it forms pit shape or cellular to improve its percent opening；
Step 2: the glass microballoon that completion is etched in above-mentioned steps is rinsed with clear water, until surface hydrofluoric acid is washed completely
It washs, by glass microballoon aeration-drying.
Step 3: the glass microballoon after the completion of above-mentioned steps is put into plasma treatment instrument cavity, and nanoscale is added
Graphene powder empties the air in plasma treatment instrument cavity；It is passed through inert protective gas；
Step 4: glass microballoon being placed in plasma treatment instrument cavity, is brought rapidly up, pressurizes, is powered in cavity, is kept
25 minutes, graphene, which is sintered, to be fixed in glass microballoon hole.
Step 5: the glass microballoon that completion is prepared in above-mentioned steps and a certain proportion of resin material are mixed equal
It is even, and be granulated using screw extruding, obtain a kind of dedicated polymolecularity graphene masterbatch of anticorrosive paint.
Embodiment 2
A kind of preparation method of the dedicated polymolecularity graphene masterbatch of anticorrosive paint, the technical solution of use includes following step
It is rapid:
Hf etching agent: being first configured to the solution of 0.15mol/L by step 1, and glass microballoon is added in this solution,
60 DEG C at a temperature of stir, etch 2 hours, until it forms pit shape or cellular to improve its percent opening；
Step 2: the glass microballoon that completion is etched in above-mentioned steps is rinsed with clear water, until surface hydrofluoric acid is washed completely
It washs, by glass microballoon aeration-drying.
Step 3: the glass microballoon after the completion of above-mentioned steps is put into plasma treatment instrument cavity, and nanoscale is added
Graphene powder empties the air in plasma treatment instrument cavity；It is passed through inert protective gas；
Step 4: glass microballoon is placed in plasma treatment instrument cavity, rapid with 200 DEG C/min of speed in cavity
It is warming up to 1000 DEG C while improving in inner body pressure to 5MPa, energization and to adjust discharge current be 200 A, power-on voltage 10V,
It is kept for 6 minutes, graphene, which is sintered, to be fixed in glass microballoon hole.
Step 5: the glass microballoon that completion is prepared in above-mentioned steps and a certain proportion of resin material are mixed equal
It is even, and be granulated using screw extruding, obtain a kind of dedicated polymolecularity graphene masterbatch of anticorrosive paint.
Embodiment 3
A kind of preparation method of the dedicated polymolecularity graphene masterbatch of anticorrosive paint, the technical solution of use includes following step
It is rapid:
Hf etching agent: being first configured to the solution of 0.18mol/L by step 1, and glass microballoon is added in this solution,
65 DEG C at a temperature of stir, etch 1 hour, until it forms pit shape or cellular to improve its percent opening；
Step 2: the glass microballoon that completion is etched in above-mentioned steps is rinsed with clear water, until surface hydrofluoric acid is washed completely
It washs, by glass microballoon aeration-drying.
Step 3: the glass microballoon after the completion of above-mentioned steps is put into plasma treatment instrument cavity, and nanoscale is added
Graphene powder empties the air in plasma treatment instrument cavity；It is passed through inert protective gas；
Step 4: glass microballoon is placed in plasma treatment instrument cavity, rapid with 200 DEG C/min of speed in cavity
It is warming up to 1280 DEG C while improving in inner body pressure to 24MPa, energization and to adjust discharge current be 250 A, power-on voltage 15V,
It is kept for 25 minutes, graphene, which is sintered, to be fixed in glass microballoon hole.
Step 5: the glass microballoon that completion is prepared in above-mentioned steps and a certain proportion of resin material are mixed equal
It is even, and crushed and be granulated using screw extrusion device, obtain a kind of dedicated polymolecularity graphene masterbatch of anticorrosive paint.
Embodiment 4
A kind of preparation method of the dedicated polymolecularity graphene masterbatch of anticorrosive paint, the technical solution of use includes following step
It is rapid:
Weighing bead degree is 10 ~ 250 microns, 1 ~ 2 micron of wall thickness, density 0.6g/cm38 grams of hollow glass micropearl it is standby
With；Configuration concentration is that the hydrofluoric acid aqueous solution 50mL of 0.18mol/L is spare；By the hollow glass micropearl and hydrofluoric acid of above-mentioned preparation
Aqueous solution mixing is placed in reaction vessel；Reaction vessel is placed in water-bath, and is kept for 65 DEG C of constant temperature, is mixed slowly 90 minutes
After filter out hydrofluoric acid solution；By the clear water repeated flushing of the glass microballoon after hf etching, until cleaning solution pH value is 7；It will
The glass microballoon cleaned up, which is placed in draught cupboard, to be completely dried, and remaining water is removed；Glass after the completion of above-mentioned steps is micro-
Pearl is put into plasma treatment instrument cavity, and nanoscale graphite alkene powder 12cm is added3, empty in plasma treatment instrument cavity
Air is passed through argon gas as inert protective gas, is forced into 24MPa；Temperature control system is adjusted, makes the temperature in cavity with every
The rate of 200 DEG C of minute rises to 1280 DEG C, after temperature reaches temperature, connects ion processing instrument electric current, discharge current 250A, electricity
15V is pressed, is kept for continuous discharge 25 minutes.Glass microballoon firmly carries graphene.
Such as Fig. 1, the ratio of the glass microballoon and resin material of completion according to volume ratio for 1:4.5 will be prepared in above-mentioned steps
It is mixed evenly, and is granulated using screw extruding, a kind of dedicated polymolecularity graphene masterbatch of anticorrosive paint is obtained, by sweeping
Electron microscope analysis is retouched, is uniformly dispersed.
Claims (9)
1. a kind of preparation method of the dedicated polymolecularity graphene masterbatch of anticorrosive paint, which comprises the following steps:
Hf etching agent: being first configured to the solution of 0.15~0.25mol/L by step 1, this solution is added in glass microballoon
In, 50~80 DEG C at a temperature of stir, etch 1~2 hour, until it forms pit shape or cellular to improve its percent opening；
Step 2: the glass microballoon that completion is etched in step 1 is rinsed with clear water, until surface hydrofluoric acid is completely washed, by glass
Glass microballon aeration-drying；
Step 3: the glass microballoon after the completion of step 2 cleaning is put into plasma treatment instrument cavity, and graphene is added
Powder empties the air in plasma treatment instrument cavity；It is passed through inert protective gas；
Step 4: will be brought rapidly up in plasma treatment instrument cavity, pressurize, be powered, and be kept for 6 ~ 25 minutes, and graphene is sintered solid
It is scheduled in glass microballoon hole；
Step 5: the glass microballoon of step 4 sintering is mixed evenly with a certain proportion of resin material, and is squeezed using screw rod
Pressure is granulated, and obtains a kind of dedicated polymolecularity graphene masterbatch of anticorrosive paint.
2. the method according to claim 1 for preparing polymolecularity graphene masterbatch, which is characterized in that the glass is micro-
Bead degree is 10 ~ 250 microns, and 1 ~ 2 micron of wall thickness, density are 0.42~0.6g/cm3。
3. the method according to claim 1 for preparing polymolecularity graphene masterbatch, which is characterized in that described in step 1
Hf etching agent solution concentration be 0.18mol/L.
4. the method according to claim 1 for preparing polymolecularity graphene masterbatch, which is characterized in that described in step 1
Acid etch temperature at 65 DEG C.
5. the method according to claim 1 for preparing polymolecularity graphene masterbatch, which is characterized in that described in step 3
Glass microballoon and nanoscale graphite alkene powder be by volume 1:0.5 ~ 1.2.
6. the method according to claim 1 for preparing polymolecularity graphene masterbatch, which is characterized in that described in step 5
The volume ratio of glass microballoon and resin material is 1:3 ~ 8.
7. the method according to claim 1 for preparing polymolecularity graphene masterbatch, which is characterized in that described in step 3
Inert protective gas refer to one of helium, argon gas, or both arbitrary proportion mixture.
8. the method according to claim 1 for preparing polymolecularity graphene masterbatch, which is characterized in that step 4 replacement
Are as follows: glass microballoon is placed in plasma treatment instrument cavity, the speed in cavity with 200 DEG C/min be brought rapidly up to 1000 DEG C ~
1500 DEG C, improve in inner body pressure simultaneously to 0Pa ~ 40MPa, energization and to adjust discharge current be 200-800 A, power-on voltage 10
~ 18V is kept for 6 ~ 25 minutes, and graphene, which is sintered, to be fixed in glass microballoon hole.
9. the method according to claim 1 for preparing polymolecularity graphene masterbatch, which is characterized in that graphite in step 4
Alkene is sintered to 1280 DEG C of the temperature condition of this process in glass microballoon hole, pressure 24Mpa, discharge current 250A, voltage
15V。
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Citations (4)
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| JP2012240891A (en) * | 2011-05-20 | 2012-12-10 | Vision Development Co Ltd | Nanocarbon-nanocomposite, and method for producing the same |
| CN105400157A (en) * | 2015-12-10 | 2016-03-16 | 四川大学 | Method for improving dispersibility of graphene in polymer matrix |
| CN107022183A (en) * | 2017-05-18 | 2017-08-08 | 成都新柯力化工科技有限公司 | A kind of preparation method of automobile engineering plastics special graphite alkene masterbatch |
| CN107151364A (en) * | 2017-05-22 | 2017-09-12 | 成都新柯力化工科技有限公司 | A kind of microballoon graphene enhancing masterbatch and preparation method |
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2017
- 2017-10-26 CN CN201711016744.2A patent/CN107603485B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012240891A (en) * | 2011-05-20 | 2012-12-10 | Vision Development Co Ltd | Nanocarbon-nanocomposite, and method for producing the same |
| CN105400157A (en) * | 2015-12-10 | 2016-03-16 | 四川大学 | Method for improving dispersibility of graphene in polymer matrix |
| CN107022183A (en) * | 2017-05-18 | 2017-08-08 | 成都新柯力化工科技有限公司 | A kind of preparation method of automobile engineering plastics special graphite alkene masterbatch |
| CN107151364A (en) * | 2017-05-22 | 2017-09-12 | 成都新柯力化工科技有限公司 | A kind of microballoon graphene enhancing masterbatch and preparation method |
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Address after: Room JT966, 4th Floor, Building 2, No. 599, Wanzhen Road, Zhenxin Xincun Street, Jiading District, Shanghai, 200000 Patentee after: Shanghai Shengyicheng Textile Group Co.,Ltd. Address before: 201824 652, 1525 Caoan Road, Zhenxin Street, Jiading District, Shanghai Patentee before: Shanghai Shengyi Cheng Textile Co.,Ltd. |
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