CN105778464A - Graphene/glass fibre reinforced polycarbonate composite material and preparation method thereof - Google Patents
Graphene/glass fibre reinforced polycarbonate composite material and preparation method thereof Download PDFInfo
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- CN105778464A CN105778464A CN201610315601.0A CN201610315601A CN105778464A CN 105778464 A CN105778464 A CN 105778464A CN 201610315601 A CN201610315601 A CN 201610315601A CN 105778464 A CN105778464 A CN 105778464A
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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
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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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
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- 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
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Abstract
The invention provides a graphene/glass fibre reinforced polycarbonate composite material which is prepared from the following ingredients in parts by weight: 60-90 parts of polycarbonate, 5-20 parts of epoxy resin, 0.01-5 parts of graphene, 5-20 parts of glass fibre, 0.1-1 part of a silane coupling agent, 5-10 parts of ethanol, 0.05-2 parts of an antioxidant and 0.5-3 parts of a compatible flexibilizer. The invention also discloses a preparation method of the graphene/glass fibre reinforced polycarbonate composite material. The graphene/glass fibre reinforced polycarbonate composite material prepared by the method not only is simple in preparation process, but also is obviously improved in thermal stability, strength and toughness according to experimental results, a glass fiber revealed phenomenon is effectively eliminated, and the actual application of a polycarbonate composite material is expanded.
Description
Technical field
The present invention relates to polymeric material field, particularly to a kind of Graphene/glass fiber reinforced polycarbonate composite and preparation method thereof.
Background technology
Merlon is the polymer of bisphenol-A, belongs to thermoplastic resin, is widely used as engineering plastic materials, shows impact resistance, electrical property and the moldability of excellence, keeps physical property, and have self-extinguishment within the scope of wider temperature.The shortcoming yet with Merlon with bad processing characteristics, is accordingly difficult to be used in Merlon in the shell of little and more complicated electric, the electronic product of size.In order to solve this problem, industrial employing, by the method for Merlon Yu the resin alloy of other kind, keeps high impact while improving drawing abillity.Glass fibre reinforced composite material is with polymer as matrix, the composite made with glass as reinforcing material, combines the performance of polymer and glass.Research shows to add fibrous material in Merlon, can the greatly intensity of reinforcing material and shrinkage factor, and improve the thermostability of material.
Rubber and plastic industry has carried out the research work relevant to Merlon/graphene nanocomposite material high performance the most.Chinese patent 201280029564.7, this invention is characterised by that provided composite comprises the component such as Merlon, graphene film, has obtained forming the formed body polycarbonate compositions that anti-flammability, rigidity, resistance to impact, electric conductivity, shaping outward appearance and heat conductivity etc. are excellent；Chinese patent 201410041139.0, it is provided that a kind of Graphene modified high-strength degree, high heat conductive polycarbonate master batch and preparation method thereof, prepared composite not only heat conductivility is greatly improved, and its mechanical property also has certain amplitude to promote simultaneously；Chinese patent 201410837169.2, discloses a kind of Graphene/Merlon heat-conductive composite material and preparation method thereof, and wherein the addition of Graphene is 5-20 mass parts；Chinese patent 201110008919.1, by by fibrous heat filling and high heat filling Graphene mix homogeneously pelletize after dispersion with thermoplastic poly carbonic ether, form high-heat-conductive composite material pellet, heat filling consumption is few, mechanical property good.
Correlational study shows that the addition of Graphene makes polycarbonate composite material possess the combination properties such as excellent mechanics, calorifics, electricity, but in method made above, directly Graphene is mixed matrix and is unfavorable for Graphene dispersibility in polycarbonate matrix and the compatibility；And prepare composite by methods such as Graphene in-situ polymerization, coupling modifier, in actual production, technique is loaded down with trivial details, and the form of Graphene and performance change are difficult to control.The Graphene of structural integrity is made up of phenyl ring, and chemical stability is high, and surface is inert, weak with other medium effect；And graphene film interlayer exists stronger Van der Waals force, easily reunite, greatly limit its research application；How to use high-efficient simple, the method for application easy to implement to realize Graphene fine dispersion in makrolon material, be the key preparing high performance polycarbonate/graphene nanocomposite material.Epoxy resin is added in glass fiber reinforced polycarbonate material, floating fine phenomenon can be effectively eliminated, and by selecting raw material and controlling preparation condition, Graphene is capable of good dispersibility in the epoxy, therefore the present invention is first with the epoxy resin dispersibility to Graphene, prepare graphene dispersing solution, then add Graphene-epoxy resin to polycarbonate composite material, obtain a kind of novel graphite alkene/glass fiber reinforced polycarbonate composite.
Summary of the invention
It is an object of the invention to provide a kind of Graphene/glass fiber reinforced polycarbonate composite and preparation method thereof, it is low that this material has possessed Graphene addition, good mechanical property, processing characteristics and heat stability.While eliminating the floating fine phenomenon of glass fiber reinforced polycarbonate composite, it is achieved that Graphene in the composite dispersed.
For reaching above-mentioned purpose, the composite that the present invention provides includes the component of following parts by weight: Merlon 60-90 mass parts, epoxy resin 5-20 mass parts, Graphene 0.01-5 mass parts, glass fibre 5-20 mass parts, silane coupler 0.1-1 mass parts, ethanol 5-10 mass parts, antioxidant 0.05-2 mass parts, compatible toughening agents 0.5-3 mass parts.
Described polycarbonate is that intrinsic viscosity is at 45-55ml/g aromatic copolycarbonate, suitable aromatic copolycarbonate has to be made up by methods such as interfacial polymerizations of at least one divalent phenol and a kind of carbonate precursor, carbonate precursor can be carbonylic halide, halocarbonate or formic acid esters, preferably bisphenol A polycarbonate, intrinsic viscosity 48ml/g；Described epoxy resin is at least one in propane type epoxy resin of di phenolic group, glycidyl ester epoxy resin, glycidyl amine epoxy resin and cycloaliphatic epoxy resin；Described glass fibre is alkali-free short glass fiber, and the silane coupler described in a length of 3-12mm is 3-aminopropyl triethoxysilane, at least one of vinyl three ('beta '-methoxy ethyoxyl) silane and vinyltrimethoxy silane；Described antioxidant is selected from one or several in pentaerythritol ester, phosphite ester, propanoic acid positive octadecanol ester；Described compatible toughening agents is selected from silicone powder, modified ethylene bis-fatty acid amides, copolymer of methyl methacrylate-styrene-butadiene.
Described Graphene has following performance parameter: sheet footpath is 5-500 micron, absorptance is 3%-5%, and it is 10-50 micron that the Graphene used by the present invention usually has the Graphene of single or multiple lift structure, preferably sheet footpath, thickness is 1-5 nanometer, and specific surface area is 20m-800m2The single-layer graphene of/g, single-layer graphene specific surface area is bigger, and the hot property enhancing of goods becomes apparent from, the most preferably.
Heretofore described Graphene/glass fiber reinforced polycarbonate composite, adds the Graphene of 0.01-5 part, preferably 0.1-2 part in proportion.When content is the lowest, the reinforced effects that Graphene plays is limited；When it is too high, the dispersed meeting realizing Graphene in composite is relatively difficult, significantly improves material processing technique requirement, the most preferred above-mentioned scope.
The preparation method of heretofore described Graphene/glass fiber reinforced polycarbonate composite, comprises the following steps:
(1) Merlon that 60-90 part is dried, antioxidant 0.05-2 part, compatible toughening agents 0.5-3 part, mix homogeneously are weighed；
(2) Graphene of 0.01-5 mass parts is joined in the epoxy resin of 5-20 mass parts, the 0.5-3h of stirring at low speed assisting ultrasonic dispersion at normal temperatures, prepare graphene dispersing solution；
(3) 0.1-1 mass parts silane coupler is dissolved in 5-10 mass parts dehydrated alcohol, it is configured to silane coupler-ethanol solution, utilize nebulization by spray solution on 5-20 part glass fibre, be then placed in baking oven being dried 50-80min, baking temperature 90-110 DEG C；
(4) by compound in step (1) through upstream spout, double screw extruder is sent into；By graphene dispersing solution in step (2) through fed downstream mouth, send into double screw extruder melted crowded；Glass fibre after processing in step (3), through gas outlet, sends into double screw extruder.Three of the above material utilizes variable pump to control to add speed, it is achieved the purpose being uniformly added into；
(5) double screw extruder described in is with evacuation and attemperating unit, composite uses extruder to melt extrude pelletize, it is 180-200 DEG C from spout respectively to extrusion die temperature, 200-230 DEG C, 220-240 DEG C, 230-250 DEG C, 240-260 DEG C, the machine screw speed 500-800r/min of extruder, feed rotating speed 40-70r/min.Cooling, pelletizing prepares product.
The method have the advantages that the Graphene prepared by the present invention/glass fiber reinforced polycarbonate composite, not only preparation technology is simple, and experimental result show prepared by the impact strength of polycarbonate composite material, thermostability, hot strength, the performance such as molding shrinkage be obviously improved, thus can expand the practical ranges of polycarbonate composite material.
Accompanying drawing illustrates:
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.
Detailed description of the invention
Embodiments of the invention are given below, by embodiment, the present invention are specifically described.Be necessary it is pointed out here that, embodiment be to further instruction of the present invention, it is impossible to be interpreted as limitation of the scope of the invention, person skilled in art present disclosure can be made some adjust.
The preparation process of a kind of Graphene/glass fiber reinforced polycarbonate composite comprises the following steps: (1) weighs dry Merlon (bisphenol A polycarbonate, intrinsic viscosity 48ml/g), antioxidant, compatible toughening agents, mix homogeneously；(2) Graphene is joined in glycidyl amine epoxy resin, the 2h of stirring at low speed assisting ultrasonic dispersion at normal temperatures, prepare graphene dispersing solution；(3) silane coupler is dissolved in dehydrated alcohol, is configured to silane coupler-ethanol solution, utilize nebulization by spray solution on the glass fibers, be then placed in baking oven being dried 50-80min, baking temperature 90-110 DEG C；(4) by compound in step (1) through upstream spout, double screw extruder is sent into.By graphene dispersing solution in step (2) through fed downstream mouth, send into double screw extruder melted crowded.Glass fibre after processing in step (3), through gas outlet, sends into double screw extruder.Three of the above material utilizes variable pump to control to add speed, it is achieved the purpose being uniformly added into；(5) double screw extruder described in is with evacuation and attemperating unit, composite uses extruder to melt extrude pelletize, it is 180-200 DEG C from spout respectively to extrusion die temperature, 200-230 DEG C, 220-240 DEG C, 230-250 DEG C, 240-260 DEG C, the machine screw speed 500-800r/min of extruder, feed rotating speed 40-70r/min.Cooling, pelletizing prepares product.
In embodiment and comparative example, the mass fraction of each component is shown in Table 1:
Table
1.
The ratio of each component of composite
Sampling material is dried after 4 hours in 95 DEG C and is molded into standard batten, carries out performance test, and performance data is shown in Table 2:
Table
2.
The performance test of composite
In embodiments of the invention, hot strength is tested according to GB GB/T1040.2-2006；Bending strength, bending modulus are tested according to GB GB/T9341-2000；Izod notched impact strength is tested according to GB GB/T1843.2-1996；Heat distortion temperature is tested according to GB GB/T1634.2-2004；Molding shrinkage is tested by GB GB/T17037.4-2003.
It will be seen that the compound system formed with Graphene and glass fibre from table 2, the performances such as the impact strength of polycarbonate composite material, thermostability, hot strength, molding shrinkage are all made moderate progress.
Further, microscopic appearance test showing, the polycarbonate composite material (comparative example 4) of the epoxy resin not added occurs in that surface floating fiber phenomenon (seeing Fig. 1)；After adding epoxy resin, all there is not floating fine phenomenon (seeing Fig. 2) in the surface of embodiment 1-4.After adding Graphene-epoxy resin, the impact strength of products obtained therefrom is the most relatively not added with the impact strength height of products obtained therefrom, show that Graphene-epoxy resin plays the stronger compatibility in the composite, glass fibre is combined with makrolon material, while improving the surface floating fiber phenomenon that fibrous composite easily occurs, also improve the intensity of composite.
Claims (10)
1. Graphene/glass fiber reinforced polycarbonate composite, it is characterized in that, including following components: the Merlon of 60-90 mass parts, the epoxy resin of 5-20 mass parts, the Graphene of 0.01-5 mass parts, the glass fibre of 5-20 mass parts, the silane coupler of 0.1-1 mass parts, the ethanol of 5-10 mass parts, the antioxidant of 0.05-2 mass parts, the compatible toughening agents of 0.5-3 mass parts.
Graphene the most according to claim 1/glass fiber reinforced polycarbonate composite, it is characterized in that, described Merlon is that intrinsic viscosity is at 45-55ml/g aromatic copolycarbonate, suitable aromatic copolycarbonate has to be made up by methods such as interfacial polymerizations of at least one divalent phenol and a kind of carbonate precursor, and carbonate precursor can be carbonylic halide, halocarbonate or formic acid esters.
Graphene the most according to claim 1/glass fiber reinforced polycarbonate composite, it is characterised in that described Merlon is bisphenol A polycarbonate, intrinsic viscosity 48ml/g.
Graphene the most according to claim 1/glass fiber reinforced polycarbonate composite, it is characterised in that: described epoxy resin is at least one in propane type epoxy resin of di phenolic group, glycidyl ester epoxy resin, glycidyl amine epoxy resin and cycloaliphatic epoxy resin.
5. according to the Graphene/glass fiber reinforced polycarbonate composite described in claim 1,2 or 3, it is characterised in that described Graphene has following performance parameter: sheet footpath is 5-500 micron, and absorptance is 3%-5%；Described glass fibre is alkali-free short glass fiber, a length of 3-12mm.
Graphene the most according to claim 4/glass fiber reinforced polycarbonate composite, it is characterised in that described Graphene be sheet footpath be 10-50 micron, thickness is 1-5nm, and specific surface area is 20m-800m2The single-layer graphene of/g.
Graphene the most according to claim 1/glass fiber reinforced polycarbonate composite, it is characterized in that: described silane coupler is 3-aminopropyl triethoxysilane, at least one of vinyl three ('beta '-methoxy ethyoxyl) silane and vinyltrimethoxy silane.
Graphene the most according to claim 1/glass fiber reinforced polycarbonate composite, it is characterised in that described antioxidant is selected from one or several in pentaerythritol ester, phosphite ester, propanoic acid positive octadecanol ester.
Graphene the most according to claim 1/glass fiber reinforced polycarbonate composite, it is characterized in that, described compatible toughening agents is selected from one or several in silicone powder, modified ethylene bis-fatty acid amides, copolymer of methyl methacrylate-styrene-butadiene.
10. the preparation method of a kind of Graphene/glass fiber reinforced polycarbonate composite described in any one of claim 1-9, it is characterised in that comprise the following steps:
(1) the compatible toughening agents mix homogeneously of the Merlon, the antioxidant of 0.05-2 mass parts and the 0.5-3 mass parts that 60-90 mass parts are dried；
(2) Graphene of 0.01-5 mass parts is joined in the epoxy resin of 5-20 mass parts, the 0.5-3h of stirring at low speed assisting ultrasonic dispersion at normal temperatures, prepare graphene dispersing solution；
(3) 0.1-1 mass parts silane coupler is dissolved in 5-10 mass parts dehydrated alcohol, it is configured to silane coupler-ethanol solution, nebulization is utilized to be sprayed at by silane coupler-ethanol solution on 5-20 mass parts glass fibre, it is then placed in baking oven being dried 50-80min, baking temperature 90-110 DEG C；
(4) by compound in step (1) through upstream spout, double screw extruder is sent into；By graphene dispersing solution in step (2) through fed downstream mouth, send into double screw extruder melted crowded；Glass fibre after processing in step (3), through gas outlet, sends into double screw extruder；Three of the above material utilizes variable pump to control to add speed, it is achieved the purpose being uniformly added into；
(5) double screw extruder described in is with evacuation and attemperating unit, composite uses extruder to melt extrude pelletize, it is 180-200 DEG C from spout respectively to extrusion die temperature, 200-230 DEG C, 220-240 DEG C, 230-250 DEG C, 240-260 DEG C, the machine screw speed 500-800r/min of extruder, feed rotating speed 40-70r/min；Cooling, pelletizing prepares product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446239A (en) * | 2017-09-07 | 2017-12-08 | 南京汉尔斯生物科技有限公司 | Superpower tough graphene new material applied to satellite element and preparation method thereof |
| CN109721997A (en) * | 2018-12-28 | 2019-05-07 | 方万漂 | A kind of graphene toughening polyester material and preparation method thereof |
| CN112457548A (en) * | 2020-11-26 | 2021-03-09 | 四川六九一二科技有限公司 | Preparation method of super-wear-resistant, flame-retardant, high-strength and mould-resistant graphene composite material |
| CN113372702A (en) * | 2021-05-21 | 2021-09-10 | 大河宝利材料科技(苏州)有限公司 | Graphene composite material |
| CN113604023A (en) * | 2021-08-24 | 2021-11-05 | 中山市汇鑫打印耗材有限公司 | High-strength hard plastic scraper for printer and processing technology thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104292817A (en) * | 2014-01-08 | 2015-01-21 | 上海智高贸易有限公司 | Continuous fiber composite high thermal conductive material and processing technology thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104292817A (en) * | 2014-01-08 | 2015-01-21 | 上海智高贸易有限公司 | Continuous fiber composite high thermal conductive material and processing technology thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446239A (en) * | 2017-09-07 | 2017-12-08 | 南京汉尔斯生物科技有限公司 | Superpower tough graphene new material applied to satellite element and preparation method thereof |
| CN109721997A (en) * | 2018-12-28 | 2019-05-07 | 方万漂 | A kind of graphene toughening polyester material and preparation method thereof |
| CN112457548A (en) * | 2020-11-26 | 2021-03-09 | 四川六九一二科技有限公司 | Preparation method of super-wear-resistant, flame-retardant, high-strength and mould-resistant graphene composite material |
| CN113372702A (en) * | 2021-05-21 | 2021-09-10 | 大河宝利材料科技(苏州)有限公司 | Graphene composite material |
| CN113604023A (en) * | 2021-08-24 | 2021-11-05 | 中山市汇鑫打印耗材有限公司 | High-strength hard plastic scraper for printer and processing technology thereof |
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