CN106947233A - A kind of PC/PA6/ graphene composite materials and preparation method thereof - Google Patents
A kind of PC/PA6/ graphene composite materials and preparation method thereof Download PDFInfo
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- CN106947233A CN106947233A CN201710255904.2A CN201710255904A CN106947233A CN 106947233 A CN106947233 A CN 106947233A CN 201710255904 A CN201710255904 A CN 201710255904A CN 106947233 A CN106947233 A CN 106947233A
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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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
- C08K2201/017—Additives being an antistatic agent
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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
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/04—Antistatic
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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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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a kind of PC/PA6/ graphene composite materials and preparation method thereof, belong to modifying plastics field.PC/PA6/ graphene composite materials are made up of PC, PA6, graphene and compatilizer SMA, the composite is to carry out melt blending extrusion using graphene/PA6 nano composite materials and PC to be made, and the graphene/PA6 nano composite materials are to be obtained by modified graphene with caprolactam in-situ polymerization.Preparation-obtained power PC/PA6/ the graphene composite materials of the present invention have good toughness and intensity, there is the performances such as more excellent anti-ultraviolet ageing, anti-flammability, heat resistance, antistatic behaviour and processing characteristics simultaneously, application of the PC/PA6 composites in more high-end field has been expanded.
Description
Technical field
The invention belongs to modifying plastics field, and in particular to a kind of PC/PA6/ graphene composite materials and preparation method thereof.
Background technology
Makrolon (PC) has the erosion-resisting characteristics and creep-resistant property of protrusion, and cold-resistant, heat-resist, water absorption rate is low, system
Product dimensionally stable, but there is also processing fluidity is poor, solvent resistance is poor, easy stress cracking and notch sensitive etc. is lacked
Fall into.Nylon (PA) is a kind of engineering plastics of excellent performance, and mechanical strength is high, and fluidity of molten and oil resistivity are good, but it is rushed
Hit intensity is low, heat resistance is poor, Yin Qigao water imbibition and cause the dimensional stability of product poor, make it in some particular fields
Application under closing is restricted.As can be seen here, PC and PA materials have preferable complementarity in aspect of performance, and prepared answers
Condensation material may apply to the fields such as automobile, electronics, aircraft, office furniture, building, show extremely strong vitality.
The method for being typically prepared PC/PA6 alloys is to carry out capacity increasing modifying using bulking agent to improve performance, but the degree improved
It is limited, it still can not meet requirement of some high-end fields to power PC/PA6 alloy materials.Graphene is a kind of with two
The nano material of crystal structure is tieed up, due to its outstanding mechanical property, electric property, thermal property and unique electromagnetic property
Deng graphene shows wide application prospect in many fields, and has progressively moved towards practical application.Graphene is both most thin
Material, is also most tough material, and graphene is combined by existing many reports with high polymer, can be obviously improved the strong of material
Degree, modulus, toughness, heat resistance and ageing-resistant performance.Thus, if can be by high performance graphene nano materials application to PC/PA6
In composite, it will assign material more excellent combination property.
The content of the invention
For above shortcomings in the prior art, the invention provides a kind of PC/PA6/ graphene composite materials and
Its preparation method.
The purpose of the present invention, is achieved through the following technical solutions：A kind of PC/PA6/ graphene composite materials, it is special
Levy and be, the material is obtained after being extruded by PC with graphene/PA6 nano composite materials through melt blending, the graphene/
PA6 nano complexes materials are made up of PA6 with the single-layer graphene for being grafted with PA6, the single-layer graphene for being grafted with PA6
Lateral dimension is more than 3 microns；The ratio between the quality of graphene and PA6 gross mass are 0.1-1:100.
Further, the graphene/being made by the steps for PA6 nano composite materials obtains：
(1) by the modified graphene of 0.1-1 mass parts and 1-10 mass parts deionized water add 100 mass parts oneself in acyl
In amine melt, (300~500rpm) stirs and evenly mixs to form dispersion liquid at a high speed at 80 DEG C.The modified graphene has for surface
The single-layer graphene of the oxygen-containing functional groups such as carboxyl, hydroxyl；Carbon-to-oxygen ratio be 2.5 to 6 between；
(2) under nitrogen protection, above-mentioned dispersion liquid is warming up to 250-220 DEG C in batch condensation polymerization reactor, in 0.5-1MPa
Lower reaction 3 hours；Then react 4 hours under vacuo, obtain polymer melt；Finally granulate polymer melt is water cooled
To graphene/PA6 nano composite materials.
Further, the preparation process of power PC/PA6/ graphene composite materials is as follows：
(1) it is 50~25 by ratio of weight and the number of copies by PC, graphene/PA6 nano composite materials and compatilizer SMA:25~50:
5~10, premixed in mixer, obtain well mixed premix；
(2) with double screw extruder under conditions of 240~220 DEG C of processing temperature, 150~250rpm of rotating speed melt blending
Extrusion, is cooled down, and PC/PA6/ graphene composite materials are made in granulation.
The beneficial effects of the invention are as follows：
1st, it is combined by using graphene/PA6 nano composite materials and PC, prepares power PC/PA6/ graphenes
Composite, it is beneficial in that prepared graphene/PA6 nano composite materials, and Sheet Graphite alkene leads to caprolactam
Cross the mode effecting reaction of in-situ polymerization so that the graphene of lamella can be uniformly dispersed in PA6 matrixes, utilize ultralow graphene
Addition can just prepare High-performance graphene/PA6 nano composite material master batches, then graphene/PA6 that polymerisation is obtained
Composite master batch is mixed with PC, can properly settle the scattering problem of graphene in the composite, and then improve composite wood
Expect combination property.
2nd, graphene is added to preparation PC/PA6/ graphene composite materials in PC/PA6 composites, graphene is not only
Improve the mechanical property of composite, at the same can also assign the higher heat resistance of material, it is anti-ultraviolet ageing, anti-flammability, anti-
The combination properties such as static behaviour.
3rd, power PC/PA6/ graphene composite materials are processed by way of melt blending is extruded, this method operative employee
Skill is simple, solvent-free pollution, and production efficiency is high, is adapted to large-scale production.
Brief description of the drawings
Fig. 1 is the partial structural diagram of graphene of the present invention/PA6 nano composite materials, wherein 1 is to be grafted with PA6's
Single-layer graphene film, 2 be free PA6.
Embodiment
Present invention use situ aggregation method first prepares High-performance graphene/PA6 nanometers of ultralow graphene addition again
In condensation material, preparation process, from individual layer, lateral dimension be more than 3 μm, carbon-to-oxygen ratio be 2.5~6 between modified graphene.
By many experiments, draw to draw a conclusion：(1) graphene performance and the number of plies are closely related, and the performance of multi-layer graphene is inferior to
Single-layer graphene.(2) graphene lateral dimension influences also larger to polymer performance, and lateral dimension is too small to be unfavorable for improving compound
The mechanical property of materials, however, lateral dimension is excessive to be then significantly increased Composite Melt viscosity very much greatly, is unfavorable for shaping and adds
Work, therefore, the preferred lateral dimension of the present invention are less than 80um graphene；(3) the too low explanation graphene oxidation defect of carbon-to-oxygen ratio
Too much, graphene its own mechanical poor performance, it is limited to composite each side resultant performance enhancements.Another aspect carbon-to-oxygen ratio is too
It is low, illustrate there are a large amount of carboxyls on graphene, and carboxyl also results in polymer molecular weight decline；And opposite carbon-to-oxygen ratio is too high also can
So that graphene dispersion is poor, occurs clustering phenomena in polymeric matrix.Graphene/PA6 that the present invention is prepared receives
Nano composite material, is made up of, structure is as shown in Figure 1 free PA6 and the single-layer graphene film for being grafted with PA6.Sheet Graphite alkene
With caprolactam by way of in-situ polymerization effecting reaction so that the graphene of lamella can be uniformly dispersed in PA6 matrixes, profit
High-performance graphene/PA6 nano composite material master batches can be just prepared with ultralow graphene addition, then polymerisation is obtained
Graphene/PA6 composites master batch and PC melt blendings extrusion prepare PC/PA6/ graphene composite materials, can properly solve
The certainly scattering problem of graphene in the composite, and then more effectively improve composite material combination property.
Power PC/PA6/ graphene composite materials of the preparation of the present invention are molded using ASTM standard, and injection machine is 230
Injection moulding under the conditions of~220 DEG C, by each raw material in 110 DEG C of dry 3h processing before injection.
Measuring mechanical property method：
1st, tensile property：By GB/T1040-2006 standard testings, draw speed is 50mm/min；
2nd, bending property：By CB/T9341-2008 standard testings, rate of bending is 2mm/min；
3rd, Izod notched impact strength：By GB/T1843-2008 standard testings.
Sample shaping after temperature be 23 ± 2 DEG C, humidity for 50 ± 5% standard environment in place 88h after test, test
Environment is that temperature is 23 ± 2 DEG C, and humidity is 50 ± 5%.
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
Bright, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment belong to protection scope of the present invention.
Embodiment 1
(1) 0.1 mass parts lateral dimension is more than 3 μm of modified graphene and 1 mass parts deionized water adds 100 mass
In the caprolactam melt of part, (300rpm) stirs and evenly mixs to form dispersion liquid at a high speed at 80 DEG C.The modified graphene is table
Face has the single-layer graphene of the oxygen-containing functional groups such as carboxyl, hydroxyl；Carbon-to-oxygen ratio is 2.5；
(2) under nitrogen protection, above-mentioned dispersion liquid is warming up to 250 DEG C in batch condensation polymerization reactor, 3 is reacted under 0.6MPa
Hour；Then react 4 hours under vacuo, obtain polymer melt；The water cooled granulation of polymer melt is finally obtained into graphite
Alkene/PA6 nano composite materials.
(3) it is 25 by weight by PC, graphene/PA6 nano composite materials and SMA:25:5, premixed in mixer,
Obtain well mixed premix；
(4) with double screw extruder, melt blending is extruded under conditions of 250 DEG C of melting temperature, rotating speed 200rpm, cooling,
Granulation, is made PC/PA6/ graphene composite materials.
Composite after melt blending is molded into standard testing batten with injection machine and carries out Mechanics Performance Testing, performance
Test data is shown in Table 1.
Embodiment 2
(1) 1 mass parts lateral dimension is more than 3 μm of modified graphene and 10 mass parts deionized waters adds 100 matter
In the caprolactam melt for measuring part, (300rpm) stirs and evenly mixs to form dispersion liquid at a high speed at 80 DEG C.The modified graphene is
Surface has the single-layer graphene of the oxygen-containing functional groups such as carboxyl, hydroxyl；Carbon-to-oxygen ratio is 6；
(2) under nitrogen protection, above-mentioned dispersion liquid is warming up to 220 DEG C in batch condensation polymerization reactor, 3 is reacted under 1MPa small
When；Then react 4 hours under vacuo, obtain polymer melt；Finally by polymer melt it is water cooled granulation obtain graphene/
PA6 nano composite materials.
(3) it is 50 by weight by PC, graphene/PA6 nano composite materials and SMA:50:5, premixed in mixer,
Obtain well mixed premix；
(4) with double screw extruder, melt blending is extruded under conditions of 250 DEG C of melting temperature, rotating speed 200rpm, cooling,
Granulation, is made PC/PA6/ graphene composite materials.
Composite after melt blending is molded into standard testing batten with injection machine and carries out Mechanics Performance Testing, performance
Test data is shown in Table 1.
Embodiment 3
(1) it is that 3 μm of modified graphene and 10 mass parts deionized waters add 100 mass by 1 mass parts lateral dimension
In the caprolactam melt of part, (300rpm) stirs and evenly mixs to form dispersion liquid at a high speed at 80 DEG C.The modified graphene is table
Face has the single-layer graphene of the oxygen-containing functional groups such as carboxyl, hydroxyl；Carbon-to-oxygen ratio is 6；
(2) under nitrogen protection, above-mentioned dispersion liquid is warming up to 250 DEG C in batch condensation polymerization reactor, 3 is reacted under 0.8MPa
Hour；Then react 4 hours under vacuo, obtain polymer melt；The water cooled granulation of polymer melt is finally obtained into graphite
Alkene/PA6 nano composite materials.
(3) PC, graphene/PA6 nano composite materials and SMA are matched as 50 by weight:50:8, in mixer
Premix, obtains well mixed premix；
(4) with double screw extruder, melt blending is extruded under conditions of 250 DEG C of melting temperature, rotating speed 250rpm, cooling,
Granulation, is made PC/PA6/ graphene composite materials.
Composite after melt blending is molded into standard testing batten with injection machine and carries out Mechanics Performance Testing, performance
Test data is shown in Table 1.
Comparative example
(1) it is 50 by weight by PC, PA6 and SMA:50:5, premixed in mixer, obtain well mixed premix
Material；
(4) with double screw extruder, melt blending is extruded under conditions of 250 DEG C of melting temperature, rotating speed 200rpm, cooling,
Granulation, is made PC/PA6 composites.
Composite after melt blending is molded into standard testing batten with injection machine and carries out Mechanics Performance Testing, performance
Test data is shown in Table 1.
The performance test data of the composite of table 1
From table 1, tensile strength, bending strength and the breach punching of the PC/PA6 composites being modified with graphene
The all more unmodified PC/PA6 composites of hit intensity are significantly improved, and graphene can significantly improve the mechanics of composite
Performance, while graphene can also assign the more excellent anti-ultraviolet ageing of material, anti-flammability, heat resistance and antistatic property etc.,
The requirement to power PC/PA6 composites in some use occasions is disclosure satisfy that, the application of PC/PA6 composites has been expanded
Field, with market potential application value.
Claims (3)
1. a kind of PC/PA6/ graphene composite materials, it is characterised in that the material is by PC and the nano combined materials of graphene/PA6
Material is obtained after being extruded through melt blending, and the graphene/PA6 nano complexes materials are by PA6 and the mono-layer graphite for being grafted with PA6
Alkene is constituted, and the lateral dimension of the single-layer graphene for being grafted with PA6 is more than 3 microns；The quality of graphene and PA6 gross mass
The ratio between be 0.1-1:100.
2. according to the method described in claim 1, it is characterised in that the graphene/PA6 nano-complexes are as follows
Prepare：
(1) caprolactam that the modified graphene of 0.1-1 mass parts and 1-10 mass parts deionized water are added into 100 mass parts melts
In body, (300~500rpm) stirs and evenly mixs to form dispersion liquid at a high speed at 80 DEG C.The modified graphene has carboxylic for surface
The single-layer graphene of the oxygen-containing functional groups such as base, hydroxyl；Carbon-to-oxygen ratio be 2.5 to 6 between；
(2) under nitrogen protection, above-mentioned dispersion liquid is warming up to 250-220 DEG C in batch condensation polymerization reactor, it is anti-under 0.5-1MPa
Answer 3 hours；Then react 4 hours under vacuo, obtain polymer melt；The water cooled granulation of polymer melt is finally obtained into stone
Black alkene/PA6 nano composite materials.
3. a kind of preparation method of PC/PA6/ graphene composite materials, it is characterised in that its preparation process is as follows：
(1) it is 50~25 by weight by PC, graphene/PA6 nano composite materials and compatilizer SMA:25~50:5~10,
Premixed in mixer, obtain well mixed premix；
(2) with double screw extruder, melt blending is squeezed under conditions of 240~220 DEG C of processing temperature, 150~250rpm of rotating speed
Go out, cool down, PC/PA6/ graphene composite materials are made in granulation.
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| CN111675877A (en) * | 2020-05-28 | 2020-09-18 | 安徽钰泽塑业科技股份有限公司 | Anti-aging modified ABS plastic and preparation method thereof |
| 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 |
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