CN105622983B - A kind of preparation method of heat-conducting plastic special graphite alkene microplate - Google Patents
A kind of preparation method of heat-conducting plastic special graphite alkene microplate Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention proposes a kind of preparation method of heat-conducting plastic special graphite alkene microplate.This method uses natural flake graphite as primary raw material, intercalation modifying is carried out using urea, shearing stripping is carried out by twin-screw Vibration Extrusion machine, using urea, fast decoupled releases substantial amounts of gas in a heated condition, make substantial amounts of graphite linings peeling-off, by the temperature control of different phase, crystalline flake graphite is successively peeled off into graphene microchip, the fault of construction of graphene microchip is reduced, improves the heat conductivility of graphene；Then graphene microchip is coated by organic microcapsules, reduces the electric conductivity of graphene, improve graphene microchip and the high molecular compatibility of heat-conducting plastic, improve the utilization rate of graphene, reduce application cost of the graphene in heat-conducting plastic.The graphene microchip that the present invention is prepared using mechanical stripping method, fault of construction is small, and heat conductivility is high, and whole technical process is safe and reliable, and cost is cheap, environmental protection, has significant market application value.
Description
Technical field
The present invention relates to grapheme material field, and in particular to heat-conducting plastic special graphite alkene material, more particularly to one
The preparation method of kind heat-conducting plastic special graphite alkene microplate.
Background technology
Since graphene in 2004 is by Univ Manchester UK science An Deliehaimu and Constantine Nuo Woxiao
Love is found, always as the focus of people's research.Graphene is the cellular hexagonal formed by one layer of carbon atom with sp2 hydridization
The two-dimensional material of planar structure, its thickness are only 0.335nm, are current most thin materials known in the world.Graphene has height
Mechanical moduli（1.0 TPa）, thermal conductivity（5300 W/m•K）, specific surface area（2630 m2/g）And charge mobility（250,
000 cm2/V•s）, before the numerous areas such as the energy, electronic material, biomedicine and environmental protection have potential application
Scape.
Heat-conducting plastic has the characteristics that easy-formation, density are low, insulation is high pressure resistant, easy to use, in power industry, electronics work
Prospect and potentiality in an increasingly wide range of applications in the fields such as industry, especially steep the production such as lamp, battery pack heat-dissipating casing in LED
It is widely adopted in product.High polymer material in heat-conducting plastic is the non-conductor of heat mostly, to expand it in heat conduction field
Using, it is necessary to high polymer material is modified.Graphene is as a kind of Heat Conduction Material and polymer-based bluk recombination, having obtained property
Can preferable heat-conducting plastic.At present, graphene powder mainly is added in high polymer material, because carbon has good heat transfer
Performance so that the high polymer material by graphene modification also has good heat conductivility.
China Patent Publication No. CN104072868A discloses a species graphene and is modified heat-conducting plastic and preparation method thereof,
The component of class graphene modification heat-conducting plastic includes 80%~90% plastic basis material and 10%~20% class graphene, wherein class stone
Black alkene is to carry out chemical acidification processing by natural graphite scale, and native graphite interlayer is inserted with Strong oxdiative intercalator, 800~
Heat treatment is carried out under 1200 DEG C of hot environment and forms vermiform graphite, can be uniformly distributed in plastic basis material, and and plastics
Macromolecule forms network structure so that the present invention farthest retains every mechanical performance of plastics, and is led with good
Hot property.
China Patent Publication No. CN 104017331A disclose a kind of insulating and heat-conducting plastics and preparation method thereof, using just
The ethanol solution modified graphene of tetraethyl orthosilicate, and in plastics preparation process segmented add modified graphene and
Select the suitable amounts of modified graphene so that gained plastics have excellent insulating properties and thermal conductivity.Made in above-mentioned technology
Graphene powder is using graphite as raw material, is made by violent oxidation intercalation, expansion reduction.
At present, apply what the grapheme material in heat-conducting plastic was largely prepared using chemical oxidization method, using the party
Graphene prepared by method, due to passing through strong oxidizing process, a large amount of defects of graphene-structured are caused, cause graphene performance
Significantly decline.The graphene aoxidized in addition still also has the unreduced oxide group in part even across reduction in graphene,
These faults of construction and oxide group destroy graphene perfection of lattice, so as to significantly reduce the thermal conductivity of graphene
Rate.And the shortcomings of grapheme material is expensive at present, low yield, cumbersome preparation process, very big limit it and is moulded in heat conduction
Expect industrial application.
Graphene microchip generally refers to carbon-coating number and is more than 10 layers, ultra-thin graphene of the thickness in 5-100 nanometer ranges
Stratiform accumulation body.Graphene microchip maintains the original planar carbon hexatomic ring conjugation crystal structure of graphite, has the shape of super large
Shape ratio (diameter/thickness ratio), and there is nano thickness, therefore with excellent mechanical strength, conduction, heat conductivility etc..This makes
Obtain graphene microchip to be compounded to form as additive and high polymer material, it is possessed excellent heat conductivility, so as to obtaining property
The excellent Heat Conduction Material of energy.It is therefore an object of the present invention to a kind of high-quality graphene microplate is prepared using mechanical stripping method, with
Reach the application in heat-conducting plastic.
The content of the invention
The present invention in view of the shortcomings of the prior art, proposes a kind of preparation method of heat-conducting plastic special graphite alkene microplate, should
Method carries out intercalation modifying using natural flake graphite as primary raw material, using urea, is cut by twin-screw Vibration Extrusion machine
Stripping is cut, fast decoupled releases substantial amounts of gas in a heated condition using urea, makes substantial amounts of graphite linings peeling-off, passes through
The temperature control of different phase, crystalline flake graphite is successively peeled off into graphene microchip, reduce the fault of construction of graphene microchip, carry
The heat conductivility of high graphene；Then graphene microchip is coated by organic microcapsules, reduces the conduction of graphene
Property, graphene microchip and the high molecular compatibility of heat-conducting plastic are improved, improves the utilization rate of graphene, graphene is reduced and is leading
Application cost in thermoplastic materials.Graphene microchip prepared by the present invention can be directly appended in heat-conducting plastic, solved at present
Graphene is applied in heat-conducting plastic the problem of must being disperseed by solution.
To solve the above problems, the present invention uses following technical scheme：
A kind of preparation method of heat-conducting plastic special graphite alkene microplate, it is characterised in that：Based on natural flake graphite
Raw material is wanted, by urea intercalation modifying, is sheared using twin-screw Vibration Extrusion machine and peels off acquisition graphene, then by organic micro-
Capsule cladding handles to obtain powdered heat-conducting plastic special graphite alkene microplate, and specific preparation method is as follows：
（1）By the natural flake graphite of 70 ~ 80 parts by weight, the nano inorganic powder of 10 ~ 15 parts by weight, 5 ~ 10 parts by weight
Stearate mixes 30 ~ 50min by expanded extruder and obtains pre-composition；
（2）By step（1）Obtained pre-composition and concentration is 10 ~ 20 mol/L urea liquid by 1：5 ~ 10 matter
After amount is than mixing, 1 ~ 2h is reacted under 60 ~ 80 DEG C, stirring, is centrifuged, gained sediment is washed with absolute ethyl alcohol, dried
Afterwards, urea intercalated graphite compound is made；Then urea intercalated graphite compound is pumped into twin-screw Vibration Extrusion machine, twin-screw
Vibration Extrusion machine sets gradually ground section, intercalation section from feed end to discharge end, peels off section, 60 ~ 80 DEG C of control ground section temperature；
150 ~ 180 DEG C of intercalation section temperature；Peel off 180 ~ 360 DEG C of section temperature；In screw extruder extrusion, intercalation is compound in graphite
Urea in thing, which decomposes, discharges substantial amounts of gas, makes substantial amounts of graphite linings peeling-off, is revolved by the high speed of Vibration Extrusion machine
Turn shearing force field and the vibration drawing field of force, peeling-off crystalline flake graphite is quickly peeled off into graphene microchip；
（3）By step（2）The graphene microchip obtained through twin-screw Vibration Extrusion machine is added to 80 ~ 100 parts organic poly-
In the compound aqueous solution, 20 ~ 40min is dispersed with stirring at 60~80 DEG C, then cools down, stand, filter, in 60 ~ 80 DEG C of dryings, obtain
The graphene microchip of organic microcapsule coated；
（4）By step（3）The graphene microchip of obtained organic microcapsule coated is crushed to the powder that particle diameter is less than 10 μm,
It can be used as heat-conducting plastic special graphite alkene microplate.
Described natural flake graphite is that radial dimension is more than 50 microns, crystalline flake graphite of the carbon content more than 97%.
Described nano inorganic powder is in nano aluminium oxide, nano aluminum nitride, nm-class boron nitride, nano silicon
It is at least one.
Described stearate is water-based stearate, including water-based magnesium stearate, odium stearate, water-based zinc stearate,
At least one of water-based stearic amide.
The content of organic polymer is 10 ~ 30% in the described organic polymer aqueous solution；Described organic polymer is poly-
At least one of methacrylic acid, polyacrylamide, Ionic water-soluble epoxy resin, Arabic gum.
The rotating speed of the twin-screw Vibration Extrusion machine is 1000 ~ 1500rpm.
A kind of preparation method of heat-conducting plastic special graphite alkene microplate of the present invention, using natural flake graphite as primary raw material,
Intercalation modifying is carried out using urea, weakens the active force between crystalline flake graphite layer；Twin-screw Vibration Extrusion machine not same order is set
The control temperature of section, makes intercalation discharge substantial amounts of ammonia and a small amount of contracting two in the urea fast decoupled of crystalline flake graphite interlayer
Urea, cyanuric acid, the quick release of a large amount of gases make it that most of crystalline flake graphite layer is peeling-off；Again pass by and peel off rank
Section, makes biuret, cyanuric acid fusion and decomposition, and the crystalline flake graphite layer for making the intercalation stage unstripped is peeling-off again, so as to real
The successively stripping of existing crystalline flake graphite, the fault of construction of graphene is reduced, improve the heat conductivility of graphene.The graphene that will be obtained
Microplate is dispersed in watersoluble organic polymer, forms the graphene microchip of organic microcapsule coated, be advantageous to graphene microchip with
It plastics high molecular compatible, can be directly appended in heat-conducting plastic, without carrying out solution decentralized processing, improve graphene microchip and leading
Utilization rate in thermoplastic materials, improve the mechanical strength and heat conductivility of heat-conducting plastic.
The graphene microchip that preparation method of the present invention obtains passes through amino modified processing, is easy to high polymer material and is compounded to form
Heat-conducting plastic.After the graphene microchip that the inventive method obtains is added into polyamide nylon heat-conducting plastic system with 10%, heat conduction
The mechanical strength and heat conductivility of plastics greatly improve, and its physical function parameter is as shown in table 1.
Table 1：
| Physical property | Tensile strength (MPa) | Bending strength (MPa) | Thermal conductivity factor (w/mk) | Heat distortion temperature（℃） |
| Add the polyamide nylon of graphene microchip | 115 | 123.6 | 2.8 | 185℃ |
| Polyamide nylon | 72 | 84.7 | 0.27 | 72 |
A kind of preparation method of heat-conducting plastic special graphite alkene microplate of the present invention, compared with prior art, its spy protruded
Point and excellent effect are：
1st, peeled off by twin-screw Vibration Extrusion machine continuously grinding, intercalation, shearing, gas is produced using the heat resolve of urea
Body makes crystalline flake graphite be effectively peeled off into graphene microchip, and the Quick mechanical for realizing graphene microchip is peeled off, and reduces graphene
The fault of construction on surface, improve the heat conductivility of graphene.
2nd, graphene microchip is handled using organic microcapsule coated, reduces the electric conductivity of graphene, improve graphene
Microplate dispersiveness high molecular with heat-conducting plastic and compatibility, reduce the reunion of graphene, improve the utilization rate of graphene, drop
Application cost of the low graphene in heat-conducting plastic.
3rd, preparation method of the present invention is easily controllable, the closed production of serialization can be achieved, input is small, cost is low, without environment
Pollution, yield are high, have significant market application value.
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）By the natural flake graphite of 70 parts by weight, the nano aluminium oxide of 10 parts by weight, 5 parts by weight water-based stearic acid
Magnesium mixes 30 ~ 50min by expanded extruder and obtains pre-composition；
（2）By step（1）Obtained pre-composition and concentration is 20 mol/L urea liquid by 1：5 mass ratio mixing
Afterwards, in 60 ~ 80 DEG C, stirring 1 ~ 2h of lower reaction, centrifuge, gained sediment washed with absolute ethyl alcohol, dry after, be made and urinate
Plain intercalated graphite compound；Then urea intercalated graphite compound is pumped into twin-screw Vibration Extrusion machine, twin-screw Vibration Extrusion
Machine sets gradually ground section, intercalation section from feed end to discharge end, peels off section, 60 ~ 80 DEG C of control ground section temperature；Intercalation Duan Wen
150 ~ 180 DEG C of degree；Peel off 180 ~ 360 DEG C of section temperature；In screw extruder extrusion, urine of the intercalation in graphite composite
Element decomposes and discharges substantial amounts of gas, makes substantial amounts of graphite linings peeling-off, passes through the high-speed revolution shearing power of Vibration Extrusion machine
Field and the vibration drawing field of force, peeling-off crystalline flake graphite is set quickly to peel off into graphene microchip；
（3）By step（2）The graphene microchip obtained through twin-screw Vibration Extrusion machine is added to 100 parts of polymethyl
In aqueous acid, 20 ~ 40min is dispersed with stirring at 60~80 DEG C, then cools down, stand, filter, in 60 ~ 80 DEG C of dryings, had
The graphene microchip of machine microcapsule coated；
（4）By step（3）The graphene microchip of obtained organic microcapsule coated is crushed to the powder that particle diameter is less than 10 μm,
It can be used as heat-conducting plastic special graphite alkene microplate.
Embodiment 2
The preparation method of concrete heat-conducting plastic special graphite alkene microchip composite material：
（1）The odium stearate of the natural flake graphite of 80 parts by weight, the nano aluminum nitride of 10 parts by weight, 5 parts by weight is led to
Cross 30 ~ 50min of expanded extruder mixing and obtain pre-composition；
（2）By step（1）Obtained pre-composition and concentration is 10 mol/L urea liquid by 1：8 mass ratio mixing
Afterwards, in 60 ~ 80 DEG C, stirring 1 ~ 2h of lower reaction, centrifuge, gained sediment washed with absolute ethyl alcohol, dry after, be made and urinate
Plain intercalated graphite compound；Then urea intercalated graphite compound is pumped into twin-screw Vibration Extrusion machine, twin-screw Vibration Extrusion
Machine sets gradually ground section, intercalation section from feed end to discharge end, peels off section, 60 ~ 80 DEG C of control ground section temperature；Intercalation Duan Wen
150 ~ 180 DEG C of degree；Peel off 180 ~ 360 DEG C of section temperature；In screw extruder extrusion, urine of the intercalation in graphite composite
Element decomposes and discharges substantial amounts of gas, makes substantial amounts of graphite linings peeling-off, passes through the high-speed revolution shearing power of Vibration Extrusion machine
Field and the vibration drawing field of force, peeling-off crystalline flake graphite is set quickly to peel off into graphene microchip；
（3）By step（2）The graphene microchip obtained through twin-screw Vibration Extrusion machine is added to 80 parts of polyacrylamide
In the aqueous solution, 20 ~ 40min is dispersed with stirring at 60~80 DEG C, then cools down, stand, filter, in 60 ~ 80 DEG C of dryings, obtain organic
The graphene microchip of microcapsule coated；
（4）By step（3）The graphene microchip of obtained organic microcapsule coated is crushed to the powder that particle diameter is less than 10 μm,
It can be used as heat-conducting plastic special graphite alkene microplate.
Embodiment 3
The preparation method of timber heat-conducting plastic special graphite alkene microchip composite material：
（1）By the natural flake graphite of 80 parts by weight, the nm-class boron nitride of 15 parts by weight, 10 parts by weight water-based stearic acid
Zinc mixes 30 ~ 50min by expanded extruder and obtains pre-composition；
（2）By step（1）Obtained pre-composition and concentration is 15 mol/L urea liquid by 1：6 mass ratio mixes
After conjunction, in 60 ~ 80 DEG C, stirring 1 ~ 2h of lower reaction, centrifuge, gained sediment washed with absolute ethyl alcohol, dry after, it is obtained
Urea intercalated graphite compound；Then urea intercalated graphite compound is pumped into twin-screw Vibration Extrusion machine, twin-screw vibration is squeezed
Go out machine to set gradually ground section, intercalation section from feed end to discharge end, peel off section, 60 ~ 80 DEG C of control ground section temperature；Intercalation section
150 ~ 180 DEG C of temperature；Peel off 180 ~ 360 DEG C of section temperature；In screw extruder extrusion, intercalation is in graphite composite
Urea decomposes and discharges substantial amounts of gas, makes substantial amounts of graphite linings peeling-off, passes through the high-speed revolution shearing of Vibration Extrusion machine
The field of force and the vibration drawing field of force, peeling-off crystalline flake graphite is set quickly to peel off into graphene microchip；
（3）By step（2）The ionic that the graphene microchip obtained through twin-screw Vibration Extrusion machine is added to 100 parts is water-soluble
Property the epoxy resin aqueous solution in, 20 ~ 40min is dispersed with stirring at 60~80 DEG C, then cools down, stand, filter, it is dry at 60 ~ 80 DEG C
It is dry, obtain the graphene microchip of organic microcapsule coated；
（4）By step（3）The graphene microchip of obtained organic microcapsule coated is crushed to the powder that particle diameter is less than 10 μm,
It can be used as heat-conducting plastic special graphite alkene microplate.
Embodiment 4
The preparation method of concrete heat-conducting plastic special graphite alkene microchip composite material：
（1）By the natural flake graphite of 70 parts by weight, the nano silicon of 15 parts by weight, 5 parts by weight water-based tristearin
Sour acid amides mixes 30 ~ 50min by expanded extruder and obtains pre-composition；
（2）By step（1）Obtained pre-composition and concentration is 20 mol/L urea liquid by 1：5 mass ratio mixes
After conjunction, in 60 ~ 80 DEG C, stirring 1 ~ 2h of lower reaction, centrifuge, gained sediment washed with absolute ethyl alcohol, dry after, it is obtained
Urea intercalated graphite compound；Then urea intercalated graphite compound is pumped into twin-screw Vibration Extrusion machine, twin-screw vibration is squeezed
Go out machine to set gradually ground section, intercalation section from feed end to discharge end, peel off section, 60 ~ 80 DEG C of control ground section temperature；Intercalation section
150 ~ 180 DEG C of temperature；Peel off 180 ~ 360 DEG C of section temperature；In screw extruder extrusion, intercalation is in graphite composite
Urea decomposes and discharges substantial amounts of gas, makes substantial amounts of graphite linings peeling-off, passes through the high-speed revolution shearing of Vibration Extrusion machine
The field of force and the vibration drawing field of force, peeling-off crystalline flake graphite is set quickly to peel off into graphene microchip；
（3）By step（2）The graphene microchip obtained through twin-screw Vibration Extrusion machine is added to 100 parts of Arabic glue
In solution, 20 ~ 40min is dispersed with stirring at 60~80 DEG C, then cools down, stand, filter, in 60 ~ 80 DEG C of dryings, obtain organic micro-
The graphene microchip of capsule cladding；
（4）By step（3）The graphene microchip of obtained organic microcapsule coated is crushed to the powder that particle diameter is less than 10 μm,
It can be used as heat-conducting plastic special graphite alkene microplate.
Claims (8)
- A kind of 1. preparation method of heat-conducting plastic special graphite alkene microplate, it is characterised in that：It is main to use natural flake graphite Raw material, by urea intercalation modifying, sheared using twin-screw Vibration Extrusion machine and peel off acquisition graphene, then pass through organic micro- glue Capsule cladding handles to obtain powdered heat-conducting plastic special graphite alkene microplate, and specific preparation method is as follows：（1）By the natural flake graphite of 70~80 parts by weight, the nano inorganic powder of 10~15 parts by weight, 5~10 parts by weight Stearate mixes 30~50min by expanded extruder and obtains pre-composition；（2）By step（1）Obtained pre-composition and concentration is 10~20mol/L urea liquid by 1：5~10 mass ratio mixes After conjunction, react 1~2h under 60~80 DEG C, stirring, centrifuge, gained sediment washed with absolute ethyl alcohol, dry after, be made Urea intercalated graphite compound；Then urea intercalated graphite compound is pumped into twin-screw Vibration Extrusion machine, twin-screw vibration is squeezed Go out machine to set gradually ground section, intercalation section from feed end to discharge end, peel off section, 60~80 DEG C of control ground section temperature；Intercalation 150~180 DEG C of Duan Wendu；Peel off 180~360 DEG C of section temperature；In screw extruder extrusion, intercalation is in graphite composite In urea decompose and discharge substantial amounts of gas, make substantial amounts of graphite linings peeling-off, rotated by the high speed of Vibration Extrusion machine Shearing force field and the vibration drawing field of force, peeling-off crystalline flake graphite is set quickly to peel off into graphene microchip；（3）By step（2）The graphene microchip obtained through twin-screw Vibration Extrusion machine is added to 80~100 parts of organic polymer In the aqueous solution, 20~40min is dispersed with stirring at 60~80 DEG C, then cools down, stand, filter, in 60~80 DEG C of dryings, had The graphene microchip of machine microcapsule coated；（4）By step（3）The graphene microchip of obtained organic microcapsule coated is crushed to the powder that particle diameter is less than 10 μm, you can As heat-conducting plastic special graphite alkene microplate.
- 2. a kind of preparation method of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described Natural flake graphite is that radial dimension is more than 50 microns, crystalline flake graphite of the carbon content more than 97%.
- 3. a kind of preparation method of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described Nano inorganic powder is at least one of nano aluminium oxide, nano aluminum nitride, nm-class boron nitride, nano silicon.
- 4. a kind of preparation method of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described Stearate is water-based stearate, including at least one of water-based magnesium stearate, odium stearate, water-based zinc stearate.
- 5. a kind of preparation method of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described The rotating speed of twin-screw Vibration Extrusion machine is 1000~1500rpm.
- 6. a kind of preparation method of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described Organic polymer is polymethylacrylic acid, at least one in polyacrylamide, Ionic water-soluble epoxy resin, Arabic gum Kind.
- 7. a kind of preparation method of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described The content of organic polymer is 10~30% in the organic polymer aqueous solution.
- 8. a kind of preparation method of heat-conducting plastic special graphite alkene microplate according to claim 1, it is characterised in that described Graphene microchip is directly appended to heat-conducting plastic.
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