CN105820496B - A kind of graphene/glass fiber reinforced ABS composite material and preparation method thereof - Google Patents
A kind of graphene/glass fiber reinforced ABS composite material and preparation method thereof Download PDFInfo
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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
- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
- C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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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
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
A kind of graphene/glass fiber reinforced ABS composite material, described graphene/glass fiber reinforced ABS composite material, include the components of following components parts by weight：The mass parts of ABS60 90, the mass parts of epoxy resin 5 20, the mass parts of graphene 0.01 5, the mass parts of glass fibre 16, the mass parts of silane coupler 0.01 0.1, the mass parts of ethanol 12, the mass parts of antioxidant 0.05 2, the mass parts of compatible toughening agents 0.5 3.The invention also discloses the preparation method of above-mentioned graphene/glass fiber reinforced ABS composite material.Graphene/glass fiber reinforced ABS composite material prepared by the present invention, not only preparation technology is simple, and experimental result shows that heat endurance, intensity and the toughness of prepared graphene/glass fiber reinforced ABS composite material are obviously improved, and floating fine phenomenon has been effectively eliminated, thus the practical application of ABS composite material can be expanded.
Description
Technical field
The present invention relates to polymeric material field, more particularly to a kind of graphene/glass fiber reinforced ABS composite material and
Its preparation method.
Background technology
ABS（Acrylonitrile butadiene styrene terpolymer）It is a kind of novel universal of exploitation the 1940s
Thermoplastic engineering plastic, be it is a kind of using polybutadiene chain as skeleton styrene and acrylonitrile graft copolymer and styrene,
The copolymer blended multiphase polymer formed of acrylonitrile.ABS has good combination property：Resistant to chemical etching, processing fluidity
And higher case hardness, heat resistance, toughness, impact property and rigidity, have been widely used in make various machines at present
Tool, the parts of instrument and equipment and electrical equipment, the shell of instrument.But molding shrinkage larger ABS, relatively low thermal deformation temperature
Degree and relatively low bending strength, processing and rear assembling to product bring certain difficulty.Glass fibre reinforced composite material be with
Polymer is matrix, using glass as reinforcing material manufactured composite, combine the performance of polymer and glass.Study table
It is bright that fibrous material is added in ABS, can greatly reinforcing material intensity and shrinkage factor, and improve the heat resistance of material.
Rubber and plastic industry has carried out in the industry the research work related to ABS/ graphene nanocomposite materials high performance.In
State's number of patent application 201510446241.3, a kind of graphene-ABS composite flame-proof plastics and preparation method thereof are disclosed, are being improved
ABS other performances are not influenceed while fire resistance.A kind of X of Chinese Patent Application No. 201510589095., there is provided LED
With filling-modified PA6/ABS composite heat-conducting plastics of nano-silicon nitride-graphene and preparation method thereof, the heat-conducting plastic is by PA6
It is used in mixed way with ABS, composite shows excellent in terms of plasticity, durability, electric insulating quality；Chinese patent
201410456105.8, and in particular to a kind of method that body in-situ polymerization prepares graphene/ABS composite material.The method is by rubber
Peptization solution in a solvent, adds styrene, acrylonitrile monomer, graphene, carries out polymerisation in bulk, it is compound to obtain graphene/ABS
Material；A kind of Chinese patent 201410456117. 0, there is provided method of in-situ modified ABS resin.This method is in emulsion graft polymerization
Graphene is introduced during SAN blending methods, can be in larger model by changing the addition and addition manner of graphene
Interior heat conduction, conduction and the mechanical property for adjusting composite is enclosed so as to obtain the composite of excellent performance.
It is comprehensive that correlative study shows that the addition of graphene makes ABS composite material possess excellent mechanics, calorifics, electricity etc.
Can, but in method made above, graphene incorporation matrix is directly unfavorable for dispersiveness of the graphene in ABS matrixes and phase
Capacitive；And composite is prepared by the methods of graphene in-situ polymerization, coupling modifier, technique is cumbersome in actual production, stone
The form and performance change of black alkene are difficult to control.The graphene of structural integrity is made up of phenyl ring, and chemical stability is high, and surface is in lazy
Property, acted on other media weak；And graphene film interlayer has stronger Van der Waals force, easily reunites, its research application is greatly limited；
How using high-efficient simple, the method for application easy to implement realizes fine dispersion of the graphene in ABS material, be to prepare high property
The key of energy ABS/ graphene nanocomposite materials.Epoxy resin is added in glass fiber reinforced ABS material, can be effective
Elimination float fine phenomenon, and by selecting raw material and control preparation condition, graphene can be realized good in the epoxy
Dispersiveness.Therefore dispersiveness of the present invention first with epoxy resin to graphene, is made graphene dispersing solution, then by graphite
Alkene-epoxy resin is added to ABS composite material, obtains a kind of novel graphite alkene/glass fiber reinforced ABS composite material.
The content of the invention
, should it is an object of the invention to provide a kind of graphene/glass fiber reinforced ABS composite material and preparation method thereof
Material possesses that graphene addition is low, good mechanical property, processing characteristics and heat endurance.Eliminating glass fiber reinforcement
While the floating fine phenomenon of ABS composite material, graphene in the composite dispersed is realized.
To reach above-mentioned purpose, composite provided by the invention includes the component of following parts by weight：60-90 mass parts
The epoxy resin of ABS, 5-20 mass parts, the graphene of 0.01-5 mass parts, glass fibre, the 0.01-0.1 of 1-6 mass parts
The compatible increasing of the silane coupler of mass parts, the ethanol of 1-2 mass parts, the antioxidant of 0.05-2 mass parts, 0.5-3 mass parts
Tough dose.
The ABS is the copolymer of acrylonitrile, butadiene and styrene, and the wherein percentage composition of butadiene unit is 10-
40 wt%；The epoxy resin is propane type epoxy resin of di phenolic group, glycidyl ester epoxy resin, glycidol amine ring
At least one of oxygen tree fat and cycloaliphatic epoxy resin；Described glass fibre is alkali-free short glass fiber, length 3-
Silane coupler described in 12mm is 3- aminopropyl triethoxysilanes, vinyl three（'beta '-methoxy ethyoxyl）Silane and ethene
At least one of base trimethoxy silane；The antioxidant is selected from pentaerythritol ester, phosphite ester, the positive octadecanol ester of propionic acid
In one or several kinds；The compatible toughening agents are selected from silicone powder, modified ethylene bis-fatty acid amides, methyl methacrylate
Ester-SB.
The graphene has following performance parameter：Piece footpath is 5-500 microns, absorptance 3%-5%, used in the present invention
Graphene is usually the graphene with single or multiple lift structure, and preferably piece footpath is 10-50 microns, and thickness is 1-5 nanometers, compares table
Area is 20m-800m2/ g single-layer graphene, single-layer graphene specific surface area is bigger, and the hot property enhancing of product becomes apparent from,
Therefore preferably.
Heretofore described graphene/glass fiber reinforced ABS composite material, the graphite of 0.01-5 parts is added in proportion
Alkene, preferably 0.1-2 parts.When content is too low, the enhancing effect that graphene plays is limited；When it is too high, composite
It is middle to realize that the dispersed of graphene be relatively difficult, significantly improve material processing technique requirement, therefore preferably above-mentioned model
Enclose.
The preparation method of heretofore described graphene/glass fiber reinforced ABS composite material, comprises the following steps：
（1）Weigh 60-90 parts drying ABS, antioxidant 0.05-2 parts, compatible toughening agents 0.5-3 parts, be well mixed；
（2）The graphene of 0.01-5 mass parts is added in the epoxy resin of 5-20 mass parts, low speed stirs at normal temperatures
Mix assisting ultrasonic and disperse 0.5-3h, graphene dispersing solution is made；
（3）0.01-0.1 mass parts silane couplers are dissolved in 1-2 mass parts absolute ethyl alcohols, are configured to silane coupled
Agent-ethanol solution, using spray-on process by spray solution on 1-6 part glass fibres, be then placed in baking oven dry 50-80min,
90-110 DEG C of drying temperature；
（4）By step（1）Middle compound is sent into double screw extruder through upstream spout；By step（2）Middle graphene point
Dispersion liquid is sent into double screw extruder melting and squeezed through fed downstream mouth；By step（3）Glass fibre after middle processing through gas outlet,
It is sent into double screw extruder.Three of the above material adds speed using variable pump control, realizes the purpose being uniformly added into；
（5）Described double screw extruder is with vacuumizing and temperature control device, composite use extruder melting extrusion
It is granulated, is 190-210 DEG C respectively from spout to extrusion die temperature, 210-240 DEG C, 230-250 DEG C, 240-260 DEG C, 250-
270 DEG C, the machine screw speed 400-1000r/min of extruder, charging rotating speed 30-60r/min.Product is made in cooling, pelletizing.
The invention has the advantages that：Graphene/glass fiber reinforced ABS composite material prepared by the present invention,
Not only preparation technology is simple, and experimental result shows that the impact strength, heat resistance, stretching of prepared ABS composite material are strong
The performances such as degree, molding shrinkage are obviously improved, thus can expand the practical ranges of ABS composite material.
Brief description of the drawings：
Fig. 1 is the microscopic appearance figure of comparative example 4 in the present invention.
Fig. 2 is the microscopic appearance figure of embodiment 3 in the present invention.
Embodiment
Embodiments of the invention are given below, the present invention is specifically described by embodiment.Be necessary it is pointed out here that
, embodiment is simply to further instruction of the present invention, it is impossible to is interpreted as limitation of the scope of the invention, the technology in the field
Personnel can make some adjustment to present disclosure.
A kind of preparation process of graphene/glass fiber reinforced ABS composite material comprises the following steps：（1）Weigh drying
ABS, antioxidant, compatible toughening agents, be well mixed；（2）Graphene is added in glycidyl amine epoxy resin,
Stirring at low speed assisting ultrasonic disperses 2h under normal temperature, and graphene dispersing solution is made；（3）Silane coupler is dissolved in absolute ethyl alcohol
In, be configured to silane coupler-ethanol solution, using spray-on process by spray solution on the glass fibers, be then placed in baking oven
Dry 50-80min, 90-110 DEG C of drying temperature；（4）By step（1）Middle compound is sent into twin-screw extrusion through upstream spout
Machine.By step（2）Middle graphene dispersing solution is sent into double screw extruder melting and squeezed through fed downstream mouth.By step（3）Middle processing
Glass fibre afterwards is sent into double screw extruder through gas outlet.Three of the above material adds speed using variable pump control, realizes
The purpose being uniformly added into；（5）Described double screw extruder is with vacuumizing and temperature control device, composite are melted using extruder
Melt extruding pelletization, be 190-210 DEG C respectively from spout to extrusion die temperature, 210-240 DEG C, 230-250 DEG C, 240-260
DEG C, 250-270 DEG C, the machine screw speed 400-1000r/min of extruder, charging rotating speed 30-60r/min.Cooling, pelletizing are made
Product.
The mass fraction of each component is shown in Table 1 in embodiment and comparative example：
The ratio of the composite each component of table 1.
Sampling material is molded into standard batten after being dried 4 hours in 90 DEG C, carries out performance test, and performance data is shown in Table 2：
The performance test of the composite of table 2.
In embodiments of the invention, tensile strength is tested according to national standard GB/T1040.2-2006；It is bending strength, curved
Bent modulus is tested according to national standard GB/T9341-2000；Izod notched impact strength is according to national standard GB/T1843.2-1996
Tested；Heat distortion temperature is tested according to national standard GB/T1634.2-2004；Molding shrinkage presses national standard GB/
T17037.4-2003 is tested.
It can see from table 2, the compound system formed with graphene and glass fibre, the impact to ABS composite material
The performances such as intensity, heat resistance, tensile strength, molding shrinkage all make moderate progress.
Also, shown by microscopic appearance test, the ABS composite material for the epoxy resin not added（Comparative example 4）Occur
Surface floating fiber phenomenon（Referring to Fig. 1）；After epoxy resin is added, embodiment 1-4 surface does not occur the phenomenon for floating fibre（Referring to
Fig. 2）.The impact strength of products obtained therefrom is relatively not added with the impact strength height of products obtained therefrom after addition graphene-epoxy resin,
Show that graphene-epoxy resin plays stronger compatibility in the composite, glass fibre is organically combined with ABS material
Together, while improving the surface floating fiber phenomenon that fibrous composite easily occurs, the intensity of composite is also improved.
Claims (10)
1. a kind of graphene/glass fiber reinforced ABS composite material, it is characterised in that including following components：60-90 mass parts
The epoxy resin of ABS, 5-20 mass parts, the graphene of 0.01-5 mass parts, glass fibre, the 0.01-0.1 of 1-6 mass parts
The silane coupler of mass parts, the absolute ethyl alcohol of 1-2 mass parts, the antioxidant of 0.05-2 mass parts, the phase of 0.5-3 mass parts
Hold toughener；The method that the graphene/glass fiber reinforced ABS composite material comprises the following steps is made：
（1）The antioxidant for ABS, 0.05-2 mass parts that 60-90 mass parts are dried and the compatible toughening agents of 0.5-3 mass parts
It is well mixed；
（2）The graphene of 0.01-5 mass parts is added in the epoxy resin of 5-20 mass parts, stirring at low speed is auxiliary at normal temperatures
Ultrasonic disperse 0.5-3h is helped, graphene dispersing solution is made；
（3）0.01-0.1 mass parts silane couplers are dissolved in 1-2 mass parts absolute ethyl alcohols, be configured to silane coupler-
Ethanol solution, silane coupler-ethanol solution is sprayed on 1-6 mass parts glass fibres using spray-on process, is then placed in baking
50-80min, 90-110 DEG C of drying temperature are dried in case；
（4）By step（1）Middle compound is sent into double screw extruder through upstream spout；By step（2）Middle graphene dispersing solution
Through fed downstream mouth, double screw extruder melting extrusion is sent into；By step（3）Glass fibre after middle processing is sent through gas outlet
Enter double screw extruder；Three of the above material adds speed using variable pump control, realizes the purpose being uniformly added into；
（5）Described double screw extruder with vacuumizing and temperature control device, composite using extruder melting extrusion granulation,
It is 190-210 DEG C respectively from spout to extrusion die temperature, 210-240 DEG C, 230-250 DEG C, 240-260 DEG C, 250-270
DEG C, the machine screw speed 400-1000r/min of extruder, charging rotating speed 30-60r/min；Product is made in cooling, pelletizing.
2. graphene/glass fiber reinforced ABS composite material according to claim 1, it is characterised in that the ABS is
It is the copolymer of acrylonitrile, butadiene and styrene, wherein the percentage composition of butadiene unit is 10-40 wt%.
3. graphene/glass fiber reinforced ABS composite material according to claim 1, it is characterised in that the asphalt mixtures modified by epoxy resin
Fat is propane type epoxy resin of di phenolic group, glycidyl ester epoxy resin, glycidyl amine epoxy resin and aliphatic ring
At least one of oxygen tree fat.
4. according to graphene/glass fiber reinforced ABS composite material described in claim 1,2 or 3, it is characterised in that described
Graphene has following performance parameter：Piece footpath is 5-500 microns, absorptance 3%-5%.
5. graphene/glass fiber reinforced ABS composite material according to claim 4, it is characterised in that the graphene
It is 10-50 microns for piece footpath, thickness 1-5nm, specific surface area 20m2 -800m2/ g single-layer graphene.
6. graphene/glass fiber reinforced ABS composite material according to claim 1, it is characterised in that：Described glass
Fiber is alkali-free short glass fiber, length 3-12mm.
7. graphene/glass fiber reinforced ABS composite material according to claim 1, it is characterised in that：Described silane
Coupling agent is 3- aminopropyl triethoxysilanes, vinyl three（'beta '-methoxy ethyoxyl）Silane and vinyltrimethoxy silane
At least one.
8. graphene/glass fiber reinforced ABS composite material according to claim 1, it is characterised in that described anti-oxidant
One or several kinds of the agent in pentaerythritol ester, phosphite ester, the positive octadecanol ester of propionic acid.
9. graphene/glass fiber reinforced ABS composite material according to claim 1, it is characterised in that the compatible increasing
Tough dose in silicone powder, modified ethylene bis-fatty acid amides, copolymer of methyl methacrylate-styrene-butadiene one
Kind is several.
10. a kind of preparation method of graphene/glass fiber reinforced ABS composite material described in claim any one of 1-9, its
It is characterised by, comprises the following steps：
（1）The antioxidant for ABS, 0.05-2 mass parts that 60-90 mass parts are dried and the compatible toughening agents of 0.5-3 mass parts
It is well mixed；
（2）The graphene of 0.01-5 mass parts is added in the epoxy resin of 5-20 mass parts, stirring at low speed is auxiliary at normal temperatures
Ultrasonic disperse 0.5-3h is helped, graphene dispersing solution is made；
（3）0.01-0.1 mass parts silane couplers are dissolved in 1-2 mass parts absolute ethyl alcohols, be configured to silane coupler-
Ethanol solution, silane coupler-ethanol solution is sprayed on 1-6 mass parts glass fibres using spray-on process, is then placed in baking
50-80min, 90-110 DEG C of drying temperature are dried in case；
（4）By step（1）Middle compound is sent into double screw extruder through upstream spout；By step（2）Middle graphene dispersing solution
Through fed downstream mouth, double screw extruder melting extrusion is sent into；By step（3）Glass fibre after middle processing is sent through gas outlet
Enter double screw extruder；Three of the above material adds speed using variable pump control, realizes the purpose being uniformly added into；
（5）Described double screw extruder with vacuumizing and temperature control device, composite using extruder melting extrusion granulation,
It is 190-210 DEG C respectively from spout to extrusion die temperature, 210-240 DEG C, 230-250 DEG C, 240-260 DEG C, 250-270
DEG C, the machine screw speed 400-1000r/min of extruder, charging rotating speed 30-60r/min；Product is made in cooling, pelletizing.
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