CN106117747A - A kind of preparation method of Graphene modified poly ethylene composite - Google Patents
A kind of preparation method of Graphene modified poly ethylene composite Download PDFInfo
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- CN106117747A CN106117747A CN201610598898.6A CN201610598898A CN106117747A CN 106117747 A CN106117747 A CN 106117747A CN 201610598898 A CN201610598898 A CN 201610598898A CN 106117747 A CN106117747 A CN 106117747A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/20—Recycled plastic
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Abstract
A kind of preparation method with electric heating and heat sinking function thin film is graphene oxide solution ultrasonic disperse, obtains graphene oxide solution carbon solution, and carbon fiber substrate is dried after impregnating in poly-vinyl alcohol solution, obtains containing polyvinyl alcohol carbon fiber substrate；To be combined with graphene oxide solution carbon solution containing polyvinyl alcohol carbon fiber substrate, obtain carbon fiber/graphene oxide composite membrane；The carbon fiber obtained/graphene oxide composite membrane is carried out high-temperature hot reduction in inertia or reducing atmosphere, obtains electric heating and heat sinking function thin film.The present invention has low cost, good cycling stability, the advantage that can be mass-produced.
Description
Technical field
The invention belongs to technical field of polymer composite materials, relate to the system of a kind of Graphene modified poly ethylene composite
Preparation Method.
Background technology
Graphene is a kind of allotrope of carbon, and it is through sp by monolayer carbon atom2What hydridization was constituted has Cellular Networks
The two-dimensional material of shape structure.Due to numerous startling character such as calorifics, mechanics, optics and electricity that Graphene is excellent, closely
By concern that scientific circles are extensive and lasting over a little years.The intensity of Graphene is to have tested in material the highest, reaches 130GPa,
Its carrier mobility is 15000cm2·.v-1·.s-1, thermal conductivity is up to 50000W m-1·.K-1.A small amount of Graphene
Just can be remarkably reinforced mechanical property (the J.R. Potts et al. Graphene-based polymer of macromolecular material
The graphene-based polymer composites of nanocomposites [J]. Polymer 52 (2011) 5-25).Along with country is to stone
The great attention of ink alkene industry and the development of graphene preparation technology, low cost mass prepares high-quality Graphene
For possible, this enables Graphene to be really applied in polymeric material as high-quality Nano filling, prepares high performance Graphene
Polymer nanocomposites.
Macromolecular material be not only the clothing, food, lodging and transportion--basic necessities of life of industrial and agricultural production and people with etc. provide widely, make rapid progress new
Product and new material, the also development for new and high technology provide high performance structures material and functional material.Polyethylene is a kind of
There is crystallinity, nonpolar thermoplastic resin, chemical stability is strong, but mechanical property is poor, actually used in need to add
The shortcoming that a lot of reinforcing agents overcome its poor mechanical property.Graphene just can substantially increase as material upstart, few addition
Strong material mechanical performance.At present, Graphene/composite polyethylene material report is the most fewer.It is related to Graphene/high-density polyethylene
The report of olefinic functionality material, but the addition of Graphene is the highest, and have ignored mechanical property (Chinese invention patent
N103756103A).
Summary of the invention
It is an object of the invention to provide the preparation side of the high Graphene modified poly ethylene composite of a kind of mechanical property
Method.
Its preparation method of the present invention a kind of Graphene modified poly ethylene composite, this composite is to be filled out by Graphene
Material enhanced polyethylene matrix is constituted, and mechanical property is strengthened, and can apply to the field such as cable material, reinforced plastics.
The Graphene modified poly ethylene composite of the present invention, it include Graphene and polyethylene, wherein Graphene exists
In composite, shared mass percent is 0.05-0.5wt%.
The technical solution used in the present invention is:
(1) weigh Graphene, carry out incipient impregnation with dehydrated alcohol, the Graphene after dipping and polyethylene are sufficiently stirred for,
Obtaining premix material, wherein Graphene shared mass percent in the composite is 0.05-0.5wt%；
(2) premix material is added and banbury adjusts kneading temperature and rotating speed, carry out taking out after kneading processes 14-25 minute being combined
Material, cooling；
(3) and by the composite wood obtained carry out broken after carry out hot-forming, extrude or be blow molded.
High density (the 0.941-0.970g/cm that polyethylene is a diameter of 3-5mm described in step (1)3) polyethylene particle,
Low-density (the 0.910-0.925g/cm of a diameter of 3-5mm3) polyethylene, the linea low density (0.910-of a diameter of 3-5mm
0.940g/cm3) polyethylene particle.
Mixing time described in step (1) is the stirring of 3-6min, stirring rod or agitating device blade chamber wall to be pressed close to.
Premix material described in step (2) adds the 85-95% that amount is cavity volume in banbury.
In step (2), banbury is first preheated before referring to charging by kneading, and preheating temperature is higher than polyethylene fusing point 80-
100℃.Temperature parameter is modified by kneading process, after material melts, operating temperature is turned down 10-30 DEG C than preheating temperature,
Carry out kneading process further.
The kneading rotating speed of step (2) is banburying initial stage 2-4min, and rotating speed is set to 120-180r/min, banburying 10-in mid-term
17 min, rotating speed is set to 360-480r/min, and banburying later stage 2-4min, rotating speed is set to 750-900r/min.
Kneading described in step (2) is to carry out evacuation process in whole kneading process, it is ensured that the sealing of working cavity
Property.
Shattering process described in step (3) be disintegrating machine rotating speed be 8000-12000r/min, the broken time is 50-
80s。
Advantages of the present invention and benefit be:
(1) composite prepared by the present invention, the addition of Graphene is few, and mass percent is only 0.05-0.5%.Graphite
Alkene/polyethylene is compared with pure polyethylene, and mechanical property increases substantially, and hot strength promotes 5.98MPa-8.1MPa.
(2) present invention uses the method for melting mixing to prepare Graphene/composite polyethylene material.The method effectively avoids molten
The environmental pollution that liquid method causes, overcomes the high cost of situ aggregation method simultaneously.Present invention process is simple, and efficiency is high, can be used for
Industrialization large-scale production high-performance masterbatch.
(3) composite prepared by the present invention, the Graphene of use is not through functionalization, it is to avoid Graphene Optimality
Loss of energy, decreases the use of chemical agent, simple to operate, environmental protection.The present invention make use of the strong of banbury cleverly
Shearing force and frictional force make graphene uniform be scattered in matrix.
Accompanying drawing explanation
Fig. 1 (a) is the electromicroscopic photograph of polyethylene in comparative example of the present invention；
Fig. 1 (b) is composite electromicroscopic photograph in the embodiment of the present invention 4；
Fig. 2 is comparative example of the present invention and the stress-strain diagram of embodiment 4 composite；
Fig. 3 is comparative example of the present invention and the melting enthalpy curve of embodiment 4 composite.
Detailed description of the invention
Being explained in further detail the present invention below by example, the polyethylene mentioned in the present invention includes low-density
Polyethylene, high density polyethylene (HDPE), linear low density polyethylene and reclaimed materials thereof, but it is not limited to above raw material.Embodiment is to this
Bright being specifically described, the present embodiment is served only for being further detailed the present invention, it is impossible to be interpreted as the guarantor to the present invention
Protect the restriction of scope, those skilled in the art as described above present disclosure is made some nonessential improvement and
Adjust, belong to protection scope of the present invention.
Embodiment 1:
(1) 0.05g Graphene and high density (0.96 g/cm of a diameter of 3-4mm of 100g are weighed3) polyethylene particle, Graphene
The percent accounting for gross mass is 0.05%, with dehydrated alcohol, Graphene is carried out incipient impregnation.After high density polyethylene (HDPE) and dipping
Graphene mix, carry out being sufficiently stirred for 4min by stirring rod.
(2) during the material of premixing joins the banbury being preheated to 250 DEG C, after adding the material of 95% of cavity volume, with
Time cavity is carried out evacuation, temperature is set to 230 DEG C, rotating speed be set to 150r/min run 3min, rotating speed is set to 450r/
Min runs 15min, finally rotating speed is set to 900r/min and runs 3min.
(3) turn off actuating device, after taking out the material cooling of mixing, use 12000r/min high speed pulverization crusher machine 50s.
(4) weighing the composite after 7g crushes hot-forming under the mould of 7cm*7cm, thickness is 1mm composite
Sheet material.With film cutter, the sheet material after hot pressing being cut into the dumbbell shaped of standard, testing its hot strength with omnipotent mechanics tester is
30.6MPa(high density polyethylene (HDPE) hot strength is 22.7MPa).
Embodiment 2
(1) 0.1g Graphene and low-density (0.92 g/cm of a diameter of 3-4mm of 100g are weighed3) polyethylene particle, Graphene accounts for
The percent of gross mass is 0.1%, with dehydrated alcohol, Graphene is carried out incipient impregnation.After Low Density Polyethylene and moistening
Graphene mixes, and carries out being sufficiently stirred for 3min by stirring rod.
(2) during the material of premixing joins the banbury being preheated to 230 DEG C, after adding the material of 90% of cavity volume, with
Time cavity is carried out evacuation, temperature is set to 220 DEG C, rotating speed be set to 120r/min run 2min, rotating speed is set to 450r/
Min runs 15min, finally rotating speed is set to 800r/min and runs 4min.
(3) turn off actuating device, after taking out the material cooling of mixing, crush 60s with the pulverizer of 10000r/min.
(4) weighing the composite after 7g crushes hot-forming under the mould of 7cm*7cm, thickness is 1mm composite
Sheet material.With film cutter, the sheet material after hot pressing being cut into the dumbbell shaped of standard, testing its hot strength with omnipotent mechanics tester is
15.9MPa(Low Density Polyethylene hot strength is 9.7MPa).
Embodiment 3:
(1) weigh 0.1g Graphene and a diameter of 4-5mm of 100g reclaims low-density (0.91 g/cm3) polyethylene particle, Graphene
The percent accounting for gross mass is 0.1%, with dehydrated alcohol, Graphene is carried out incipient impregnation.Reclaim Low Density Polyethylene and profit
Graphene after wet mixes, and carries out being sufficiently stirred for 4min by stirring rod.
(2) during the material of premixing joins the banbury being preheated to 220 DEG C, same after the material of the 85% of addition cavity volume
Time cavity is carried out evacuation, temperature is set to 210 DEG C, rotating speed be set to 180r/min run 4min, rotating speed is set to 480r/
Min runs 17min, finally rotating speed is set to 750r/min and runs 2min.
(3) turn off actuating device, after taking out the material cooling of mixing, use 9000r/min high speed pulverization crusher machine 70s.
(4) weighing the composite after 7g crushes hot-forming under the mould of 7cm*7cm, thickness is 1mm composite
Sheet material.With film cutter, the sheet material after hot pressing being cut into the dumbbell shaped of standard, testing its hot strength with omnipotent mechanics tester is
13.68MPa(high density polyethylene (HDPE) hot strength is 7.7MPa).
Embodiment 4:
(1) 0.25g Graphene and recovery high density (0.95 g/cm of a diameter of 4-5mm of 100g are weighed3) polyethylene particle, stone
It is 0.25% that ink alkene accounts for the percent of gross mass, with dehydrated alcohol, Graphene is carried out incipient impregnation.Recycled HDPE
Mix with the Graphene after moistening, carry out being sufficiently stirred for 5min by stirring rod.
(2) during the material of premixing joins the banbury being preheated to 240 DEG C, same after the material of the 93% of addition cavity volume
Time cavity is carried out evacuation, temperature is set to 230 DEG C, rotating speed be set to 140r/min run 3min, rotating speed is set to 360r/
Min runs 16min, finally rotating speed is set to 850r/min and runs 3min.
(3) turn off actuating device, after taking out the material cooling of mixing, use 8000r/min broken crusher machine 80s.
(4) weighing the composite after 7g crushes hot-forming under the mould of 7cm*7cm, thickness is 1mm composite
Sheet material.With film cutter, the sheet material after hot pressing being cut into the dumbbell shaped of standard, testing its hot strength with omnipotent mechanics tester is
18.05MPa(Recycled HDPE hot strength is 11.2MPa).
Embodiment 5:
(1) 0.25g Graphene and linea low density (0.93 g/cm of a diameter of 3-4mm of 100g are weighed3) polyethylene particle, stone
It is 0.25% that ink alkene accounts for the percent of gross mass, with dehydrated alcohol, Graphene is carried out incipient impregnation.Linear low density polyethylene
Mix with the Graphene after moistening, carry out being sufficiently stirred for 6min by stirring rod.
(2) during the material of premixing joins the banbury being preheated to 220 DEG C, same after the material of the 88% of addition cavity volume
Time cavity is carried out evacuation, temperature is set to 210 DEG C, rotating speed be set to 160r/min run 2min, rotating speed is set to 400r/
Min runs 14min, finally rotating speed is set to 880r/min and runs 2min.
(3) turn off actuating device, after taking out the material cooling of mixing, use 9000r/min high speed pulverization crusher machine 80s.
(4) weighing the composite after 7g crushes hot-forming under the mould of 7cm*7cm, thickness is 1mm composite
Sheet material.With film cutter, the sheet material after hot pressing being cut into the dumbbell shaped of standard, testing its hot strength with omnipotent mechanics tester is
34.68MPa(linear low density polyethylene hot strength is 26.7MPa).
Embodiment 6:
(1) 0.5g Graphene and recovery linea low density (0.92 g/cm of a diameter of 4-5mm of 100g are weighed3) polyethylene particle,
It is 0.5% that Graphene accounts for the percent of gross mass, with dehydrated alcohol, Graphene is carried out incipient impregnation.Reclaim linea low density
Graphene after polyethylene and moistening mixes, and carries out being sufficiently stirred for 6min by stirring rod.
(2) during the material of premixing joins the banbury being preheated to 230 DEG C, same after the material of the 90% of addition cavity volume
Time cavity is carried out evacuation, temperature is set to 200 DEG C, rotating speed be set to 150r/min run 4min, rotating speed is set to 480r/
Min runs 10min, finally rotating speed is set to 810r/min and runs 2min.
(3) turn off actuating device, after taking out the material cooling of mixing, use 8000r/min high speed pulverization crusher machine 70s.
(4) weighing the composite after 7g crushes hot-forming under the mould of 7cm*7cm, thickness is 1mm composite
Sheet material.With film cutter, the sheet material after hot pressing being cut into the dumbbell shaped of standard, testing its hot strength with omnipotent mechanics tester is
23.8MPa(high density polyethylene (HDPE) hot strength is 15.7MPa).
Embodiment 7:
(1) 0.05g Graphene and recovery high density (0.95 g/cm of a diameter of 4-5mm of 100g are weighed3) polyethylene particle, stone
It is 0.05% that ink alkene accounts for the percent of gross mass, with dehydrated alcohol, Graphene is carried out incipient impregnation.Recycled HDPE
Mix with the Graphene after moistening, carry out being sufficiently stirred for 6min by stirring rod.
(2) material of premixing add in joining the banbury being preheated to 240 DEG C cavity volume 95% material after simultaneously
Cavity being carried out evacuation, temperature is set to 210 DEG C, rotating speed is set to 150r/min and runs 3min, and rotating speed is set to 540r/
Min runs 14min, finally rotating speed is set to 810r/min and runs 3min.
(3) turn off actuating device, after taking out the material cooling of mixing, use 10000r/min high speed pulverization crusher machine 80s.
(4) weighing the composite after 7g crushes hot-forming under the mould of 7cm*7cm, thickness is 1mm composite
Sheet material.With film cutter, the sheet material after hot pressing being cut into the dumbbell shaped of standard, testing its hot strength with omnipotent mechanics tester is
16.8MPa(Recycled HDPE hot strength is 11.2MPa).
Comparative example 1:
In this comparative example, Graphene addition is 0, and raw material uses Recycled HDPE, and other feeds intake and processing step is with real
Executing example 4, testing its hot strength with omnipotent mechanics tester is 11.2MPa.
Claims (10)
1. a Graphene modified poly ethylene composite, it is characterised in that Graphene modified poly ethylene composite includes graphite
Alkene and polyethylene, wherein Graphene shared mass percent in the composite is 0.05-0.5wt%.
The preparation method of a kind of Graphene modified poly ethylene composite the most as claimed in claim 1, it is characterised in that include
Following steps:
(1) weigh Graphene, carry out incipient impregnation with dehydrated alcohol, the Graphene after dipping and polyethylene are sufficiently stirred for,
Obtaining premix material, wherein Graphene shared mass percent in the composite is 0.05-0.5wt%；
(2) premix material is added and banbury adjusts kneading temperature and rotating speed, carry out taking out after kneading processes 14-25 minute being combined
Material, cooling；
(3) and by the composite wood obtained carry out broken after carry out hot-forming, extrude or be blow molded.
The preparation method of a kind of Graphene modified poly ethylene composite the most as claimed in claim 1, it is characterised in that step
(1) polyethylene described in is a diameter of 3-5mm, and density is 0.941-0.970g/cm3Polyethylene；Or a diameter of 3-5mm, low
Density is 0.910-0.925g/cm3Polyethylene；Or a diameter of 3-5mm, density is 0.910-0.940g/cm3Polyethylene.
The preparation method of a kind of Graphene modified poly ethylene composite the most as claimed in claim 1, it is characterised in that step
(1) mixing time described in is 3-6min.
The preparation method of a kind of Graphene modified poly ethylene composite the most as claimed in claim 1, it is characterised in that step
(2) premix material described in adds the 85-95% that amount is cavity volume in banbury.
The preparation method of a kind of Graphene modified poly ethylene composite the most as claimed in claim 1, it is characterised in that step
(2) in, banbury is first preheated before being charging by kneading, and preheating temperature is higher than polyethylene fusing point 80-100 DEG C.
The preparation method of a kind of Graphene modified poly ethylene composite the most as claimed in claim 1, it is characterised in that step
(2) kneading process turns down 10-30 DEG C operating temperature than preheating temperature after material melts.
The preparation method of a kind of Graphene modified poly ethylene composite the most as claimed in claim 1, it is characterised in that step
(2) rotating speed of kneading is banburying initial stage 2-4min, and rotating speed is set to 120-180r/min, banburying 10-17 in mid-term min, rotating speed
Being set to 360-480r/min, banburying later stage 2-4min, rotating speed is set to 750-900r/min.
The preparation method of a kind of Graphene modified poly ethylene composite the most as claimed in claim 1, it is characterised in that step
(2) kneading described in is to carry out evacuation process in whole kneading process.
The preparation method of a kind of Graphene modified poly ethylene composite the most as claimed in claim 1, it is characterised in that step
(3) shattering process described in be disintegrating machine rotating speed be 8000-12000r/min, the broken time is 50-80s.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115260638A (en) * | 2022-09-15 | 2022-11-01 | 郑州大学 | High-strength polyethylene/graphene nano composite film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304887A (en) * | 2012-03-06 | 2013-09-18 | 上海杰事杰新材料(集团)股份有限公司 | Graphene-modified high-strength conductive polypropylene particles and preparation method thereof |
| CN104004251A (en) * | 2014-05-07 | 2014-08-27 | 武汉金牛经济发展有限公司 | Preparation method of graphene-modified heat-resistant polyethylene composite tubing |
| CN104151664A (en) * | 2014-05-07 | 2014-11-19 | 武汉金牛经济发展有限公司 | Preparation method of polyethylene composite pipes modified by using graphene |
| CN104479205A (en) * | 2014-12-09 | 2015-04-01 | 宁波大学 | Injection molding method of graphene-modified polyethylene high-strength composite thin product |
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2016
- 2016-07-27 CN CN201610598898.6A patent/CN106117747A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304887A (en) * | 2012-03-06 | 2013-09-18 | 上海杰事杰新材料(集团)股份有限公司 | Graphene-modified high-strength conductive polypropylene particles and preparation method thereof |
| CN104004251A (en) * | 2014-05-07 | 2014-08-27 | 武汉金牛经济发展有限公司 | Preparation method of graphene-modified heat-resistant polyethylene composite tubing |
| CN104151664A (en) * | 2014-05-07 | 2014-11-19 | 武汉金牛经济发展有限公司 | Preparation method of polyethylene composite pipes modified by using graphene |
| CN104479205A (en) * | 2014-12-09 | 2015-04-01 | 宁波大学 | Injection molding method of graphene-modified polyethylene high-strength composite thin product |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115260638A (en) * | 2022-09-15 | 2022-11-01 | 郑州大学 | High-strength polyethylene/graphene nano composite film and preparation method thereof |
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Application publication date: 20161116 |