CN108285630A - A kind of graphene/thermoplastic transparent composite and preparation method thereof - Google Patents

A kind of graphene/thermoplastic transparent composite and preparation method thereof Download PDF

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CN108285630A
CN108285630A CN201810146814.4A CN201810146814A CN108285630A CN 108285630 A CN108285630 A CN 108285630A CN 201810146814 A CN201810146814 A CN 201810146814A CN 108285630 A CN108285630 A CN 108285630A
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graphene
transparent composite
thermoplastic transparent
parts
thermoplastic
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黄巧玲
陈紫萦
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Huazhou City Associating People's Livelihood Lun Ye Co Ltd
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Huazhou City Associating People's Livelihood Lun Ye Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L69/00Compositions of polycarbonates; Compositions of derivatives of polycarbonates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/10Transparent films; Clear coatings; Transparent materials
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/08Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers

Abstract

The present invention discloses a kind of graphene/thermoplastic transparent composite and preparation method thereof.The composite material is counted in parts by weight, including the following raw material component:95~97.5 parts of thermoplastic;0.1~0.5 part of graphene;2~4 parts of compatilizer;0.2~0.5 part of antioxidant.Preparation method of the present invention includes the following steps:Each raw material is put into loading hopper dry-mixed in super mixer, then that the raw material mixed is put into double screw extruder by the parts by weight, through melting extrusion, is granulated, obtains the graphene/thermoplastic transparent composite.Graphene nano effect is more prominent in graphene/thermoplastic transparent composite of the present invention, makes composite material not only high transparency, but also have higher Martin Heat Resistant Temperature.

Description

A kind of graphene/thermoplastic transparent composite and preparation method thereof
Technical field
The present invention relates to thermoplastic transparent material field more particularly to a kind of graphene/thermoplastic are transparent multiple Condensation material and preparation method thereof.
Background technology
As a kind of novel two-dimension nano materials, graphene has excellent electrical property, hot property, mechanical performance etc., There is important potential application in Material Field.Graphene is prepared by graphite, and current most common preparation method is oxygen Change reduction method(101613098 B of Chinese invention patent CN).The preparation process is although simple and practicable, but strong due to largely using Acid, oxidant, waste reaction solution are difficult to handle, and serious pollution can be brought to natural environment.And only a few researcher is faced using super Boundary's carbon dioxide process prepares graphene(102515155 B of Chinese invention patent CN)Although will not be produced relative to oxidation-reduction method Raw waste reaction solution, but reaction medium carbon dioxide is greenhouse gases, needs specially to prepare, and can increase the earth table when being discharged after reaction Surface green house gas content can equally generate earth environment and seriously affect.
With economic development, the demand rapid growth of high transparency and high heat resistance thermoplastic.But current thermoplastic is normal Method of modifying cannot fully meet requirement (transparent and high heat-resisting).Although the addition of graphene can improve plastics Heat resistance(106188928 A of Chinese invention patent CN), but the transparency of composite material can be by the transparent of plastic substrate itself The influence of property, graphene size and auxiliary agent, does not occur graphene/thermoplastic transparent composite also at present in document.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to which it is transparent multiple to provide a kind of graphene/thermoplastic Condensation material.
The present invention also aims to provide the side for preparing a kind of graphene/thermoplastic transparent composite Method.The high stone of transparency is prepared in graphene and thermoplastic, compatilizer and antioxidant melt blending by the preparation method Black alkene/thermoplastic transparent composite.
The purpose of the present invention is achieved through the following technical solutions.
A kind of graphene/thermoplastic transparent composite, is counted, including the following raw material component in parts by weight:
95~97.5 parts of thermoplastic;
0.1~0.5 part of graphene;
2~4 parts of compatilizer;
0.2~0.5 part of antioxidant.
Further, the thermoplastic include polyethylene terephthalate -1,4-CHDM ester and One or more of lined polymethyl ethylene carbonate.
Further, the compatilizer is that lined polymethyl ethylene carbonate is grafted oxazoline and lined polymethyl ethylene carbonate grafting One or more of glycidyl methacrylate.
Further, the antioxidant includes the bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) of triethylene-glycol Propionic ester].
Further, the graphene is prepared via a method which to obtain:
It is passed through ethane gas into reaction kettle, the air in reaction kettle is discharged;Graphite powder and barrier are added in reaction kettle again, It is passed through ethane gas and propane gas, while being that 2 DEG C/min~5 DEG C/min is warming up to 100~120 DEG C, and makes with heating rate Air pressure reaches 5~7MPa in kettle, and after keeping the temperature 30~50 minutes, slow release pressure to atmospheric pressure obtains graphene.
Further, the barrier is one or more of palmitin acid butyl ester and octyl palmitate.
Further, the mass ratio of the barrier and graphite powder is 1:100~2:100.
Further, after being passed through ethane gas and propane gas, in reaction kettle, the molar ratio of ethane and propane is 1:1 ~3:1.
Further, after being passed through ethane gas and propane gas, in reaction kettle, the gross mass and graphite of ethane and propane The mass ratio of powder is 3:10~8:10.
The method for preparing a kind of graphene/thermoplastic transparent composite described in any one of the above embodiments, including it is as follows Step:
Each raw material put by the parts by weight dry-mixed in super mixer, then the raw material mixed is put into twin-screw The loading hopper of extruder through melting extrusion, is granulated, obtains the graphene/thermoplastic transparent composite.
Further, the dry-mixed time is 4~7min.
Further, the heating region of the double screw extruder is set as:One area's temperature is 100~130 DEG C, two area's temperature It it is 220~250 DEG C, three area's temperature are 220~240 DEG C, and four area's temperature are 220~240 DEG C, and head temperature is 220~235 DEG C.
Further, residence time 2~5 min of the raw material in twin-screw extrusion, pressure are 5~9 MPa.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1)The raw material sources of the present invention are extensive and environmentally protective, and the graphene used is using ethane/the third of supercriticality Alkane mixture is prepared, and will not additionally increase earth surface greenhouse gases content;
(2)Graphene nano effect is more prominent in graphene/thermoplastic transparent composite of the present invention, makes composite wood Expect not only high transparency, but also there is higher Martin Heat Resistant Temperature;
(3)Preparation method of the present invention is simple for process, is advantageously implemented industrialized production.
Specific implementation mode
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment, but the protection model of the present invention It encloses and embodiment is without being limited thereto.
In the specific embodiment of the invention, the graphene of use is prepared via a method which to obtain:
(1)Ethane gas is first passed through into reaction kettle(Air pressure is 0.5~2 MPa, and purity is more than 99.999%)30~45 minutes, By the air discharge in kettle;
(2)Again by graphite powder(200~500 μm of fineness)And barrier(One or more of palmitin acid butyl ester and octyl palmitate) It is added in reaction kettle, while being passed through ethane gas(Air pressure is 0.5~2 MPa, and purity is more than 99.999%)And propane gas(Gas Pressure is 0.5~2 MPa, and purity is more than 99.998%);
The molar ratio of ethane and propane is 1 in reaction kettle:1~3:1, the gross mass and graphite powder mass ratio of ethane and propane are 3: 10~8:10, the mass ratio of barrier and graphite powder is 1:100~2:100;
(3)So that the temperature of reaction kettle is risen to 100~120 DEG C with 2 DEG C/min~5 DEG C of heating rate/min, in kettle air pressure reach 5~ Air pressure in kettle is slowly lowered to atmospheric pressure, graphene is prepared by 7 MPa after being kept for 30~50 minutes with this condition, standby With.
In the specific embodiment of the invention, the preparation method of graphene/thermoplastic transparent composite specifically include as Lower step:
(1)Raw material is weighed by the parts by weight, then puts into dry-mixed 4~7min in SHR series of high speed mixers, main shaft 300~750 revs/min of rotating speed;
(2)The loading hopper that the raw material mixed is put into double screw extruder through melting extrusion, is granulated, obtains graphene/heat Thermoplastic plastic transparent composite;
Processing technology is as follows:One area's temperature of double screw extruder is 100~130 DEG C, and two area's temperature are 220~250 DEG C, three area's temperature Degree is 220~240 DEG C, and four area's temperature are 220~240 DEG C, and head temperature is 220~235 DEG C;When raw material stops in an extruder Between 2~5 min, pressure be 5~9 MPa.
Embodiment 1
A kind of graphene/thermoplastic transparent composite, is counted, including the following raw material component in parts by weight:
95 parts of lined polymethyl ethylene carbonate;
0.5 part of graphene;
Compatilizer(Lined polymethyl ethylene carbonate is grafted oxazoline)4 parts;
Antioxidant(Triethylene-glycol is bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester])0.5 part.
The graphene of use is made by the steps to obtain:
(1)Ethane gas is first passed through into reaction kettle(Air pressure is 0.5 MPa, and purity is more than 99.999%)It 45 minutes, will be in kettle Air is discharged;
(2)Again by graphite powder(200 μm of fineness)It is added in reaction kettle with barrier palmitin acid butyl ester, while being passed through ethane gas (Air pressure is 0.5 MPa, and purity is more than 99.999%)And propane gas(Air pressure is 0.5 MPa, and purity is more than 99.998%);
The molar ratio of ethane and propane is 1 in reaction kettle:1, the gross mass and graphite powder mass ratio of ethane and propane are 3:10, resistance Every the mass ratio of agent and graphite powder be 2:100;
(3)Make the temperature of reaction kettle with 2 DEG C/min of heating rate rise to temperature be 120 DEG C, in kettle air pressure reach 7 MPa, herein Under the conditions of kept for 30 minutes after, air pressure in kettle is slowly lowered to atmospheric pressure, graphene is prepared, it is spare.
A kind of above-mentioned graphene/thermoplastic transparent composite is prepared, is specifically comprised the following steps:
(1)95 parts of lined polymethyl ethylene carbonate, 0.5 part of graphene, compatilizer lined polymethyl ethylene carbonic acid are weighed in parts by weight Ester is grafted 4 parts of oxazoline and bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic acid of antioxidant triethylene-glycol Ester] 0.5 part, put into dry-mixed 4 min in SHR series of high speed mixers, 500 revs/min of the speed of mainshaft;
(2)The raw material mixed is put into the loading hopper of double screw extruder, wherein each heating region temperature of double screw extruder Setting is respectively:One area:100 ℃;2nd area:220 ℃;3rd area:220 ℃;4th area:220 ℃;Head:220 ℃;Raw material exists 2 min of residence time in extruder, pressure are 5 MPa;It through melting extrusion, is granulated, it is transparent multiple to obtain graphene/thermoplastic Condensation material.
Embodiment 2
A kind of graphene/thermoplastic transparent composite, is counted, including the following raw material component in parts by weight:
Polyethylene terephthalate -97.5 parts of 1,4 cyclohexane dimethanol ester;
0.3 part of graphene;
Compatilizer(Lined polymethyl ethylene carbonate graft glycidyl methacrylate)2 parts;
Antioxidant(Triethylene-glycol is bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester])0.2 part.
The graphene of use is made by the steps to obtain:
(1)Ethane gas is first passed through into reaction kettle(Air pressure is 1 MPa, and purity is more than 99.999%)35 minutes, by the sky in kettle Gas is discharged;
(2)Again by graphite powder(500 μm of fineness)It is added in reaction kettle with barrier octyl palmitate, while being passed through ethane gas (Air pressure is 1 MPa, and purity is more than 99.999%)And propane gas(Air pressure is 1 MPa, and purity is more than 99.998%);
The molar ratio of ethane and propane is 2 in reaction kettle:1, the gross mass and graphite powder mass ratio of ethane and propane are 6.5:10, The mass ratio of barrier and graphite powder is 1.6:100;
(3)Make the temperature of reaction kettle with 5 DEG C/min of heating rate rise to temperature be 1112 DEG C, in kettle air pressure reach 6.1 MPa, It keeps with this condition after forty minutes, air pressure in kettle is slowly lowered to atmospheric pressure, graphene is prepared, it is spare.
A kind of above-mentioned graphene/thermoplastic transparent composite is prepared, is specifically comprised the following steps:
(1)Polyethylene terephthalate -97.5 parts of 1,4 cyclohexane dimethanol ester, graphene are weighed in parts by weight 0.3 part, 2 parts of compatilizer lined polymethyl ethylene carbonate graft glycidyl methacrylate and three second two of contracting of antioxidant two 0.2 part of alcohol bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic esters] is put into SHR series of high speed mixers and is done Mixed 5 min, 300 revs/min of the speed of mainshaft;
(2)The raw material mixed is put into the loading hopper of double screw extruder, wherein each heating region temperature of double screw extruder Setting is respectively:One area:130℃;2nd area:250℃;3rd area:240℃;4th area:240℃;Head:235℃;Raw material is squeezing out 4 min of residence time in machine, pressure are 9 MPa;It through melting extrusion, is granulated, obtains the transparent composite wood of graphene/thermoplastic Material.
Embodiment 3
A kind of graphene/thermoplastic transparent composite, is counted, including the following raw material component in parts by weight:
Polyethylene terephthalate -90 parts of 1,4 cyclohexane dimethanol ester;
6 parts of lined polymethyl ethylene carbonate;
0.1 part of graphene;
Compatilizer(Lined polymethyl ethylene carbonate is grafted oxazoline)2 parts;
Compatilizer(Lined polymethyl ethylene carbonate graft glycidyl methacrylate)1.5 part;
Antioxidant(Triethylene-glycol is bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester])0.4 part,
The graphene of use is made by the steps to obtain:
(1)Ethane gas is first passed through into reaction kettle(Air pressure is 2 MPa, and purity is more than 99.999%)30 minutes, by the sky in kettle Gas is discharged;
(2)Again by graphite powder(350 μm of fineness)With the mixture of barrier palmitin acid butyl ester/octyl palmitate(Mass ratio is 1:1)It is added in reaction kettle, while being passed through ethane gas(Air pressure is 2 MPa, and purity is more than 99.999%)And propane gas(Air pressure For 2 MPa, purity is more than 99.998%);
The molar ratio of ethane and propane is 3 in reaction kettle:1, the gross mass and graphite powder mass ratio of ethane and propane are 8:10, resistance Every the mass ratio of agent and graphite powder be 1:100;
(3)Make the temperature of reaction kettle with 3 DEG C/min of heating rate rise to temperature be 100 DEG C, in kettle air pressure reach 5 MPa, herein Under the conditions of kept for 50 minutes after, air pressure in kettle is slowly lowered to atmospheric pressure, graphene is prepared, it is spare.
A kind of above-mentioned graphene/thermoplastic transparent composite is prepared, is specifically comprised the following steps:
(1)Polyethylene terephthalate -90 parts of 1,4 cyclohexane dimethanol ester, lined polymethyl ethylene are weighed in parts by weight 6 parts of carbonic ester, 0.1 part of graphene, 2 parts of oxazoline of compatilizer lined polymethyl ethylene carbonate grafting, compatilizer lined polymethyl ethylene 1.5 parts of carbonic ester graft glycidyl methacrylate and the bis- [β-(3- tertiary butyl -4- hydroxyls of antioxidant triethylene-glycol Base -5- aminomethyl phenyls) propionic ester] 0.4 part, put into dry-mixed 7 min, the speed of mainshaft 750 in SHR series of high speed mixers Rev/min;
(2)The raw material mixed is put into the loading hopper of double screw extruder, wherein each heating region temperature of double screw extruder Setting is respectively:One area:120℃;2nd area:240℃;3rd area:235℃;4th area:235℃;Head:230℃;Raw material is squeezing out 5 min of residence time in machine, pressure are 7.6 MPa;It through melting extrusion, is granulated, it is transparent compound to obtain graphene/thermoplastic Material.
Comparative example 1
A kind of graphene/thermoplastic transparent composite, is counted, including the following raw material component in parts by weight:
95 parts of lined polymethyl ethylene carbonate;
0.5 part of graphene (ug-SGraphene-02, Suzhou You Gao nano materials Co., Ltd, thickness 0.7-1.2nm);
Compatilizer(Lined polymethyl ethylene carbonate is grafted oxazoline)4 parts;
Antioxidant(Triethylene-glycol is bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester])0.5 part.
A kind of above-mentioned graphene/thermoplastic transparent composite is prepared, is specifically comprised the following steps:
(1)95 parts of lined polymethyl ethylene carbonate, graphene are weighed in parts by weight(Ug-SGraphene-02, the excellent zirconium in Suzhou are received Rice Materials Co., Ltd, thickness 0.7-1.2nm)0.5 part, compatilizer lined polymethyl ethylene carbonate 4 parts of oxazoline of grafting and anti- 0.5 part of oxygen agent triethylene-glycol bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic esters] puts into SHR series Dry-mixed 4 min in super mixer, 500 revs/min of the speed of mainshaft;
(2)The raw material mixed is put into the loading hopper of double screw extruder, wherein each heating region temperature of double screw extruder Setting is respectively:One area:100 ℃;2nd area:220 ℃;3rd area:220 ℃;4th area:220 ℃;Head:220 ℃;Raw material exists 2 min of residence time in extruder, pressure are 5 MPa;It through melting extrusion, is granulated, it is transparent multiple to obtain graphene/thermoplastic Condensation material.
Comparative example 2
A kind of graphene/thermoplastic transparent composite, is counted, including the following raw material component in parts by weight:
Polyethylene terephthalate -97.5 parts of 1,4 cyclohexane dimethanol ester;
0.3 part of graphene (ug-SGraphene-02, Suzhou You Gao nano materials Co., Ltd, thickness 0.7-1.2nm);
Compatilizer(Lined polymethyl ethylene carbonate graft glycidyl methacrylate)2 parts;
Antioxidant(Triethylene-glycol is bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester])0.2 part.
A kind of above-mentioned graphene/thermoplastic transparent composite is prepared, is specifically comprised the following steps:
(1)Polyethylene terephthalate -97.5 parts of 1,4 cyclohexane dimethanol ester, graphene are weighed in parts by weight (Ug-SGraphene-02, Suzhou You Gao nano materials Co., Ltd, thickness 0.7-1.2nm)0.3 part, the poly- methyl second of compatilizer Support 2 parts of carbonic ester graft glycidyl methacrylate and the bis- [β-(3- tertiary butyl -4- hydroxyls of antioxidant triethylene-glycol Base -5- aminomethyl phenyls) propionic ester] 0.2 part, put into dry-mixed 5 min, the speed of mainshaft 300 in SHR series of high speed mixers Rev/min;
(2)The raw material mixed is put into the loading hopper of double screw extruder, wherein each heating region temperature of double screw extruder Setting is respectively:One area:130℃;2nd area:250℃;3rd area:240℃;4th area:240℃;Head:235℃;Raw material is squeezing out 4 min of residence time in machine, pressure are 9 MPa.It through melting extrusion, is granulated, obtains the transparent composite wood of graphene/thermoplastic Material.
Performance test:
Tensile strength is tested by 1040 standards of GB/T.Specimen types are I types, batten size(mm):170(It is long)×(20± 0.2)(End portion width)× ( 4±0.2 )(Thickness), tensile speed is 50 mm/min.
Bending modulus is tested by 9341 standards of GB/T.Specimen types are specimen size(mm):(80±2)×(10± 0.2)× (4 ± 0.2), rate of bending are 20 mm/min.
Light transmittance is detected by 2410 standards of GB/T.
Martin Heat Resistant Temperature is detected by 1035 standards of GB/T.Specimen size(mm):(120±1)×(15±0.2) × (10 ± 0.2), constant heatingrate's rate are:50±3℃/h.
The formula and material properties test result of 1 ~ 3 graphene of embodiment/thermoplastic transparent composite such as 1 institute of table Show.
11 ~ 3 graphene of embodiment of table/thermoplastic transparent composite formula and material properties test result
Embodiment 1 Embodiment 2 Embodiment 3
Lined polymethyl ethylene carbonate 95 6
Polyethylene terephthalate -1,4 cyclohexane dimethanol ester 97.5 90
Graphene 0.5 0.3 0.1
Lined polymethyl ethylene carbonate is grafted oxazoline 4 2
Lined polymethyl ethylene carbonate graft glycidyl methacrylate 2 1.5
Triethylene-glycol is bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester] 0.5 0.2 0.4
Tensile strength(MPa) 68 79 73
Bending modulus(MPa) 5742 6310 6150
Light transmittance(%) 93.6 96 95
Martin Heat Resistant Temperature(℃) 94 100.6 98.5
The results are shown in Table 2 for the formula and material properties test of 1 ~ 2 graphene of comparative example/thermoplastic transparent composite.
21 ~ 2 graphene of comparative example of table/thermoplastic transparent composite formula and material properties test result
Comparative example 1 Comparative example 2
Lined polymethyl ethylene carbonate 95
Polyethylene terephthalate -1,4 cyclohexane dimethanol ester 97.5
Graphene 0.5 0.3
Lined polymethyl ethylene carbonate is grafted oxazoline 4
Lined polymethyl ethylene carbonate graft glycidyl methacrylate 2
Triethylene-glycol is bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester] 0.5 0.2
Tensile strength(MPa) 55 70
Bending modulus(MPa) 5026 5606
Light transmittance(%) 90.1 91.8
Martin Heat Resistant Temperature(℃) 86 92.4
It can be seen from Tables 1 and 2 the graphene of embodiment 1 ~ 3/thermoplastic transparent composite system be have it is high-strength Degree, high rigidity, high transparency, high heat-resisting composite system, properties are superior to graphene/thermoplasticity of comparative example 1 ~ 2 Plastic composite.
Above example is merely preferred embodiments of the present invention, but protection scope of the present invention is not limited to This, any one skilled in the art the variation that can readily occur in or replaces in the technical scope that discloses of the present invention It changes, should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claim Subject to enclosing.

Claims (10)

1. a kind of graphene/thermoplastic transparent composite, which is characterized in that count in parts by weight, including the following raw material Component:
95~97.5 parts of thermoplastic;
0.1~0.5 part of graphene;
2~4 parts of compatilizer;
0.2~0.5 part of antioxidant.
2. a kind of graphene/thermoplastic transparent composite according to claim 1, which is characterized in that the heat Thermoplastic plastic includes one kind in polyethylene terephthalate -1,4 cyclohexane dimethanol ester and lined polymethyl ethylene carbonate More than.
3. a kind of graphene/thermoplastic transparent composite according to claim 1, which is characterized in that the phase It is that lined polymethyl ethylene carbonate is grafted in oxazoline and lined polymethyl ethylene carbonate graft glycidyl methacrylate to hold agent More than one.
4. a kind of graphene/thermoplastic transparent composite according to claim 1, which is characterized in that described anti- Oxygen agent includes that triethylene-glycol is bis- [β-(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyls) propionic ester].
5. a kind of graphene/thermoplastic transparent composite according to claim 1, which is characterized in that the stone Black alkene is prepared via a method which to obtain:
It is passed through ethane gas into reaction kettle, the air in reaction kettle is discharged;Graphite powder and barrier are added in reaction kettle again, It is passed through ethane gas and propane gas, while being that 2 DEG C/min~5 DEG C/min is warming up to 100~120 DEG C, and makes with heating rate Air pressure reaches 5~7MPa in kettle, and after keeping the temperature 30~50 minutes, slow release pressure to atmospheric pressure obtains graphene.
6. a kind of graphene/thermoplastic transparent composite according to claim 5, which is characterized in that the resistance It is one or more of palmitin acid butyl ester and octyl palmitate every agent, the mass ratio of barrier and graphite powder is 1:100~2:100.
7. a kind of graphene/thermoplastic transparent composite according to claim 5, which is characterized in that be passed through second After alkane gas and propane gas, in reaction kettle, the molar ratio of ethane and propane is 1:1~3:1, the gross mass of ethane and propane with The mass ratio of graphite powder is 3:10~8:10.
8. the method for preparing a kind of graphene of claim 1 ~ 7 any one of them/thermoplastic transparent composite, special Sign is, includes the following steps:
Each raw material put by the parts by weight dry-mixed in super mixer, then the raw material mixed is put into twin-screw The loading hopper of extruder through melting extrusion, is granulated, obtains the graphene/thermoplastic transparent composite.
9. preparation method according to claim 8, which is characterized in that the dry-mixed time is 4~7min;Double spiral shells The heating region of bar extruder is set as:One area's temperature is 100~130 DEG C, and two area's temperature are 220~250 DEG C, and three area's temperature are 220~240 DEG C, four area's temperature are 220~240 DEG C, and head temperature is 220~235 DEG C.
10. preparation method according to claim 8, which is characterized in that residence time 2 of the raw material in twin-screw extrusion~ 5 min, pressure are 5~9 MPa.
CN201810146814.4A 2018-02-12 2018-02-12 A kind of graphene/thermoplastic transparent composite and preparation method thereof Pending CN108285630A (en)

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Application publication date: 20180717