CN108972937A - Processing method is blended in graphene filling system based on multiburst effect - Google Patents
Processing method is blended in graphene filling system based on multiburst effect Download PDFInfo
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- CN108972937A CN108972937A CN201810761535.9A CN201810761535A CN108972937A CN 108972937 A CN108972937 A CN 108972937A CN 201810761535 A CN201810761535 A CN 201810761535A CN 108972937 A CN108972937 A CN 108972937A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
- B29B7/40—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with single shaft
- B29B7/42—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with single shaft with screw or helix
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
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Abstract
It is related to the graphene filling system based on multiburst effect and processing method is blended, graphene filling system is added in volume fluctuation plasticizing feeding device, make graphene filling system volume axially and radially in alternately cyclically-varying, carry out periodic compression release, generate multiburst effect, to removing and dispersed graphite alkene, increase polymeric matrix free volume, and makes in graphene intercalation polymeric object matrix free volume.Particularly, critical medium can be introduced into graphene filling system, enhance multiburst effect.The present invention increases polymeric matrix free volume using the physical force that graphene filling system volume compression release generates, and removes dispersed graphite alkene, has many advantages, such as environmentally protective；The present invention realizes graphene removing dispersion and mixes the continuous process that work combines together, has many advantages, such as simply, efficient, may be used on the large-scale industrial production of graphene composite material product.
Description
Technical field
The present invention relates to polymer material molding processing technique fields, more particularly to the graphene based on multiburst effect
Processing method is blended in filling system.
Background technique
In recent years, using graphene be blended with high molecular material the nanocomposite being prepared show it is excellent
The performances such as conductive, thermally conductive, mechanics, have broad application prospects.However, since the thickness of graphene nano lamella is only one
Carbon atom diameter leads to polymer nanocomposite composite wood so that being easy to pile up by Van der Waals force between lamella and lamella
Graphene sheet layer in material is easy to happen agglomeration, to weaken, limit the function and effect of graphene.Particularly with non-pole
For property polymeric matrix, such as polypropylene, polyethylene etc., carbon conjugated double bond and this kind of material phase as contained by graphene
Interaction is weaker, it is easier to graphene sheet layer be caused to be reunited in its matrix.The study found that utilizing graphene sheet layer structure
On the oxygen-containing groups such as carboxyl, hydroxyl and epoxy group, carry out covalent modification and non-covalent modification to it, or to polymeric matrix into
Row modification can effectively improve the interaction between graphene and polymeric matrix, to promote its dispersion in the base.
However, these method of modifying, can all be related to organic chemical reactions, with time-consuming, low efficiency, needs organic solvent, difference
The disadvantages of graphene original structure is destroyed in degree.In order to give full play to the function and effect of graphene, preparation has high dispersive
Polymer graphite alkene nanocomposite seem most important.
Now, main composite Nano filler and there are three ways to polymer: in-situ polymerization, solution mixing and melting are altogether
It is mixed.In-situ polymerization, solution mixing, both methods undoubtedly again increase the manufacturing cost and work of graphene nanocomposite material
Skill complexity.Melt blending is most to be close to industrial application, however graphene filling system viscosity is high in these methods, difficult
With processing, and graphene is difficult to be uniformly dispersed in a polymer matrix.Traditional melt blending processing method is made using Strong shear
With dispersed graphite alkene, it is easily destroyed the original laminated structure of graphene.
Publication No. is the patent of CN107298440A, and expanded graphite and dispersant are obtained mixture, screw rod is added
In machine, it is passed through supercritical carbon dioxide and penetrates into the interlayer of graphite step by step.The shearing of screw rod makes graphite be in the state of activation, then
In screw rod head quick pressure releasing, supercritical fluid preparation and dispersed graphite alkene are utilized.This method is tentatively divided using screw rod shearing
Graphite is dissipated, its lamellar structure is easily destroyed.And it is higher in the shearing of screw rod carbonization section temperature setting, it is unfavorable for energy saving.
Publication No. be CN107226467A patent, by graphite dispersion in polymer, and with mixer to polymer into
Row melting mixing stretches, while applying supercritical fluid, and the interlayer of expanded graphite is permeated by supercritical fluid, in mixer
Expanded graphite because quickly removing expanded graphite under supercritical fluid osmosis by polymeric shear, stretching, dispersion in situ
For graphene, and it is scattered in polymer.After mixing, slow pressure release to normal pressure is prepared and is dispersed using supercritical fluid
Graphene.Entire melting mixing process carries out in mixer, there is very strong shear action, the graphene after being easily destroyed separation
Lamellar structure, and make the preparation process batch process of entire polymer composites, do not have long-time continuity, and
And the yield of a production cycle is determined by mixer cavity capacity.
For conventional melt be blended processing method can not fine dispersion graphene, be easily destroyed graphene sheet layer structure, it is difficult
With the deficiency of processing graphite alkene filling system, it is plasticized transport property using volume fluctuation, developing one kind has efficient, environmental protection,
Processing method is blended in the graphene filling system that plasticizing transports the advantages that effect is good, graphene dispersion degree is high, to macromolecule material
Material machine-shaping is of great significance.
Summary of the invention
For the technical problems in the prior art, the purpose of the present invention is: based on volume compression release generate it is quick-fried
Fried effect removes dispersed graphite alkene, provides a kind of graphene filling system efficiently, environmentally friendly, simply based on multiburst effect
Processing method is blended.
In order to achieve the above object, the present invention adopts the following technical scheme:
Processing method is blended in graphene filling system based on multiburst effect, and it includes graphene that graphene, which fills system,
Filling system includes graphene, polymeric matrix and processing aid；It is defeated that graphene filling system is added to volume fluctuation plasticizing
In shipping unit, graphene filling system volume is made axially and radially in alternately cyclically-varying, to carry out periodic compression release,
Multiburst effect is generated, so that removing and dispersed graphite alkene, increase polymeric matrix free volume, and keeps graphene intercalation poly-
It closes in object matrix free volume.
Preferably, polymeric matrix includes thermoplastic polymer, and polymeric matrix is a kind of polymer, or for two kinds or
The blend of two or more polymer.
Preferably, volume fluctuation is plasticized feeding device and is divided into feed zone according to function on material conveying direction, melts
Melt fluxing zone, pressurization mixing section, decompression section and metering section.
Preferably, in fusion plastification section, graphene fills system volume axially and radially in alternately cyclically-varying, body
Long-pending compression release generates multiburst effect, to remove dispersed graphite alkene, increases polymeric matrix free volume.
Preferably, in pressurization mixing section, small size compression unit is arranged alternately with large volume releasing unit, graphene filling
System volume is axially and radially being in alternately cyclically-varying, and the significantly compression of volume, which discharges, enhances multiburst effect, into
One step removes dispersed graphite alkene, increases polymeric matrix free volume.
Preferably, in pressurization mixing section, critical medium is added into graphene filling system, enhances multiburst effect,
Inhibit graphene to reunite, promotes the removing and dispersion of graphene.
Preferably, critical medium includes subcritical water, supercritical carbon dioxide, supercritical nitrogen.
Preferably, pressure is reduced near polymeric matrix processing temperature, makes critical medium that liquid, gaseous state transformation occur.
Preferably, in pressurization mixing section, the compression release that graphene fills system volume promotes critical medium to penetrate into graphite
Alkene piece interlayer, and wrap up graphene and enter in polymeric matrix free volume.
Preferably, in pressurization mixing section, compression unit is arranged alternately with releasing unit, is controlled pressure change, is made critical Jie
The conversion of matter generating period liquid-gas state, enhances multiburst effect.
The principle of the present invention is: being plasticized feeding device using volume fluctuation, compresses graphene filling system volume
Release generates pressure difference and causes multiburst effect.So-called explosion effect, that is, the graphene obturator compressed tie up to volume and release
It converts the energy of system itself when putting and mechanical work is done to internal graphene aggregate, break a nanometer aggregate, while also right
Polymeric matrix acting, increases polymeric matrix free volume.During subsequent volume compression, the graphene sheet layer of dispersion
Have little time to reunite, be drawn by the stretching action in compression process, in intercalation polymeric object matrix free volume.It is being pressurized mixing section,
Small size compression unit is arranged alternately with large volume releasing unit, is increased graphene filling system volume compression and is discharged amplitude, increases
Intense explosion effect.
Particularly, in pressurization mixing section, critical medium, graphene system volume can be added into graphene filling system
The stretching action that significantly compression release generates promotes critical medium to enter graphene film interlayer, and wraps up graphene, and intercalation enters
In polymeric matrix；In addition the significantly compression release of graphene filling system periodical volume, can control pressure cycle
Raising and reduction, so that critical medium be made to generate the conversion of periodic liquid-gas state, the gas of graphene film interlayer critical medium
Change effect can offset the Van der Waals force between graphene layer, enhance explosion effect, promote the removing and dispersion of graphene.It is being depressured
Section, graphene filling system volume are totally in release process, and pressure, which constantly reduces, forms medium experience nuclei of bubbles, and bubble is raw
It grows, the process of bubbles burst, the gasification of critical medium counteracts the Van der Waals force between graphene layer between graphene layer, generates
Release effect again reduces graphene number of plies, at the same the gasification of critical medium to the graphene of surrounding while removing
Apply stretching action, to reinforce dispersion effect on the basis of original volume elongation flow field.
Generally speaking, the present invention has the advantage that
1. the compression release of volume brings the accumulation and release of graphene filling system pressure, multiburst effect is generated,
Increase polymeric matrix free volume, breaks graphene reunion, graphene is promoted to be inserted into polymeric matrix free volume, promote stone
The mixed effect of black alkene filling system.
2. graphene needs not move through chemical modification, the integrality of graphene-structured is kept, improves production efficiency.
3. being pressurized mixing section pressure controllable, critical medium is made to generate periodical liquid-gas state conversion, enhancing removing dispersion effect
Fruit.
4. critical medium gasifying stage, does not need quick pressure releasing, the safety that processing is blended is improved.
5. the viscosity of graphene filling system transports influence less to volume plasticizing, so the filling system that the present invention adapts to
Application viscosity range is wide.
6. processing method, which is blended, in the graphene filling system based on multiburst effect has adding based on stretching action
Work flow field, compares traditional diamond-making technique, has more dispersion effect.
7. processing method, which is blended, in the graphene filling system based on multiburst effect can be realized graphene removing dispersion
The continuous process that work combines is mixed together, may be used on the large-scale industrial production of graphene composite material product.
Detailed description of the invention
Fig. 1 is that volume fluctuation is plasticized feeding device structural schematic diagram.
Fig. 2 is that volume is plasticized sending unit equivalent model figure.
Fig. 3 is explosion effect schematic diagram.
Label and corresponding parts title in figure are as follows: 1 is feeder, and 2 critical medium input ports, 3 be vacuum orifice,
4 be eccentric rotor, and 5 be stator, and A is feed zone, and B is fusion plastification section, and C is pressurization mixing section, and D is decompression section, and E is metering
Section.
Specific embodiment
It is next with reference to the accompanying drawings and examples that the present invention will be further described in detail.
Embodiment 1
Graphene fills system, by percentage to the quality, including following components: 94.5wt% (mass fraction) high density is poly-
Ethylene (density=0.95g/cm3, melt flow rate (MFR): 24g/10min), 5wt% graphene microchip (thickness 120nm, average piece
6 μm of diameter), 0.5wt% (mass fraction) antioxidant 1010.
Processing method is blended in graphene filling system based on multiburst effect, comprising the following steps:
S1. graphene filling system is added in volume fluctuation plasticizing feeding device shown in FIG. 1 by feeder.In object
Expect conveying direction, the screw pitch of feed zone is gradually reduced, and head and the tail screw pitch ratio is 3.5, and graphene obturator ties up to feed zone and completes pressure
Real process.
S2. fusion plastification section screw pitch is constant, is less than feed zone end screw pitch.In fusion plastification section, by the heating of stator,
Heat is stretched with the volume of eccentric rotor, graphene fills system melting, and melt volume is axially and radially being submitted with cavity volume
For cyclically-varying, pressure difference caused by volume compression discharges can produce multiburst effect, open graphene aggregate, increase
Add polymeric matrix free volume.
S3. then under the positive conveyance effect of eccentric rotor, polymer melt is full of pressurization mixing section.It is mixed in pressurization
Section is closed, fine pitch compression unit is arranged alternately with big screw pitch releasing unit, is repeated 3-6 times, and graphene fills system volume in list
Individual toy plastic building blocks sending unit compression release, while also significantly being compressed between the adjacent compression unit of conveying direction and releasing unit
Release, increases the compression releasing degree of melt volume, enhances explosion effect, further opens graphene aggregate, increases
Polymeric matrix free volume.And the stretching action in compression process, promote Sheet Graphite alkene intercalation polymeric object matrix free
In volume.
S4. eccentric rotor positive conveyance graphene filling system enters decompression section.The screw pitch of decompression section is gradually increased, first
Tail screw pitch ratio is 3.5, gradually decreases pressure, alleviates melt internal stress, is reduced because of hypertonia bring equipment loss.
S5. last graphene filling system is extruded by metering section.Metering section screw pitch is constant with fusion plastification section screw pitch
Unanimously.
Embodiment 2
Graphene fills system, by percentage to the quality, including following components: 90wt% (mass fraction) polypropylene is (close
Degree=0.9g/cm3, melt flow rate (MFR): 24g/10min), 10wt% graphene microchip (thickness 100nm, average 8 μm of piece diameter),
Critical medium is supercritical CO2。
Processing method is blended in graphene filling system based on multiburst effect, comprising the following steps:
S1. graphene filling system is added in volume fluctuation plasticizing transport system shown in FIG. 1 by feeder.In object
Expect conveying direction, the screw pitch of feed zone is gradually reduced, and for the range of head and the tail screw pitch ratio between 3.0-6.0, graphene fills system
Compacting process is completed in feed zone.
S2. fusion plastification section screw pitch is constant, is less than or equal to feed zone end screw pitch.In fusion plastification section, by stator
Heating, stretch heat with the volume of eccentric rotor, graphene fills system melting, and melt volume is with cavity volume in axial direction and diameter
To in alternately cyclically-varying, pressure difference caused by volume compression discharges can produce multiburst effect, open graphene group
Aggressiveness increases polymeric matrix free volume.
S3. then under the positive conveyance effect of eccentric rotor, polymer melt is full of pressurization mixing section.It is mixed in pressurization
Section is closed, fine pitch compression unit is arranged alternately with big screw pitch releasing unit, is repeated 3-6 times, the compression for increasing melt volume is released
Degree is put, explosion effect is enhanced, further opens graphene aggregate, increases polymeric matrix free volume.
S4. simultaneously in pressurization mixing section, by the high-pressure metering pump of temperature controllable from critical medium input port, with
The egress rate of 0.05ml/min and the pressure of 7.38MPa~22MPa inject supercritical CO2Fluid, and pass through pressure sensor
Detect pressure value.Under volume stretching action, high temperature polymer melt and supercritical CO2Uniformly mixing, polymeric matrix occur
Swelling, supercritical CO2Into between graphene layer, and graphene is wrapped up, reduce its friction between polymeric matrix, drawn in volume
It stretches in effect underthrust one polymer matrix.Meanwhile the compression unit being arranged alternately presses melt volume significantly with releasing unit
When pressure is higher than 7.38MPa the above process occurs for contracting release, the variation of melt pressure generating period.And whenever melt pressure
When lower than 7.38MPa, supercritical CO2Fluid can all be become gaseous state from liquid, generated multiburst effect, counteracted graphene layer
Between Van der Waals force, inhibit graphene reunite, remove graphene sheet layer.
S5. eccentric rotor positive conveyance graphene filling system enters decompression section.The screw pitch of decompression section is gradually increased, first
The range of tail screw pitch ratio is between 1/6~1/3, and pressure gradually decreases, supercritical CO2Experience nuclei of bubbles is formed, air bubble growth, gas
Steep the process of rupture, supercritical CO between graphene layer2Gasification counteract the Van der Waals force between graphene layer, inhibit graphite
Alkene is reunited, and is realized removing and dispersing again for graphene, is reduced graphene number of plies, while supercritical CO2Gasification to week
The graphene enclosed applies stretching action while removing, to reinforce dispersion effect on the basis of original volume elongation flow field
Fruit.Last supercritical CO2Fluid releases from high temperature polymer melt and is converted to gaseous state, using vacuum pump from vacuum orifice
Extraction reduces entrapped supercritical CO2Influence to graphene composite material performance.
S6. last graphene filling system is extruded by metering section.Metering section screw pitch is constant with fusion plastification section screw pitch
Unanimously.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. processing method is blended in the graphene filling system based on multiburst effect, it includes that graphene is filled out that graphene, which fills system,
The system of filling includes graphene, polymeric matrix and processing aid, it is characterised in that: graphene filling system is added to volume arteries and veins
In dynamic plasticizing feeding device, carrying out graphene filling system volume axially and radially in alternately cyclically-varying, periodically
Compression release, generates multiburst effect, so that removing and dispersed graphite alkene, increase polymeric matrix free volume, and make stone
In black alkene intercalation polymeric object matrix free volume.
2. processing method, feature is blended in the graphene filling system described in accordance with the claim 1 based on multiburst effect
Be: polymeric matrix includes thermoplastic polymer, and polymeric matrix is a kind of polymer, or poly- for two or more
Close the blend of object.
3. processing method, feature is blended in the graphene filling system described in accordance with the claim 1 based on multiburst effect
Be: volume fluctuation plasticizing feeding device is divided into feed zone, fusion plastification section according to function on material conveying direction, increases
Press mixing section, decompression section and metering section.
4. processing method, feature is blended in the graphene filling system described in accordance with the claim 3 based on multiburst effect
Be: in fusion plastification section, it is axially and radially being in replace cyclically-varying that graphene, which fills system volume, and the compression of volume is released
It puts and generates multiburst effect, to remove dispersed graphite alkene, increase polymeric matrix free volume.
5. processing method, feature is blended in the graphene filling system described in accordance with the claim 3 based on multiburst effect
Be: in pressurization mixing section, small size compression unit is arranged alternately with large volume releasing unit, and graphene filling system volume exists
Axially and radially in alternately cyclically-varying, the significantly compression release enhancing multiburst effect of volume, further removing point
Graphene is dissipated, polymeric matrix free volume is increased.
6. processing method, feature is blended in the graphene filling system based on multiburst effect according to claim 5
It is: in pressurization mixing section, critical medium is added into graphene filling system, enhances multiburst effect, inhibits graphene
Reunite, promotes the removing and dispersion of graphene.
7. processing method, feature is blended in the graphene filling system based on multiburst effect according to claim 6
Be: critical medium includes subcritical water, supercritical carbon dioxide, supercritical nitrogen.
8. processing method, feature is blended in the graphene filling system based on multiburst effect according to claim 7
It is: reduces pressure near polymeric matrix processing temperature, makes critical medium that liquid, gaseous state transformation occur.
9. processing method, feature is blended in the graphene filling system based on multiburst effect according to claim 6
Be: in pressurization mixing section, the compression release that graphene fills system volume promotes critical medium to penetrate into graphene film interlayer, and
Package graphene enters in polymeric matrix free volume.
10. processing method, feature is blended in the graphene filling system based on multiburst effect according to claim 8
Be: in pressurization mixing section, compression unit is arranged alternately with releasing unit, is controlled pressure change, is made critical medium generating period
Property liquid-gas state conversion, enhance multiburst effect.
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Cited By (5)
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| CN110065940A (en) * | 2019-06-19 | 2019-07-30 | 侯梦斌 | A kind of equipment and technology for intervening subcritical solvent pressure changeable removing carbon material |
| CN112624098A (en) * | 2021-01-20 | 2021-04-09 | 湖北卓熙氟化股份有限公司 | Preparation method and application of fluorinated graphene with high fluorocarbon ratio |
| CN112895269A (en) * | 2021-02-04 | 2021-06-04 | 华南理工大学 | Polymer circulating dynamic force field pressure forming method |
| CN113276376A (en) * | 2021-04-27 | 2021-08-20 | 华南理工大学 | Series explosion synergistic blending polymer-based graphene foam extrusion molding method |
| CN114133746A (en) * | 2021-12-30 | 2022-03-04 | 华中科技大学 | Flame-retardant silicone rubber boron nitride nanocomposite and preparation method thereof |
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