CN107603131A - A kind of low energy consumption, the method for prepare with scale graphene filling master batch - Google Patents
A kind of low energy consumption, the method for prepare with scale graphene filling master batch Download PDFInfo
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Abstract
The present invention proposes a kind of low energy consumption, the method for prepare with scale graphene filling master batch; the porous resin microballoon good with matrix resin compatibility is adsorbed to graphene; blowing agent H is dissolved in organic solvent again; organic solvent is removed through atomization; make blowing agent H be deposited on porous resin microsphere surface to be packaged, coat, crushed after centrifuge separates and obtain above-mentioned functional master batch.The present invention provides such scheme and overcome using screw extruder, and not only technique is cumbersome, and equipment cost is high, the technological deficiency of high energy consumption, prepares masterbatch without extrusion equipment, equipment cost and energy consumption is reduced, beneficial to large-scale production；Further, it is good using porous resin microballoon and matrix resin compatibility, improve graphene dispersion effect, during using masterbatch, it is sustained with the decomposition graphene uniform of foaming agent to inside resin, graphene dispersion effect is improved, porous resin microballoon is avoided and is again to reunite during resin matrix fusion.
Description
Technical field
The present invention relates to material processing field, and in particular to a kind of low energy consumption, prepare with scale graphene filling master batch
Method.
Background technology
Grapheme material is successfully prepared within 2004, has triggered the upsurge of new ripple carbon materials research since then.Graphene
The plane carbon nanomaterial being made up of one layer of carbon atom, is to be currently known most thin two-dimensional material, and its thickness is only
0.335nm, it is made up of the lattice of six sides.By σ key connections between carbon atom in graphene, it is extremely excellent to impart graphene
Mechanical property and structural rigidity.Moreover, in graphene, each carbon atom has the p electronics of a non-bonding, these p electricity
Son can move freely in crystal, and movement velocity is up to the 1/300 of the light velocity, impart the good electric conductivity of graphene.
Optics aspect, graphene are almost fully transparent, only absorb 2.3% light.Graphene has peculiar mechanics, optics and electricity
Property is learned, therefore extensive commercial Application is considered to have in terms of as the strengthening of polymeric matrix, conductive and heat filling
Prospect.
The conventional method for currently preparing all kinds of masterbatch is carried out for each group is placed in high-speed kneading machine or mixer first
Mediate, mixing, then discharge, extruded in double screw extruder, pelletizing, obtain masterbatch.
Chinese patent publication No. 106564175A discloses a kind of graphene conductive masterbatch and preparation method thereof, using a band
There is the Strong shear screw extruder of shearing tooth, graphite raw material is uniformly mixed with hot melt material, made using the Strong shear of shearing tooth
With graphite is peeled off and opened along screw rod direction of rotation is dispersed into graphene, and by graphene, obtains finely dispersed graphite
Alkene fused mass, finally by extruding pelletization, obtain graphene conductive masterbatch.
The A of Chinese patent publication No. 105694102 is being peeled off graphite powder by the use of screw extruder as flow reactor
While using three-dimensional porous inorganic matter carry out scattered fixation, and heat conduction network is further formed by continuous polymerization, prepared
A kind of composite graphite alkene microplate radiating masterbatch.Extensively using the radiating of top load rubber tyre, rubber blanket radiating, electronic component
Junction radiating, LED radiatings etc., have wide market prospects.
Chinese patent publication No. 107200947A discloses a kind of graphene microchip conducting masterbatch and preparation method thereof, by stone
Ink powder mixes with metallic tin, under the high temperature conditions tin fusing, is peeled off graphite for after graphene microchip by stirring broken shearing
With glass microballoon chilling coating, the scattered simultaneously coating that is present in metallic tin of graphene stable and uniform is set in glass microballoon, to enter one
Step, formed by grinding by the stable graphene particulate of tin, be scattered in high polymer material and prepared by screw extruder.Should
Graphene microchip conducting masterbatch has good dispersiveness, is suitable for various conductive plastics, electric plastics, photovoltaic plastics and leads
Electricity.
Because the above method need to use screw extruder, not only technique is cumbersome, and equipment cost is high, high energy consumption.Such as
Masterbatch pellet is prepared according to the method without using screw extruder, then production cost greatly reduces.Simultaneously as graphene meeting
Produce itself to reunite, destroy its scattered uniformity, compactness, cause composite machinery performance etc. to decline.Therefore, it is necessary to
Develop a kind of preferable low energy consumption of graphene dispersion, the preparation method of prepare with scale graphene filling master batch.
The content of the invention
For preparing graphene masterbatch using screw extruder in the prior art, not only technique is cumbersome, and dispersion effect
Poor, the technological deficiency of high energy consumption, the present invention proposes a kind of preferable low energy consumption of graphene dispersion, prepare with scale graphene
The preparation method of filling master batch, the porous resin microballoon of graphene is loaded with by using blowing agent H encapsulation, then crushes and mother is made
Material, the present invention prepare masterbatch without extrusion equipment, equipment cost and energy consumption are reduced, beneficial to large-scale production.
To solve the above problems, the present invention uses following technical scheme：
A kind of low energy consumption, the method for prepare with scale graphene filling master batch, comprise the following steps：
（1）Take 3-15 parts by weight of graphite alkene powders, 30-65 parts by weight porous resin microballoons, 20-25 parts by weight of blowing agent H, 40-
100 weight parts organic solvents, 1-2 parts by weight of graphite alkene dispersants are as raw material；
（2）The blowing agent H is divided into two parts, then by the graphene powder, the graphene dispersion agent, first part of foaming agent
H and the porous resin microballoon are compound, rotating speed 160-430rpm, stir 20-50 minutes, make porous resin microballoon uniform load
Graphene, produce composite porous resin microballoon；
（3）The composite porous resin microballoon is added in the organic solvent, second part of blowing agent H is added and stirs, then
The organic solvent is removed through atomization process, blowing agent H is deposited on porous resin microsphere surface and porous resin microballoon is sealed
Dress, cladding, after centrifuge separates, crushing obtains graphene filling master batch.
Preferably, the graphene powder be single-layer graphene, bilayer graphene, multi-layer graphene, graphene oxide and
Combination more than one or both of nitrogen-doped graphene.
Preferably, the porous resin microballoon is the group of one or both of phenolic resin microspheres, polystyrene microsphere
Close, the particle diameter of porous microsphere is 10-200 μm, aperture 50-800nm.
Preferably, the organic solvent be methanol, ethanol, isopropanol, acetone, in ether any one or it is two or more
Combination.
Preferably, the graphene dispersion agent is polyvinyl alcohol, pyrrolidones, cellulose, lauryl sodium sulfate, 12
In sodium alkyl benzene sulfonate, cetyl trimethylammonium bromide, Tween-80 and Qula logical -100 any one or it is two or more
Combination.
Preferably, first part of blowing agent H and second part of blowing agent H weight ratio are 1:1-2.
Preferably, the atomization process uses sprayer unit, air velocity control in 10-60m/s, the centrifuge from
Heart speed is 2000-8000rpm.
Preferably, it is specially to be crushed using ball mill ball milling that the crushing, which obtains graphene filling master batch, control ball
The rotating speed of grinding machine is 360-800rpm, and crushing obtains graphene filling master batch.
Double screw extruder is used in existing scheme, not only technique is cumbersome, and equipment cost is high, high energy consumption.Meanwhile
Reunite because graphene can produce itself, destroy its scattered uniformity, compactness, cause under composite machinery performance etc.
Drop.In consideration of it, a kind of low energy consumption, the method for prepare with scale graphene filling master batch are proposed, will be good with matrix resin compatibility
Good porous resin microballoon is adsorbed to graphene, then blowing agent H is dissolved in organic solvent, is removed through atomization organic molten
Agent, blowing agent H is deposited on porous resin microsphere surface and be packaged, coat, crushed after centrifuge separates and obtain above-mentioned work(
Can masterbatch.During using masterbatch, it is sustained with the decomposition graphene uniform of foaming agent to inside resin；This method prepares masterbatch need not
Extrusion equipment, equipment cost and energy consumption are reduced, beneficial to large-scale production；Further, porous resin microballoon and matrix tree are utilized
Lipid phase capacitive is good, improves graphene dispersion effect, and foaming agent encapsulation avoids porous resin microballoon and is that resin matrix melts
Reunite again during conjunction.
A kind of stretch release of the present invention prepares the banbury of graphene and prepares the method for graphene, with prior art phase
Than, its protrude the characteristics of and excellent effect be：
1st, the present invention proposes a kind of preferable low energy consumption of graphene dispersion, the preparation side of prepare with scale graphene filling master batch
Method, the porous resin microballoon of graphene is loaded with by using blowing agent H encapsulation, then crushes obtained masterbatch, overcome using spiral shell
Bar extruder technique is cumbersome, the technological deficiency of high energy consumption, and the present invention prepares masterbatch without extrusion equipment, reduce equipment cost and
Energy consumption, beneficial to large-scale production.
2nd, the present invention proposes a kind of preferable low energy consumption of graphene dispersion, the system of prepare with scale graphene filling master batch
Preparation Method, it is good using porous resin microballoon and matrix resin compatibility, during using masterbatch, with the decomposition graphene of foaming agent
Uniform slow release avoids porous resin microballoon and is resin to graphene dispersion effect, foaming agent encapsulation inside resin, is improved
Matrix is reunited again when fusing.
3rd, blowing agent H is divided into two parts and mixed by several times with porous resin microballoon, can be more efficiently to porous tree
Lipid microspheres are packaged, coated.
4th, masterbatch stable performance, it is easy to preserve, it is easy to use, so as to promote graphene packing material in resin art
Using.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought 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
（1）3 parts by weight single-layer graphene powders are taken, 65 parts by weight particle diameters are 200 μm, and aperture is that 50nm expanded phenol-formaldehyde resins are micro-
Ball, 25 parts by weight of blowing agent H, 50 pbw acetones, 2 weight account polyethylene alcohol are as raw material；
（2）The blowing agent H is divided into two parts, first part of blowing agent H is 1 with second part of blowing agent H weight ratio:1, then will
The graphene powder, the graphene dispersion agent, first part of blowing agent H and the porous resin microballoon are compound, and rotating speed is
430rpm, stir 20 minutes, make porous resin microballoon uniform load graphene, produce composite porous resin microballoon；
（3）The composite porous resin microballoon is added in the organic solvent, then adds second part of blowing agent H, is stirred
Speed is 120rpm, is stirred, then removes the organic solvent through atomization, and using sprayer unit, air velocity control exists
60m/s, separated through centrifuge, the centrifugal speed of the centrifuge is 2000rpm, and blowing agent H is deposited on porous resin microballoon table
It is packaged, coats in face of porous resin microballoon, crushed using ball mill ball milling, the rotating speed for controlling ball mill is
360rpm, crushing obtain graphene filling master batch.
Embodiment 2
（1）15 parts by weight bilayer graphenes, multi-layer graphene combination powder are taken, 50 parts by weight particle diameters are 200 μm, and aperture is
800nm polystyrene microspheres, 20 parts by weight of blowing agent H, 100 parts by weight Methanol and alcohol mixeding liquid, 1 parts by weight dodecyl sulphur
Sour sodium, neopelex, the mixture of cetyl trimethylammonium bromide are as raw material；
（2）The blowing agent H is divided into two parts, first part of blowing agent H is 1 with second part of blowing agent H weight ratio:2, then
The graphene powder, the graphene dispersion agent, first part of blowing agent H and the porous resin microballoon is compound, and rotating speed is
430rpm, stir 20 minutes, make porous resin microballoon uniform load graphene, produce composite porous resin microballoon；
（3）The composite porous resin microballoon is added in the organic solvent, then adds second part of blowing agent H, is stirred
Speed is 30rpm, is stirred, then removes the organic solvent through atomization, and using sprayer unit, air velocity is controlled in 10m/
S, separated through centrifuge, the centrifugal speed of the centrifuge is 8000rpm, and blowing agent H is deposited on porous resin microsphere surface pair
Porous resin microballoon is packaged, coated, and is crushed using ball mill ball milling, and the rotating speed for controlling ball mill is 360rpm, powder
It is broken to obtain graphene filling master batch.
Embodiment 3
（1）The admixed graphite alkene powder of 5 parts by weight graphene oxides and nitrogen-doped graphene is taken, 35 parts by weight particle diameters are 150 μm,
Aperture is 700nm expanded phenol-formaldehyde resin microballoons, 23 parts by weight of blowing agent H, 85 parts by weight of ethanol, isopropanol mixture, 2 weight
Part polyvinyl alcohol is as raw material；
（2）The blowing agent H is divided into two parts, first part of blowing agent H is 1 with second part of blowing agent H weight ratio:1, then will
The graphene powder, the graphene dispersion agent, first part of blowing agent H and the porous resin microballoon are compound, and rotating speed is
180rpm, stir 30 minutes, make porous resin microballoon uniform load graphene, produce composite porous resin microballoon；
（3）The composite porous resin microballoon is added in the organic solvent, then adds second part of blowing agent H, is stirred
Speed is 100rpm, is stirred, then removes the organic solvent through atomization, and using sprayer unit, air velocity control exists
30m/s, separated through centrifuge, the centrifugal speed of the centrifuge is 6000rpm, and blowing agent H is deposited on porous resin microballoon table
It is packaged, coats in face of porous resin microballoon, crushed using ball mill ball milling, the rotating speed for controlling ball mill is
400rpm, crushing obtain graphene filling master batch.
Embodiment 4
（1）Take 6 parts by weight bilayer graphenes, multi-layer graphene, graphene oxide admixed graphite alkene powder, 35 parts by weight are porous micro-
The particle diameter of ball is 180 μm, and aperture is 200nm polystyrene microspheres, 22 parts by weight of blowing agent H, 50 weight parts organic solvent methanol,
2 parts by weight Tween-80s are as raw material；
（2）The blowing agent H is divided into two parts, first part of blowing agent H is 1 with second part of blowing agent H weight ratio:1, then will
The graphene powder, the graphene dispersion agent, first part of blowing agent H and the porous resin microballoon are compound, and rotating speed is
300rpm, stir 25 minutes, make porous resin microballoon uniform load graphene, produce composite porous resin microballoon；
（3）The composite porous resin microballoon is added in the organic solvent, then adds second part of blowing agent H, is stirred
Speed is 110rpm, is stirred, then removes the organic solvent through atomization, and using sprayer unit, air velocity control exists
50m/s, separated through centrifuge, the centrifugal speed of the centrifuge is 3500rpm, and blowing agent H is deposited on porous resin microballoon table
It is packaged, coats in face of porous resin microballoon, crushed using ball mill ball milling, the rotating speed for controlling ball mill is
550rpm, crushing obtain graphene filling master batch.
Embodiment 5
（1）10 parts by weight of graphite alkene powders, 30 parts by weight porous resin microballoons are taken, the porous resin microballoon is porous microsphere
Particle diameter is 180 μm, and aperture is 230nm polystyrene microspheres, 24 parts by weight of blowing agent H, 45 weight parts organic solvent isopropanols
Mixture, 1.5 parts by weight lauryl sodium sulfate, Qula lead to -100 mixtures as raw material；
（2）The blowing agent H is divided into two parts, first part of blowing agent H is 1 with second part of blowing agent H weight ratio:1.5, then
The graphene powder, the graphene dispersion agent, first part of blowing agent H and the porous resin microballoon is compound, and rotating speed is
350rpm, stir 45 minutes, make porous resin microballoon uniform load graphene, produce composite porous resin microballoon；
（3）The composite porous resin microballoon is added in the organic solvent, then adds second part of blowing agent H, is stirred
Speed is 500rpm, is stirred, then removes the organic solvent through atomization, and using sprayer unit, air velocity control exists
45m/s, separated through centrifuge, the centrifugal speed of the centrifuge is 7200rpm, and blowing agent H is deposited on porous resin microballoon table
It is packaged, coats in face of porous resin microballoon, crushed using ball mill ball milling, the rotating speed for controlling ball mill is
650rpm, crushing obtain graphene filling master batch.
Comparative example 1
（1）10 parts by weight of graphite alkene powders, 30 parts by weight porous resin microballoons are taken, the porous resin microballoon is porous microsphere
Particle diameter be 180 μm, aperture be 230nm polystyrene microsphere, the mixture of 45 weight parts organic solvent isopropanols, 1.5 weight
Part lauryl sodium sulfate, Qula lead to -100 mixtures as raw material；
（2）Graphene powder, the graphene dispersion agent, porous resin microballoon is compound, it is 350rpm in rotating speed, stirs 45 points
Clock, make porous resin microballoon uniform load graphene, produce composite porous resin microballoon；
（3）The composite porous resin microballoon is added in the organic solvent, mixing speed 500rpm, stirred, then
The organic solvent is removed through atomization, using sprayer unit, air velocity is controlled in 45m/s, separated through centrifuge, the centrifugation
The centrifugal speed of machine is 7200rpm, is crushed using ball mill ball milling, and the rotating speed for controlling ball mill is 650rpm, is crushed
To graphene filling master batch.
Graphene filling master batch prepared by embodiment 1-5 and comparative example 1 is added in PP8303 with 5% mass ratio,
Disperseing through screw extruder, calendering obtains sheet material, by testing the performance of sheet material, weighs the dispersiveness of graphene filling master batch,
It is as shown in table 1 below.
Table 1：
| Specific embodiment | Sheet thickness（mm） | Sheet material stretching intensity（MPa） | Sheet material elongation at break（%） |
| Embodiment 1 | 1.5 | 48 | 350 |
| Embodiment 2 | 1.5 | 51 | 399 |
| Embodiment 3 | 1.8 | 44 | 400 |
| Embodiment 4 | 1,8 | 47 | 385 |
| Embodiment 5 | 1.5 | 49 | 392 |
| Comparative example 1 | 1.5 | 27 | 215 |
By the applied analysis to masterbatch, blowing agent H is divided into two parts using the present invention and mixed by several times with porous resin microballoon
Close, more efficiently porous resin microballoon can be packaged, coated, during using masterbatch, with the decomposition graphite of foaming agent
Alkene uniform slow release improves graphene dispersion effect to inside resin, and obtained plastic products intensity, flexibility significantly increases, and
Under equal conditions be not used foaming agent encapsulation, comparative example 1, due to lacking the scattered promotion of foaming agent so that graphene is not
Can effectively it disperse, so as to enhancement and unobvious.
Further, the present invention is loaded with the porous resin microballoon of graphene using foaming agent encapsulation, then crushes obtained masterbatch,
, the technological deficiency of high energy consumption cumbersome using screw extruder technique is overcome, the present invention prepares masterbatch without extrusion equipment, reduced
Equipment cost and energy consumption, beneficial to large-scale production.
Claims (8)
1. a kind of low energy consumption, the method for prepare with scale graphene filling master batch, it is characterised in that comprise the following steps：
（1）Take 3-15 parts by weight of graphite alkene powders, 30-65 parts by weight porous resin microballoons, 20-25 parts by weight of blowing agent H, 40-
100 weight parts organic solvents, 1-2 parts by weight of graphite alkene dispersants are as raw material；
（2）The blowing agent H is divided into two parts, then by the graphene powder, the graphene dispersion agent, first part of foaming agent
H and the porous resin microballoon are compound, rotating speed 160-430rpm, stir 20-50 minutes, make porous resin microballoon uniform load
Graphene, produce composite porous resin microballoon；
（3）The composite porous resin microballoon is added in the organic solvent, second part of blowing agent H is added and stirs, then
The organic solvent is removed through atomization process, blowing agent H is deposited on porous resin microsphere surface and porous resin microballoon is sealed
Dress, cladding, after centrifuge separates, crushing obtains graphene filling master batch.
2. a kind of low energy consumption according to claim 1, the method for prepare with scale graphene filling master batch, its feature exist
In the graphene powder is single-layer graphene, bilayer graphene, multi-layer graphene, graphene oxide and nitrogen-doped graphene
One or both of more than combination.
3. a kind of low energy consumption according to claim 1, the method for prepare with scale graphene filling master batch, its feature exist
In, the porous resin microballoon be one or both of expanded phenol-formaldehyde resin microballoon, polystyrene microsphere, the grain of porous microsphere
Footpath is 10-200 μm, aperture 50-800nm.
4. a kind of low energy consumption according to claim 1, the method for prepare with scale graphene filling master batch, its feature exist
In the organic solvent is any one or two or more combinations in methanol, ethanol, isopropanol, acetone, ether.
5. a kind of low energy consumption according to claim 1, the method for prepare with scale graphene filling master batch, its feature exist
In the graphene dispersion agent is polyvinyl alcohol, polyethylene, pyrrolidones, cellulose, lauryl sodium sulfate, dodecyl
Any one in benzene sulfonic acid sodium salt, cetyl trimethylammonium bromide, Tween-80 and Qula logical -100 or two or more groups
Close.
6. a kind of low energy consumption according to claim 1, the method for prepare with scale graphene filling master batch, its feature exist
In the blowing agent H is divided into two parts, and first part of blowing agent H is 1 with second part of blowing agent H weight ratio:1-2.
7. a kind of low energy consumption according to claim 1, the method for prepare with scale graphene filling master batch, its feature exist
In the atomization process uses sprayer unit, and air velocity control is in 10-60m/s, the centrifugal speed of the centrifuge
2000-8000rpm。
8. a kind of low energy consumption according to claim 1, the method for prepare with scale graphene filling master batch, its feature exist
In it is specially to be crushed using ball mill ball milling that the crushing, which obtains graphene filling master batch, and the rotating speed for controlling ball mill is
360-800rpm, crushing obtain graphene filling master batch.
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| CN109111822A (en) * | 2018-07-19 | 2019-01-01 | 佛山腾鲤新能源科技有限公司 | A kind of conductive corrosion-resistant coating |
| CN109796682A (en) * | 2018-12-18 | 2019-05-24 | 武汉金牛经济发展有限公司 | Heat-resisting PPR pipe of toughening and preparation method thereof |
| CN110105666A (en) * | 2019-05-21 | 2019-08-09 | 合肥市丽红塑胶材料有限公司 | A kind of nucleating agent master batch and preparation method thereof for toughening modifying PP resin |
| CN110144083A (en) * | 2019-05-14 | 2019-08-20 | 合肥市丽红塑胶材料有限公司 | A kind of impact-resistant modified PP material and preparation method thereof |
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| CN107603131B (en) | 2021-03-02 |
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