CN106947233B - A kind of PC/PA6/ graphene composite material and preparation method thereof - Google Patents
A kind of PC/PA6/ graphene composite material and preparation method thereof Download PDFInfo
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- CN106947233B CN106947233B CN201710255904.2A CN201710255904A CN106947233B CN 106947233 B CN106947233 B CN 106947233B CN 201710255904 A CN201710255904 A CN 201710255904A CN 106947233 B CN106947233 B CN 106947233B
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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
-
- 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
-
- 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
Abstract
The present invention provides a kind of PC/PA6/ graphene composite materials and preparation method thereof, belong to modifying plastics field.PC/PA6/ graphene composite material is made of PC, PA6, graphene and compatilizer SMA, the composite material is to carry out melt blending extrusion using graphene/PA6 nanocomposite and PC to be made, and the graphene/PA6 nanocomposite is obtained by modified graphene and caprolactam in-situ polymerization.Preparation-obtained power PC/PA6/ the graphene composite material of the present invention has good toughness and intensity, there are the performances such as superior anti-ultraviolet ageing, anti-flammability, heat resistance, antistatic property and processing performance simultaneously, expanded PC/PA6 composite material in the application of more high-end field.
Description
Technical field
The invention belongs to modifying plastics fields, and in particular to a kind of PC/PA6/ graphene composite material and preparation method thereof.
Background technique
Polycarbonate (PC) has erosion-resisting characteristics outstanding and creep-resistant property, resists cold, is heat-resist, and water absorption rate is low, system
Product dimensionally stable, but that there is also processing fluidities is poor, solvent resistance is poor, easy stress cracking and lacks to notch sensitive etc.
It falls into.Nylon (PA) is a kind of engineering plastics haveing 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, the water imbibition of Yin Qigao and cause the dimensional stability of product poor, make it in some particular fields
Application under closing is restricted.It can be seen that PC and PA material has preferable complementarity in aspect of performance, prepared is answered
Condensation material can be applied to the fields such as automobile, electronics, aircraft, office furniture, building, show extremely strong vitality.
The method for being typically prepared PC/PA6 alloy is to carry out capacity increasing modifying using expanding material to improve performance, but the degree improved
It is limited, it is not still able to satisfy some high-end fields to the requirement of power PC/PA6 alloy material.Graphene is a kind of with two
The nano material for tieing up crystal structure, due to its outstanding mechanical property, electric property, thermal property and unique electromagnetic property
Deng graphene shows wide application prospect in many fields, and gradually moves towards practical application.Graphene is both most thin
Material, and most tough material, it is there are many reporting that graphene is compound with high polymer, the strong of material can be obviously improved
Degree, modulus, toughness, heat resistance and ageing-resistant performance.If high performance graphene nano material can be applied to PC/PA6 as a result,
In composite material, it will assign material superior comprehensive performance.
Summary of the invention
Aiming at the above shortcomings existing in the prior art, the present invention provides a kind of PC/PA6/ graphene composite material and
Preparation method.
The purpose of the present invention is achieved through the following technical solutions: a kind of PC/PA6/ graphene composite material, special
Sign is that the material is obtained after melt blending squeezes out by PC and graphene/PA6 nanocomposite, the graphene/
PA6 nano complexes material is made of PA6 with the single-layer graphene for being grafted with PA6, the single-layer graphene for being grafted with PA6
Lateral dimension is greater than 3 microns；The ratio between quality and the gross mass of PA6 of graphene are 0.1-1:100.
Further, the graphene/PA6 nanocomposite is made by the steps to obtain:
(1) by acyl in oneself of the modified graphene of 0.1-1 mass parts and 1-10 mass parts deionized water 100 mass parts of addition
In amine melt, high speed (300~500rpm) stirs and evenly mixs to form dispersion liquid 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 is between 2.5 to 6；
(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 it reacts 4 hours under vacuum, obtains polymer melt；Finally it is granulated polymer melt is water cooled
To graphene/PA6 nanocomposite.
Further, power PC/PA6/ graphene composite material preparation step is as follows:
(1) by ratio of weight and the number of copies it is 50~25:25~50 by PC, graphene/PA6 nanocomposite and compatilizer SMA:
5~10, it is premixed in mixing machine, obtains uniformly mixed premix；
(2) double screw extruder melt blending under conditions of 240~220 DEG C of processing temperature, 150~250rpm of revolving speed is used
It squeezes out, it is cooling, it is granulated, PC/PA6/ graphene composite material is made.
The beneficial effects of the present invention are:
1, compound by being carried out using graphene/PA6 nanocomposite and PC, prepare power PC/PA6/ graphene
Composite material is beneficial in that prepared graphene/PA6 nanocomposite, Sheet Graphite alkene and caprolactam are logical
The mode effecting reaction of in-situ polymerization is crossed, so that the graphene of lamella can be uniformly dispersed in PA6 matrix, utilizes ultralow graphene
Additive amount can prepare High-performance graphene/PA6 nanocomposite master batch, then graphene/PA6 that polymerization reaction is obtained
Composite material master batch is mixed with PC, can properly settle the dispersion of graphene in the composite, and then improve composite wood
Expect comprehensive performance.
2, graphene is added to preparation PC/PA6/ graphene composite material in PC/PA6 composite material, graphene is not only
The mechanical property of composite material is improved, while can also assign the higher heat resistance of material, anti-ultraviolet ageing, anti-flammability, resist
The comprehensive performances such as static behaviour.
3, power PC/PA6/ graphene composite material is processed in such a way that melt blending squeezes out, this method operative employee
Skill is simple, solvent-free pollution, high production efficiency, is suitble to large-scale production.
Detailed description of the invention
Fig. 1 is graphene of the present invention/PA6 nanocomposite partial structural diagram, wherein 1 is to be grafted with PA6's
Single-layer graphene film, 2 be free PA6.
Specific embodiment
The present invention use first situ aggregation method prepare High-performance graphene/PA6 nanometers of ultralow graphene additive amount it is multiple
Condensation material, in preparation process, select single layer, lateral dimension be greater than 3 μm, carbon-to-oxygen ratio be modified graphene between 2.5~6.
By many experiments, it is concluded that (1) graphene performance and the number of plies are closely related, the performance of multi-layer graphene is inferior to
Single-layer graphene.(2) graphene lateral dimension on polymer performance influence it is also larger, lateral dimension too it is small be unfavorable for improving it is compound
The mechanical property of materials is unfavorable for molding and adds however, lateral dimension is excessive then to will increase dramatically Composite Melt viscosity greatly very much
Work, therefore, the preferred lateral dimension of the present invention are less than the graphene of 80um；(3) carbon-to-oxygen ratio is too low illustrates graphene oxidation defect
Too much, graphene own mechanical performance is poor, limited to composite material various aspects 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 excessively high also can
So that graphene dispersion is poor, occurs clustering phenomena in a polymer matrix.Graphene/PA6 that the present invention is prepared receives
Nano composite material is made of free PA6 and the single-layer graphene film for being grafted with PA6, and structure is as shown in Figure 1.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 matrix, benefit
High-performance graphene/PA6 nanocomposite master batch can be prepared with ultralow graphene additive amount, then polymerization reaction is obtained
Graphene/PA6 composite material master batch and PC melt blending squeeze out preparation PC/PA6/ graphene composite material, can properly solve
The certainly the dispersion of graphene in the composite, and then more effectively improve composite material combination property.
The power PC of preparation of the invention/PA6/ graphene composite material is molded using ASTM standard, and injection molding machine is 230
Injection molding under the conditions of~220 DEG C is handled each raw material in 110 DEG C of dry 3h before injection molding.
Measuring mechanical property method:
1, GB/T1040-2006 standard testing, tensile speed 50mm/min tensile property: are pressed；
2, CB/T9341-2008 standard testing, rate of bending 2mm/min bending property: are pressed；
3, Izod notched impact strength: GB/T1843-2008 standard testing is pressed.
Sample molding after temperature be 23 ± 2 DEG C, humidity be 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
It is bright, it should not be understood 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) 100 mass are added in the modified graphene by 0.1 mass parts lateral dimension greater than 3 μm and 1 mass parts deionized water
In the caprolactam melt of part, high speed (300rpm) stirs and evenly mixs to form dispersion liquid 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 in batch condensation polymerization reactor 250 DEG C, reacts 3 at 0.6MPa
Hour；Then it reacts 4 hours under vacuum, obtains polymer melt；The water cooled granulation of polymer melt is finally obtained into graphite
Alkene/PA6 nanocomposite.
(3) by weight it is 25:25:5 by PC, graphene/PA6 nanocomposite and SMA, is premixed in mixing machine,
Obtain uniformly mixed premix；
(4) with double screw extruder, melt blending is squeezed out under conditions of 250 DEG C of melting temperature, revolving speed 200rpm, cooling,
It is granulated, PC/PA6/ graphene composite material is made.
Composite material after melt blending is molded into standard testing batten with injection molding machine and carries out Mechanics Performance Testing, performance
Test data is shown in Table 1.
Embodiment 2
(1) 100 matter are added in the modified graphene by 1 mass parts lateral dimension greater than 3 μm and 10 mass parts deionized waters
In the caprolactam melt for measuring part, high speed (300rpm) stirs and evenly mixs to form dispersion liquid 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 in batch condensation polymerization reactor 220 DEG C, it is small that 3 is reacted at 1MPa
When；Then it reacts 4 hours under vacuum, obtains polymer melt；Finally by polymer melt it is water cooled granulation obtain graphene/
PA6 nanocomposite.
(3) by weight it is 50:50:5 by PC, graphene/PA6 nanocomposite and SMA, is premixed in mixing machine,
Obtain uniformly mixed premix；
(4) with double screw extruder, melt blending is squeezed out under conditions of 250 DEG C of melting temperature, revolving speed 200rpm, cooling,
It is granulated, PC/PA6/ graphene composite material is made.
Composite material after melt blending is molded into standard testing batten with injection molding machine and carries out Mechanics Performance Testing, performance
Test data is shown in Table 1.
Embodiment 3
(1) 100 mass are added for 3 μm of modified graphene and 10 mass parts deionized waters in 1 mass parts lateral dimension
In the caprolactam melt of part, high speed (300rpm) stirs and evenly mixs to form dispersion liquid 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 in batch condensation polymerization reactor 250 DEG C, reacts 3 at 0.8MPa
Hour；Then it reacts 4 hours under vacuum, obtains polymer melt；The water cooled granulation of polymer melt is finally obtained into graphite
Alkene/PA6 nanocomposite.
(3) PC, graphene/PA6 nanocomposite and SMA are matched in parts by weight as 50:50:8, in mixing machine
Premix, obtains uniformly mixed premix；
(4) with double screw extruder, melt blending is squeezed out under conditions of 250 DEG C of melting temperature, revolving speed 250rpm, cooling,
It is granulated, PC/PA6/ graphene composite material is made.
Composite material after melt blending is molded into standard testing batten with injection molding machine and carries out Mechanics Performance Testing, performance
Test data is shown in Table 1.
Comparative example
(1) by weight it is 50:50:5 by PC, PA6 and SMA, is premixed in mixing machine, obtains uniformly mixed premix
Material；
(4) with double screw extruder, melt blending is squeezed out under conditions of 250 DEG C of melting temperature, revolving speed 200rpm, cooling,
It is granulated, PC/PA6 composite material is made.
Composite material after melt blending is molded into standard testing batten with injection molding machine and carries out Mechanics Performance Testing, performance
Test data is shown in Table 1.
The performance test data of 1 composite material of table
Seen from table 1, tensile strength, bending strength and the notch punching for the PC/PA6 composite material being modified with graphene
The all more unmodified PC/PA6 composite material of hit intensity is significantly improved, and graphene can significantly improve the mechanics of composite material
Performance, while graphene can also assign the superior anti-ultraviolet ageing of material, anti-flammability, heat resistance and antistatic property etc.,
It can satisfy in some use occasions to the requirement of power PC/PA6 composite material, expanded the application of PC/PA6 composite material
Field has market potential application value.
Claims (3)
1. a kind of PC/PA6/ graphene composite material, which is characterized in that the material is by PC and the nano combined material of graphene/PA6
Material obtains after melt blending squeezes out, and the graphene/PA6 nanocomposite is by PA6 and the single-layer graphene for being grafted with PA6
The lateral dimension of composition, the single-layer graphene for being grafted with PA6 is greater than 3 microns；The quality of graphene and the mass ratio of PA6
For 0.1-1:100.
2. PC/PA6/ graphene composite material according to claim 1, which is characterized in that described graphene/PA6 nanometers
Composite material is made by the steps to obtain:
(1) caprolactam that 100 mass parts are added in the modified graphene of 0.1-1 mass parts and 1-10 mass parts deionized water is melted
In body, at 80 DEG C, mix to form dispersion liquid with the mixing speed of 300 ~ 500rpm；The modified graphene has for surface to be contained
The single-layer graphene of oxygen functional group；Carbon-to-oxygen ratio is between 2.5 to 6；
(2) under nitrogen protection, above-mentioned dispersion liquid is warming up to 250-270 DEG C in batch condensation polymerization reactor, it is anti-at 0.5-1MPa
It answers 3 hours；Then it reacts 4 hours under vacuum, obtains polymer melt；The water cooled granulation of polymer melt is finally obtained into stone
Black alkene/PA6 nanocomposite.
3. a kind of preparation method of PC/PA6/ graphene composite material, which is characterized in that its preparation step is as follows:
It (1) is by weight 50 ~ 75:25 ~ 50:5 ~ 10 by PC, graphene/PA6 nanocomposite and compatilizer SMA, mixed
It is premixed in conjunction machine, obtains uniformly mixed premix；The graphene/PA6 nanocomposite is by PA6 and is grafted with PA6's
The lateral dimension of single-layer graphene composition, the single-layer graphene for being grafted with PA6 is greater than 3 microns；The quality and PA6 of graphene
Mass ratio be 0.1-1:100；
(2) with double screw extruder, melt blending is squeezed out under conditions of 240 ~ 270 DEG C of processing temperature, 150 ~ 250rpm of revolving speed,
It is cooling, it is granulated, PC/PA6/ graphene composite material is made.
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| CN109294224A (en) * | 2018-10-29 | 2019-02-01 | 江苏亿超工程塑料有限公司 | A kind of polyamide compoiste material and preparation method thereof |
| 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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