CN106633037A - Preparation method of graphene/nylon-6 composite - Google Patents
Preparation method of graphene/nylon-6 composite Download PDFInfo
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- CN106633037A CN106633037A CN201611157447.5A CN201611157447A CN106633037A CN 106633037 A CN106633037 A CN 106633037A CN 201611157447 A CN201611157447 A CN 201611157447A CN 106633037 A CN106633037 A CN 106633037A
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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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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- C08K7/00—Use of ingredients characterised by shape
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
Abstract
The invention discloses a preparation method of a graphene/nylon-6 composite. The preparation method comprises the following steps: (1) pretreatment of a caprolactam monomer; (2) pre-intercalation and swelling of graphite; (3) in-situ polymerization and graphite layer stripping; and (4) product cleaning and drying. In the invention, through monomer pre-intercalation and performing an in-situ polymerization reaction between the graphite layers, the synthesis of nylon-6 is realized while the natural graphite is stripped into graphene to obtain a graphene/nylon-6 composite with high thermal conductivity. The prepared composite has the advantages of uniform dispersion of heat conducting filler graphene, short preparation process, low cost and easiness in control; compared with existing preparation method, the prepared graphene/nylon-6 composite has good thermal conductivity and is applicable to commercial production and application; and the wide application of the nylon composites can be further expanded in the fields such as electronics, communication products and mechanical industry.
Description
Technical field
The present invention relates to technical field of composite preparation, and in particular to prepared by a kind of Graphene/nylon-6 composite
Method.
Background technology
Heat Conduction Material is widely used in electronic equipment, information and display system, radiating treatment device, auto parts machinery etc. and people
Closely related field of living；Traditional Heat Conduction Material mainly adopts metal material, but its poor corrosion resistance to limit
Its range of application, and drop significantly to improve the means such as alloy technology, corrosion-inhibiting coating technology that corrosion resistance of metals is adopted
Low its heat conductivility；In recent years, as the multifunction of macromolecular material develops and applies, thermal conductive polymer material is excellent because of its
Elegant corrosion resistance and electrical insulating property and be subject to people's extensive concern；Polymer itself thermal conductivity factor is low, in order to expand its conduct
The application of Heat Conduction Material, need to improve its heat conductivility；Thermal conductive polymer common at present is divided into two classes-Intrinsical heat conduction polymerization
Thing and filled-type thermally conductive polymer；Intrinsical thermal conductive polymer be by preparation process adjust polymer molecule chain structure come
Its thermal conductivity factor is lifted, polyaniline, polypyrrole, polythiophene etc. is common are；This method is by preparation technology and cost control
Limit, the laboratory research stage is still at present；And filled-type thermally conductive polymer is then to take certain manufacturing process to lead height
Hot filler is combined with polymer, and heat-conductive composite material is obtained by learning from other's strong points to offset one's weaknesses；With preparation process is simple it is controllable, into
This is cheap and is capable of achieving the advantages such as industrialized production, is the first-selection for preparing High thermal-conductivitypolymer polymer composite material；Nylon-6 is used as one
Kind important engineering plastics, with excellent specific properties such as corrosion-resistant, fracture strength is high, excellent in abrasion resistance, high resiliency, are widely used
In numerous areas such as electronic apparatus, machine-building, Aero-Space, packagings；But as most polymers, nylon-6 itself
Thermal conductivity is bad, and its thermal conductivity coefficient is about 0.3Wm-1·K-1, less than the one thousandth of copper, this causes nylon-6 in heat conduction material
Application in material field is restricted；Graphene as a kind of new two-dimentional carbon nanomaterial, with high heat conduction system
Number, the room temperature thermal conductivity factor of single-layer graphene is up to 5300Wm-1·K-1, this allows Graphene as a kind of preferable
Heat filling；Existing Graphene/nylon-6 composite material preparation is loaded down with trivial details, and high cost is unfavorable for industrial production, and leads
Hot coefficient is not high.
The content of the invention
The present invention provides a kind of process is simple, low cost, thermal conductivity factor high Graphene/nylon-6 composite preparation side
Method.
The technical solution used in the present invention is：A kind of Graphene/nylon-6 composite material and preparation method thereof, including following step
Suddenly：
（1）Caprolactam is heated to after melting, 6-aminocaprolc acid is added, stirring is complete up to reaction, obtains pretreated
Caprolactam solution；Wherein the mass ratio of caprolactam and 6-aminocaprolc acid is 9:1~10: 1；
（2）Graphite is added into step（1）In the solution for obtaining, ultrasonication obtains mixture suspension；Wherein graphite and solution
Mass ratio be 1:100~1: 10；
（3）Step（2）Gained suspension is warming up to 150 ~ 180 DEG C and is incubated 1 ~ 2 hour, then heats to 200 ~ 260 DEG C of insulations 6 ~ 9 little
When natural cooling；
（4）Step（3）The product washing for obtaining obtains final product required Graphene/nylon-6 composite after being dried.
Further, the graphite is 300 ~ 400 mesh crystalline flake graphites.
Further, the step（1）Middle heating-up temperature is 70 ~ 100 DEG C, and mixing time is 30 ~ 90 minutes.
Further, the step（2）Middle ultrasonic treatment time is 10 ~ 120 minutes, and ultrasonic power is 400 ~ 500W.
Further, the step（3）Apply stirring in course of reaction, and be passed through nitrogen protection.
Further, the step（4）Middle washing is using 80 ~ 100 DEG C of water washing 3 ~ 5 times.
Further, the step（4）Middle employing air dry oven is carried out under conditions of 80 ~ 100 DEG C, is dried 18 ~ 24
Hour.
The invention has the beneficial effects as follows：
（1）The method process is simple that the present invention is adopted, it is only necessary to introduce to natural stone on the basis of nylon-6 cationic polymerization
, there is no contaminative emission problem in the pre- intercalation processing of ink；
（2）Low cost of the present invention, using common crystalline flake graphite as raw material；
（3）Good heat conductivity of the present invention, using native graphite interlayer polymerization exfoliated graphite layer is caused, and realizes Graphene poly-
It is dispersed between compound matrix, can effectively lift the heat conductivility of composite.
Description of the drawings
Fig. 1 is schematic flow sheet of the present invention.
Fig. 2 is the SEM figures of embodiment 1 in the present invention, embodiment 6, embodiment 7.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention will be further described with specific embodiment.
Embodiment 1
（1）Monomer is pre-processed：45g caprolactams are heated to add 5g 6-aminocaprolc acids, 30 points of mechanical agitation after 80 DEG C of meltings
Clock, obtains colourless transparent liquid；
（2）The pre- intercalation of graphite and swelling：By 5g, 325 mesh native graphites add step（1）In gained transparency liquid, Jing 450W surpass
Sonicated carries out monomer for 1 hour to the pre- intercalation of graphite and swelling, obtains mixture suspension；
（3）In-situ polymerization is peeled off with graphite linings：To step（2）Gained mixing suspension applies mechanical agitation and rises under nitrogen protection
Temperature to 180 DEG C are incubated 1 hour, and natural cooling after being incubated 9 hours to 250 DEG C is further heated up afterwards.
（4）Product cleaning and drying：Treat step（3）Middle product is cooled to after solid with 80 DEG C of hot washes 5 times, it
It is placed in afterwards in 80 DEG C of electric heating constant-temperature blowing drying box and is dried 24 hours, obtains final product Graphene/nylon-6 composite.
By step（4）Gained Graphene/nylon-6 composite is placed in mould, 220 DEG C of Jing, after 5MPa hot pressing 2 minutes,
Then normal temperature pressurize 10 minutes under the conditions of 20MPa, are obtained Graphene/nylon-6 composite print；The composite wood after testing
Material thermal conductivity factor reaches 2.2016Wm-1·K-1。
Embodiment 2
（1）Monomer is pre-processed：45g caprolactams are heated to add 5g 6-aminocaprolc acids, 30 points of mechanical agitation after 80 DEG C of meltings
Clock, obtains colourless transparent liquid；
（2）The pre- intercalation of graphite and swelling：By 2.5g, 400 mesh native graphites add step（1）In gained transparency liquid, Jing 450W
Ultrasonication carries out monomer for 1.5 hours to the pre- intercalation of graphite and swelling, obtains mixture suspension；
（3）In-situ polymerization is peeled off with graphite linings：To step（2）Gained mixing suspension applies mechanical agitation and rises under nitrogen protection
Temperature to 180 DEG C are incubated 1 hour, and natural cooling after being incubated 9 hours to 250 DEG C is further heated up afterwards.
（4）Product cleaning and drying：Treat step（3）Middle product is cooled to after solid with 80 DEG C of hot washes 5 times, it
It is placed in afterwards in 80 DEG C of electric heating constant-temperature blowing drying box and is dried 24 hours, obtains final product Graphene/nylon-6 composite.
By step（4）Gained Graphene/nylon-6 composite is placed in mould, 220 DEG C of Jing, after 5MPa hot pressing 2 minutes,
Then normal temperature pressurize 10 minutes under the conditions of 20MPa, are obtained Graphene/nylon-6 composite print；The composite wood after testing
Material thermal conductivity factor reaches 1.8406Wm-1·K-1。
Embodiment 3
（1）Monomer is pre-processed：45g caprolactams are heated to add 5g 6-aminocaprolc acids, 30 points of mechanical agitation after 80 DEG C of meltings
Clock, obtains colourless transparent liquid；
（2）The pre- intercalation of graphite and swelling：By 0.5g, 400 mesh native graphites add step（1）In gained transparency liquid, Jing 450W
Ultrasonication carries out monomer for 1 hour to the pre- intercalation of graphite and swelling, obtains mixture suspension；
（3）In-situ polymerization is peeled off with graphite linings：To step（2）Gained mixing suspension applies mechanical agitation and rises under nitrogen protection
Temperature to 180 DEG C are incubated 1 hour, and natural cooling after being incubated 9 hours to 250 DEG C is further heated up afterwards.
（4）Product cleaning and drying：Treat step（3）Middle product is cooled to after solid with 80 DEG C of hot washes 5 times, it
It is placed in afterwards in 80 DEG C of electric heating constant-temperature blowing drying box and is dried 24 hours, obtains final product Graphene/nylon-6 composite.
By step（4）Gained Graphene/nylon-6 composite is placed in mould, 220 DEG C of Jing, after 5MPa hot pressing 2 minutes,
Then normal temperature pressurize 10 minutes under the conditions of 20MPa, are obtained Graphene/nylon-6 composite print；The composite wood after testing
Material thermal conductivity factor reaches 1.4298Wm-1·K-1。
Embodiment 4
（1）Monomer is pre-processed：50g caprolactams are heated to add 5g 6-aminocaprolc acids, 30 points of mechanical agitation after 80 DEG C of meltings
Clock, obtains colourless transparent liquid；
（2）The pre- intercalation of graphite and swelling：By 5.5g, 325 mesh native graphites add step（1）In gained transparency liquid, Jing 500W
Ultrasonication carries out monomer for 1.5 hours to the pre- intercalation of graphite and swelling, obtains mixture suspension；
（3）In-situ polymerization is peeled off with graphite linings：To step（2）Gained mixing suspension applies mechanical agitation and rises under nitrogen protection
Temperature to 180 DEG C are incubated 1 hour, and natural cooling after being incubated 9 hours to 250 DEG C is further heated up afterwards.
（4）Product cleaning and drying：Treat step（3）Middle product is cooled to after solid with 80 DEG C of hot washes 5 times, it
It is placed in afterwards in 80 DEG C of electric heating constant-temperature blowing drying box and is dried 24 hours, obtains final product Graphene/nylon-6 composite.
By step（4）Gained Graphene/nylon-6 composite is placed in mould, 220 DEG C of Jing, after 5MPa hot pressing 2 minutes,
Then normal temperature pressurize 10 minutes under the conditions of 20MPa, are obtained Graphene/nylon-6 composite print；The composite wood after testing
Material thermal conductivity factor reaches 2.1582 Wm-1·K-1。
Embodiment 5
（1）Monomer is pre-processed：50g caprolactams are heated to add 5g 6-aminocaprolc acids, 30 points of mechanical agitation after 80 DEG C of meltings
Clock, obtains colourless transparent liquid；
（2）The pre- intercalation of graphite and swelling：By 2.525g, 325 mesh native graphites add step（1）In gained transparency liquid, Jing
450W ultrasonications carry out monomer for 0.5 hour to the pre- intercalation of graphite and swelling, obtain mixture suspension；
（3）In-situ polymerization is peeled off with graphite linings：To step（2）Gained mixing suspension applies mechanical agitation and rises under nitrogen protection
Temperature to 180 DEG C are incubated 1 hour, and natural cooling after being incubated 9 hours to 250 DEG C is further heated up afterwards.
（4）Product cleaning and drying：Treat step（3）Middle product is cooled to after solid with 80 DEG C of hot washes 5 times, it
It is placed in afterwards in 80 DEG C of electric heating constant-temperature blowing drying box and is dried 24 hours, obtains final product Graphene/nylon-6 composite.
By step（4）Gained Graphene/nylon-6 composite is placed in mould, 220 DEG C of Jing, after 5MPa hot pressing 2 minutes,
Then normal temperature pressurize 10 minutes under the conditions of 20MPa, are obtained Graphene/nylon-6 composite print；The composite wood after testing
Material thermal conductivity factor reaches 1.7269Wm-1·K-1。
Embodiment 6
（1）Monomer is pre-processed：45g caprolactams are heated to add 5g 6-aminocaprolc acids, 30 points of mechanical agitation after 80 DEG C of meltings
Clock, obtains colourless transparent liquid；
（2）Cationic polymerization：To step（1）In gained transparency liquid, apply mechanical agitation and heat up under nitrogen protection
180 DEG C are reacted 1 hour, and natural cooling after reacting 9 hours is further heated up to 250 DEG C afterwards；
（3）Product cleaning and drying：Treat step（2）Middle product is cooled to after solid with 80 DEG C of hot washes 5 times, it is rearmounted
It is dried 24 hours in 80 DEG C of electric heating constant-temperature blowing drying box, obtains final product nylon-6.
By step（3）Gained nylon-6 is placed in mould, 220 DEG C of Jing, after 5 MPa hot pressing 2 minutes, then in 20 MPa bars
Normal temperature pressurize 10 minutes under part, are obtained nylon-6 print；After testing the material thermal conductivity is 0.3230Wm-1·K-1。
Embodiment 7
（1）Monomer is pre-processed：45g caprolactams are heated to add 5g 6-aminocaprolc acids, 30 points of mechanical agitation after 80 DEG C of meltings
Clock, obtains colourless transparent liquid；
（2）Cationic polymerization：To step（1）In gained transparency liquid, apply mechanical agitation and heat up under nitrogen protection
180 DEG C are reacted 1 hour, and natural cooling after reacting 9 hours is further heated up to 250 DEG C afterwards；
（3）To step（2）5g, 325 mesh native graphites is added to continue to stir 30 minutes in gained liquid；
（4）Product cleaning and drying：Treat step（3）Middle product is cooled to after solid with 80 DEG C of hot washes 5 times, it is rearmounted
It is dried 24 hours in 80 DEG C of electric heating constant-temperature blowing drying box, obtains final product graphite/nylon-6 melt blended material.
By step（4）Gained graphite/nylon-6 melt blended material is placed in mould, 220 DEG C of Jing, after 5MPa hot pressing 2 minutes,
Then normal temperature pressurize 10 minutes under the conditions of 20MPa, are obtained graphite/nylon-6 melt blended material print；The composite wood after testing
Material thermal conductivity factor is 0.8966Wm-1·K-1。
Graphite and nylon-6 individualism in graphite/nylon-6 melt blended material as can be seen from Figure 2, Graphene/nylon-
Graphene layer distributed in 6 composites, nylon-6 is distributed between graphene layer, and graphene dispersion is uniform.
Graphite can regard as from structure and formed by Graphene stacking, thus peeling off graphite by way of can obtain
Graphene；Monomer molecule is attracted by special role be intercalation into native graphite interlayer, and causes home position polymerization reaction in interlayer,
Moved using reaction heat and long-chain molecule, it is possible to achieve the stripping of Graphene and its dispersed in polymeric matrix, from
And a step is obtained nylon-6/graphene composite material；The stripping of Graphene and its good dispersiveness are then conducive to significantly carrying
Rise the heat conductivility of nylon-6 composite；Preparation method of the present invention caprolactam is added first heat fusing and is added as catalysis
The 6-aminocaprolc acid of agent；After appropriate native graphite is added, by ultrasonication and churned mechanically collective effect, oneself is realized
Swelling and pre- intercalation of the lactams to expanded graphite；Subsequently the caprolactam of graphite layers is caused to carry out by controlling reaction condition
Home position polymerization reaction, native graphite is peeled off while synthetic nylon -6 and is Graphene and it is uniformly divided in polymeric matrix
Dissipate, so as to Graphene/nylon-6 high-heat-conductive composite material is obtained；Compared to pure nylon-6 or graphite mixing filled nylon-6, its
Thermal conductivity factor can lift more than 4.4 times, up to 1.43 ~ 2.20Wm-1·K-1；The present invention is by the pre- intercalation of monomer and in graphite linings
Between carry out home position polymerization reaction, while realizing that nylon-6 synthesizes, strippings native graphite is Graphene, so as to prepared Graphene/
Nylon-6 high-heat-conductive composite material；The present invention prepare composite heat filling graphene dispersion it is uniform, preparation flow is short, into
This low, preparation flow is short, control is simple, the Graphene of preparation/nylon-6 composite heat conduction compared with existing preparation method
Performance is good, and suitable for commercially producing and applying；Can further expand nylon series composite materials such as electronic apparatus,
The extensive application in the fields such as communication product, mechanical industry.
Claims (7)
1. a kind of Graphene/nylon-6 composite material and preparation method thereof, it is characterised in that comprise the following steps：
(1) caprolactam is heated to after melting, adds 6-aminocaprolc acid, stirring is complete up to reaction, obtains pretreated
Caprolactam solution；Wherein the mass ratio of caprolactam and 6-aminocaprolc acid is 9:1～10:1；
(2) in the solution for adding step (1) to obtain in graphite, ultrasonication obtains mixture suspension；Wherein graphite and solution
Mass ratio be 1:100～1:10；
(3) step (2) gained suspension is warming up to 150～180 DEG C and is incubated 1～2 hour, then heats to 200～260 DEG C of insulations 6
～9 as a child natural coolings；
(4) the product washing that step (3) is obtained obtains final product required Graphene/nylon-6 composite after being dried.
2. a kind of Graphene/nylon-6 composite material and preparation method thereof according to claim 1, it is characterised in that the stone
Ink is 300～400 mesh crystalline flake graphites.
3. a kind of Graphene/nylon-6 composite material and preparation method thereof according to claim 1, it is characterised in that the step
Suddenly heating-up temperature is 70～100 DEG C in (1), and mixing time is 30～90 minutes.
4. a kind of Graphene/nylon-6 composite material and preparation method thereof according to claim 1, it is characterised in that the step
Suddenly ultrasonic treatment time is 10～120 minutes in (2), and ultrasonic power is 400～500W.
5. a kind of Graphene/nylon-6 composite material and preparation method thereof according to claim 1, it is characterised in that the step
Suddenly apply stirring in (3) course of reaction, and be passed through nitrogen protection.
6. a kind of Graphene/nylon-6 composite material and preparation method thereof according to claim 1, it is characterised in that the step
Suddenly in (4) washing using 80～100 DEG C of water washing 3～5 times.
7. a kind of Graphene/nylon-6 composite material and preparation method thereof according to claim 1, it is characterised in that the step
Suddenly carried out under conditions of 80～100 DEG C using air dry oven in (4), it is dry 18～24 hours.
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Cited By (6)
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|---|---|---|---|---|
| CN107383363A (en) * | 2017-07-14 | 2017-11-24 | 常州轻工职业技术学院 | A kind of graphene grafting polycaprolactam composite material and preparation method thereof |
| CN107418195A (en) * | 2017-09-06 | 2017-12-01 | 张永霞 | A kind of preparation method of intercalated graphite alkene composite nylon material |
| CN109880080A (en) * | 2019-03-29 | 2019-06-14 | 宁波石墨烯创新中心有限公司 | A kind of graphene/polymer composite material and preparation method thereof |
| CN109942883A (en) * | 2019-04-03 | 2019-06-28 | 西南交通大学 | Utilize interlayer in-situ polymerization graphene/foam of polymers batch preparation |
| CN111471296A (en) * | 2020-01-20 | 2020-07-31 | 江苏华永汽车悬架有限公司 | Manufacturing method of lightweight high-fatigue air spring plastic base |
| CN111909372A (en) * | 2020-06-29 | 2020-11-10 | 宁波石墨烯创新中心有限公司 | Graphene/polyamide composite material and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107383363A (en) * | 2017-07-14 | 2017-11-24 | 常州轻工职业技术学院 | A kind of graphene grafting polycaprolactam composite material and preparation method thereof |
| CN107383363B (en) * | 2017-07-14 | 2020-08-28 | 常州工业职业技术学院 | Graphene grafted polycaprolactam composite material and preparation method thereof |
| CN107418195A (en) * | 2017-09-06 | 2017-12-01 | 张永霞 | A kind of preparation method of intercalated graphite alkene composite nylon material |
| CN109880080A (en) * | 2019-03-29 | 2019-06-14 | 宁波石墨烯创新中心有限公司 | A kind of graphene/polymer composite material and preparation method thereof |
| CN109942883A (en) * | 2019-04-03 | 2019-06-28 | 西南交通大学 | Utilize interlayer in-situ polymerization graphene/foam of polymers batch preparation |
| CN111471296A (en) * | 2020-01-20 | 2020-07-31 | 江苏华永汽车悬架有限公司 | Manufacturing method of lightweight high-fatigue air spring plastic base |
| CN111909372A (en) * | 2020-06-29 | 2020-11-10 | 宁波石墨烯创新中心有限公司 | Graphene/polyamide composite material and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN106633037B (en) | 2018-12-25 |
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