CN109608744A - A kind of carbon nanotube enhancing polyethylene based composition and preparation method thereof - Google Patents
A kind of carbon nanotube enhancing polyethylene based composition and preparation method thereof Download PDFInfo
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- CN109608744A CN109608744A CN201811569413.6A CN201811569413A CN109608744A CN 109608744 A CN109608744 A CN 109608744A CN 201811569413 A CN201811569413 A CN 201811569413A CN 109608744 A CN109608744 A CN 109608744A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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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)
Abstract
The present invention provides a kind of carbon nanotube enhancing polyethylene based composition and preparation method thereof, is related to dielectric composite technical field.The material is after polyethylene, carbon nanotube and compatilizer are blended, and demoulding obtains after hot pressing and cold pressing；The polyethylene is low density polyethylene (LDPE)；The compatilizer is ethylene-octene-glycidyl methacrylate elastomer.The present invention also provides a kind of preparation methods of carbon nanotube enhancing polyethylene based composition.Composite material dielectric constant of the invention is high, dielectric loss is low.
Description
Technical field
The present invention relates to dielectric composite technical fields, and in particular to a kind of carbon nanotube enhancing polyvinyl is compound
Material and preparation method thereof.
Background technique
Since 21st century, with the quickening of the rapid development industrialization and Development of China's Urbanization of China's economic, electric energy is made
There is nervous situation in demand.China's UHV transmission technology has obtained the approval of international industry, this builds the overseas power grid in China
If having obtained significantly promoting, the construction for global power internet provides possibility.With the continuous improvement of voltage class, surpass
The development of high voltage power transmission and UHV transmission proposes more severe requirement to the dielectric properties of Electric Power Equipment Insulation material.
Polyethylene is widely used in cable industry due to its excellent insulation performance.It is reported that polyethylene is only made in recent years
For the insulating materials of power circuit, in global annual consumption with regard to oneself up to more than 60 ten thousand tons.However, polyethylene for a long time by electricity,
When heat and other various chemical factors act on, insulation performance can be gradually reduced, i.e. the aging of insulating materials.So in order to mention
High polymer dielectric strength prolongs its service life, and domestic and foreign scholars have done many-sided research work, mainly to polyethylene material
It is special to improve polyethylene breakdown that the particles such as certain additive particles, such as addition magnesia, montmorillonite, silica are added in material
Property, reduce polymeric acceptor in defect, change crystal habit, improve carrier mobility characteristics and improve electric field concentration, improve polymerization
The performances such as object thermal stability and glass transition temperature.But inorganic additive is when improving material performance in a certain respect, it is possible to
It will lead to the decline of other performances.Test discovery micro materials are improving polymer hot property while will lead to polymer breakdown
The reduction of field strength, nano material can reduce the glass transition temperature of material while enhancing electrostrictive polymer performance.So for
The research of polyethylene insulation material dielectricity causes the extensive concern of related scholar.
Summary of the invention
It cannot meet that dielectric constant is high, dielectric loss is low simultaneously the purpose of the present invention is to solve existing composite material
The problem of, and a kind of carbon nanotube enhancing polyethylene based composition is provided and preparation method thereof.
Present invention firstly provides a kind of carbon nanotubes to enhance polyethylene based composition, which is to receive polyethylene, carbon
After mitron and compatilizer are blended, demoulding is obtained after hot pressing and cold pressing；
The polyethylene is low density polyethylene (LDPE)；
The compatilizer is ethylene-octene-glycidyl methacrylate elastomer.
Preferably, the density of the polyethylene is 0.9203g/cm3。
Preferably, the carbon nanotube is the carbon nanotube that surface has carboxyl.
The present invention also provides a kind of preparation methods of carbon nanotube enhancing polyethylene based composition, comprising:
Step 1: carbon nanotube, polyethylene, compatilizer are subjected to solution blending, obtain blend；
Step 2: step 1 blend is placed in mold and carries out hot pressing, is then transferred in cold press and is cold-pressed, is demoulded
Enhance polyethylene based composition to carbon nanotube.
Preferably, the mass ratio of polyethylene, compatilizer and carbon nanotube is (84-90) in the step one: 10:
(0.5-6)。
Preferably, the blending temperature of the step one is 85-95 DEG C, and the blending time is 50-60min.
Preferably, the hot pressing temperature of the step two be 130-140 DEG C, pressure 8-13Mpa, hot pressing time 5-
10 minutes.
Preferably, in the step two temperature of colding pressing be 20-25 DEG C, pressure 8-13Mpa, the cold pressing time be 5-10
Minute.
Beneficial outcomes of the invention
The present invention provides a kind of carbon nanotube enhancing polyethylene based composition and preparation method thereof, composite wood of the invention
Material is using low density polyethylene (LDPE) as matrix, and since the low density polyethylene (LDPE) degree of branching is higher, the good performance such as high resiliency, utilization is compatible
Agent ethylene-octene-glycidyl methacrylate (POE-GMA), copolymer of the one side POE as ethylene and octene can be with
Have a good compatibility with matrix low density polyethylene (LDPE), after the epoxy ring-opening in another aspect glycidyl methacrylate with
Esterification occurs for the carboxyl of carbon nano tube surface, and ethylene-octene-glycidyl methacrylate is made to be grafted to carbon nanotube table
On face, effective cladding to carbon nanotube is realized, so that carbon nanotube be made to may be implemented in low-density polyethylene body well
Dispersion, reduce carbon nanotube reunite the phenomenon that, further increase the dielectric properties of composite material.Meanwhile preparation of the invention
Method is simple, and raw material is easy to get, pollution-free.
Detailed description of the invention
Fig. 1 is the process schematic that the present invention prepares composite material；
Fig. 2 be dielectric constant when composite material obtained by embodiment 1-6 measures 1kHz at room temperature and dielectric loss with
The relational graph of carbon nanotube mass score variation；
Fig. 3 be dielectric constant when composite material obtained by comparative example 1-6 measures 1kHz at room temperature and dielectric loss with
The relational graph of carbon nanotube mass score variation；
Specific embodiment
Present invention firstly provides a kind of carbon nanotubes to enhance polyethylene based composition, which is to receive polyethylene, carbon
After mitron and compatilizer are blended, demoulding is obtained after hot pressing and cold pressing；The polyethylene is low density polyethylene (LDPE), poly- second
The density of alkene is preferably 0.9203g/cm3, the compatilizer is ethylene-octene-glycidyl methacrylate elastomer, institute
The carbon nanotube stated is the carbon nanotube that surface has carboxyl.
According to the present invention, the low density polyethylene (LDPE) (LDPE), ethylene-octene-glycidyl methacrylate (POE-
GMA) and the source of carbon nanotube be commercially available, described low density polyethylene (LDPE) be Yanshan Petrochemical company；Ethylene/octene-methyl-prop
Olefin(e) acid polyglycidyl is preferably preferred the model SOG-02 of Yi Rong company, and the carbon nanotube is preferably surface with carboxyl
The model TNMC3 of carbon nanotube, preferably Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences production.
Composite material of the invention is to utilize compatilizer ethylene-octene-methacrylic acid using low density polyethylene (LDPE) as matrix
On the one hand polyglycidyl (POE-GMA), POE are used as the copolymer of ethylene and octene, can there is good phase with matrix polyethylene
With the carboxyl of carbon nano tube surface esterification occurs for capacitive after another aspect glycidyl methacrylate epoxy ring-opening,
It is grafted to ethylene-octene-glycidyl methacrylate in carbon nano tube surface, realizes effective cladding to carbon nanotube,
To make carbon nanotube that good dispersion may be implemented in low-density polyethylene body, the phenomenon that carbon nanotube is reunited is reduced,
Further increase the dielectric properties of composite material.
The present invention also provides a kind of preparation method of carbon nanotube enhancing polyethylene based composition, the mistakes of the composite material
Journey schematic diagram as shown in Figure 1, this method comprises:
Step 1: carbon nanotube, polyethylene, compatilizer are subjected to solution blending, obtain blend；
Step 2: step 1 blend is placed in mold and carries out hot pressing, is then transferred in cold press and is cold-pressed, is demoulded
Enhance polyethylene based composition to carbon nanotube.
According to the present invention, polyethylene, ethylene/octene-glycidyl methacrylate, carbon nanotube in the step one
Mass ratio be preferably (84-90): 10:(0.5-6), more preferable 85:10:5, when the mass fraction of carbon nanotube be 5% when, material
The dielectric loss of material only slightly reduces, but its dielectric constant is sharply increased.And when content of carbon nanotubes is higher than 5%, though
Its right dielectric constant has a distinct increment, but its dielectric loss is promoted also more obviously.
According to the present invention, the solution blending temperature of the step one is preferably 85-95 DEG C, more preferably 90 DEG C, is blended
Time is preferably 50-60min, more preferably 50min, and drying obtains polyethylene based composition after sedimentation.
According to the present invention, the hot pressing temperature of the step two is preferably 130-140 DEG C, pressure is preferably 8-13Mpa, heat
Pressing the time is preferably 5-10 minute, and temperature of colding pressing is preferably 20-25 DEG C, pressure is preferably 8-13Mpa, and being cold-pressed the time is preferably 5-
10 minutes.
In order to become apparent from the other advantage of the present invention, technical solution, the present invention is done in detail combined with specific embodiments below
Illustrate, the raw material being related in embodiment is commercially available.
Embodiment 1
By low density polyethylene (LDPE) (density 0.9203g/cm3), ethylene-octene-glycidyl methacrylate, surface band
The carbon nanotube for having carboxyl is 89:10:1 in 90 DEG C of progress solution blending 50min in mass ratio, sedimentation, drying obtain polyethylene/
Ethylene-octene-glycidyl methacrylate/carbon nano tube compound material.
Polyethylene/vinyl-octene-glycidyl methacrylate/carbon nano tube compound material is placed in mold, is heated
To 140 DEG C, hot pressing 5 minutes under the pressure of 10MPa maintain to be cold-pressed 5 minutes at 25 DEG C under pressure condition, and demoulding is answered
Condensation material.
Composite material dielectric constant obtained by embodiment 1 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in Fig. 2, the dielectric constant of material is 4.2, and dielectric loss is at this time when carbon nanotube mass score is 1wt%
0.08。
Embodiment 2
With embodiment 1, difference is for step and condition, poly- low density polyethylene (LDPE), ethylene-octene-glycidyl
The carbon nanotube of propyl ester, surface with carboxyl is that 88:10:2 is added in mass ratio, obtains composite material.
Composite material dielectric constant obtained by embodiment 2 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in Fig. 2, the dielectric constant of material is 5.8, and dielectric loss is 0.15 at this time.
Embodiment 3
With embodiment 1, difference is for step and condition, poly- low density polyethylene (LDPE), ethylene-octene-glycidyl
The carbon nanotube of propyl ester, surface with carboxyl is that 87:10:3 is added in mass ratio, obtains composite material.
Composite material dielectric constant obtained by embodiment 3 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in Fig. 2, the dielectric constant of material is 6.7, and dielectric loss is 0.16 at this time.
Embodiment 4
With embodiment 1, difference is for step and condition, poly- low density polyethylene (LDPE), ethylene-octene-glycidyl
The carbon nanotube of propyl ester, surface with carboxyl is that 86:10:4 is added in mass ratio, obtains composite material.
Composite material dielectric constant obtained by embodiment 4 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in Fig. 2, the dielectric constant of material is 9.4, and dielectric loss is 0.24 at this time.
Embodiment 5
With embodiment 1, difference is for step and condition, poly- low density polyethylene (LDPE), ethylene-octene-glycidyl
The carbon nanotube of propyl ester, surface with carboxyl is that 85:10:5 is added in mass ratio, obtains composite material.
Composite material dielectric constant obtained by embodiment 5 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in Fig. 2, the dielectric constant of material is 84, and dielectric loss is 0.55 at this time.
Embodiment 6
With embodiment 1, difference is for step and condition, poly- low density polyethylene (LDPE), ethylene-octene-glycidyl
The carbon nanotube of propyl ester, surface with carboxyl is that 84:10:6 is added in mass ratio, obtains composite material.
Composite material dielectric constant obtained by embodiment 6 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in Fig. 2, the dielectric constant of material is 179, and dielectric loss is 7.13 at this time.
Table 1 is the crystallinity and crystallization temperature table of composite material obtained by embodiment 1-6:
Table 1
As seen from Table 1, with the increase of carbon nanotube filler content, the crystallization temperature of composite material increases therewith, this
Be because carbon nanotube as heterogeneous nucleation agent, accelerate crystalline rate, improve the crystallization temperature of composite material, meanwhile, tie
Brilliant degree decline, this is because the draw ratio of carbon nanotube is big, limits the movement of polymer chain, leaves behind sub-fraction space use
It crystallizes, the free volume of system rises, these free volumes exist again in the form in " hole ", so crystallinity is with carbon nanometer
The increase of tube packing content and decline.When content of carbon nanotubes increases, dielectric constant and dielectric loss are consequently increased, system
Free volume increase, the quantity in hole is consequently increased, the crystallinity decline of system.It can be seen that crystallization temperature and crystallinity are to multiple
The dielectric constant and dielectric loss of condensation material are influential.
Comparative example 1
With embodiment 1, difference is for step and condition, and ethylene-octene-glycidyl methacrylate is added without in step
The carbon nanotube of elastomer, low density polyethylene (LDPE) and surface with carboxyl is according to mass ratio 99:1 in 90 DEG C of progress solution blendings
50min obtains polyethylene/carbon nano tube compound material.
Composite material dielectric constant obtained by comparative example 1 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in figure 3, the dielectric constant of material is 3.8, and dielectric loss is at this time when carbon nanotube mass score is 1wt%
0.02。
Comparative example 2
With comparative example 1, difference is for step and condition, the carbon nanotube of low density polyethylene (LDPE) and surface with carboxyl according to
Mass ratio 98:2 is added.
Composite material dielectric constant obtained by comparative example 2 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in figure 3, the dielectric constant of material is 4.4, and dielectric loss is 0.03 at this time.
Comparative example 3
With comparative example 1, difference is for step and condition, the carbon nanotube of low density polyethylene (LDPE) and surface with carboxyl according to
Mass ratio 97:3 is added.
Composite material dielectric constant obtained by comparative example 3 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in figure 3, the dielectric constant of material is 4.78, and dielectric loss is 0.03 at this time.
Comparative example 4
With comparative example 1, difference is for step and condition, the carbon nanotube of low density polyethylene (LDPE) and surface with carboxyl according to
Mass ratio 96:4 is added.
Composite material dielectric constant obtained by comparative example 4 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in figure 3, the dielectric constant of material is 7.12, and dielectric loss is 0.04 at this time.
Comparative example 5
With comparative example 1, difference is for step and condition, the carbon nanotube of low density polyethylene (LDPE) and surface with carboxyl according to
Mass ratio 95:5 is added.
Composite material dielectric constant obtained by comparative example 5 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in figure 3, the dielectric constant of material is 7.94, and dielectric loss is 0.04 at this time.
Comparative example 6
With comparative example 1, difference is for step and condition, the carbon nanotube of low density polyethylene (LDPE) and surface with carboxyl according to
Mass ratio 94:6 is added.
Composite material dielectric constant obtained by comparative example 6 is tested to obtain with dielectric loss by alternating current impedance instrument, result
As shown in figure 3, the dielectric constant of material is 17.12, and dielectric loss is 0.13 at this time.
Can illustrate from the embodiment of the present invention and comparative example of Fig. 2 and Fig. 3: MWCNT/PE composite material has very low dielectric
Constant and dielectric loss, and as can be seen from Figure 2 dielectric constant has significantly for PE/POE-GMA/MWCNT composite material
It improves, dielectric loss also improves relatively.According to micro- capacitor model, the increase of composite material dielectric constant is since system introducing is permitted
Caused by mostly micro- capacitor, the dispersion of carbon nanotube can form a large amount of micro- capacitor, composite material dielectric among composite material
Constant increases, but as the content of carbon nanotube increases, is equivalent to and provides a large amount of reaction interface, interfacial polarization for matrix
It is consequently increased, dielectric loss is caused also to increase.Figure it is seen that when content of carbon nanotubes increases to 5%, PE/POE-
The dielectric constant of GMA/MWCNT composite material is 84, and dielectric loss is only 0.55, when content of carbon nanotubes increases to 6%,
Dielectric constant is 179, and the huge raising of dielectric loss, has reached 7.13, this is because content of carbon nanotubes is excessive, make its
Three-dimensional conductive network is formed in low density polyethylene (LDPE), forms leakage current, and dielectric loss significantly improves, to reduce its effectively benefit
The property used.Therefore the present invention should rationally control the content of carbon nanotube and compatilizer, reach dielectric constant and dielectric loss with this
Balance.
Claims (8)
1. a kind of carbon nanotube enhances polyethylene based composition, which is characterized in that the material be by polyethylene, carbon nanotube and
After compatilizer is blended, demoulding is obtained after hot pressing and cold pressing；
The polyethylene is low density polyethylene (LDPE)；
The compatilizer is ethylene-octene-glycidyl methacrylate elastomer.
2. a kind of carbon nanotube according to claim 1 enhances polyethylene based composition, which is characterized in that described is poly-
The density of ethylene is 0.9203g/cm3。
3. a kind of carbon nanotube according to claim 1 enhances polyethylene based composition, which is characterized in that the carbon
Nanotube is the carbon nanotube that surface has carboxyl.
4. a kind of preparation method of carbon nanotube enhancing polyethylene based composition described in claim 1, which is characterized in that packet
It includes:
Step 1: carbon nanotube, polyethylene, compatilizer are subjected to solution blending, obtain blend；
Step 2: step 1 blend being placed in mold and carries out hot pressing, is then transferred in cold press and is cold-pressed, and demoulding obtains carbon
Nanotube enhances polyethylene based composition.
5. a kind of preparation method of carbon nanotube enhancing polyethylene based composition according to claim 4, feature exist
In the mass ratio of polyethylene, compatilizer and carbon nanotube is (84-90): 10:(0.5-6 in the step one).
6. a kind of preparation method of carbon nanotube enhancing polyethylene based composition according to claim 4, feature exist
In the blending temperature of the step one is 85-95 DEG C, and the blending time is 50-60min.
7. a kind of preparation method of carbon nanotube enhancing polyethylene based composition according to claim 4, feature exist
In, the hot pressing temperature of the step two be 130-140 DEG C, pressure 8-13Mpa, hot pressing time is 5-10 minutes.
8. a kind of preparation method of carbon nanotube enhancing polyethylene based composition according to claim 4, feature exist
In, in the step two temperature of colding pressing be 20-25 DEG C, pressure 8-13Mpa, cold pressing the time be 5-10 minutes.
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Cited By (1)
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| CN114891350A (en) * | 2022-06-17 | 2022-08-12 | 山东海科创新研究院有限公司 | High-performance antistatic filler, polyether sulfone composite material containing antistatic material and preparation method of polyether sulfone composite material |
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