CN106633037B - A kind of graphene/nylon-6 composite material and preparation method thereof - Google Patents
A kind of graphene/nylon-6 composite material and preparation method thereof Download PDFInfo
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- CN106633037B CN106633037B CN201611157447.5A CN201611157447A CN106633037B CN 106633037 B CN106633037 B CN 106633037B CN 201611157447 A CN201611157447 A CN 201611157447A CN 106633037 B CN106633037 B CN 106633037B
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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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- 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 kind of graphene/nylon-6 composite material and preparation method thereofs, include the following steps, the pretreatment of (1) caprolactam monomer；(2) the pre- intercalation of graphite and swelling；(3) in-situ polymerization and graphite linings are removed；(4) product cleaning and drying；The present invention carries out home position polymerization reaction by the pre- intercalation of monomer and in graphite layers, and while realizing nylon-6 synthesis, removing natural graphite is graphene, so that graphene/nylon-6 high-heat-conductive composite material be made；The composite material heat filling graphene dispersion of preparation is uniform, preparation flow is short, at low cost, preparation flow is short, control is simple, graphene/nylon-6 composite material the good heat conductivity prepared compared with existing preparation method, and be suitable for commercially producing and applying；Can further expansion nylon series composite materials the fields such as electronic apparatus, communication product, mechanical industry extensive use.
Description
Technical field
The present invention relates to technical field of composite preparation, and in particular to a kind of graphene/nylon-6 composite material preparation
Method.
Background technique
Heat Conduction Material is widely used in electronic equipment, information and display system, radiating treatment device, automobile parts etc. and people
Closely related field of living；Traditional Heat Conduction Material mainly uses metal material, but its poor corrosion resistance limits
Its application range, and dropped significantly to improve the means such as alloy technology used by corrosion resistance of metals, corrosion-inhibiting coating technology
Its low heating conduction；In recent years, as the multifunction of high molecular material develops and application, thermal conductive polymer material are excellent because of its
Elegant corrosion resistance and electrical insulating property and by people's extensive concern；Polymer itself thermal coefficient is low, in order to expand its conduct
The application of Heat Conduction Material need to improve its heating conduction；Thermal conductive polymer common at present is divided into the thermally conductive polymerization of two classes-Intrinsical
Object and filled-type thermally conductive polymer；Intrinsical thermal conductive polymer be by adjust during the preparation process polymer molecule chain structure come
Its thermal coefficient is promoted, common are polyaniline, polypyrrole, polythiophene etc.；This method is by preparation process and cost control
Limitation is still in the laboratory research stage at present；And filled-type thermally conductive polymer is then that certain manufacturing process is taken to lead height
Hot filler and polymer progress are compound, obtain heat-conductive composite material and learning from other's strong points to offset one's weaknesses；It is simple controllable with preparation process, at
This is cheap and can realize the advantages such as industrialized production, is the first choice for preparing High thermal-conductivitypolymer polymer composite material；Nylon-6 is as one
The important engineering plastics of kind, have the excellent characteristics such as corrosion-resistant, breaking strength is high, wearability is excellent, high resiliency, are widely used
In numerous areas such as electronic apparatus, machine-building, aerospace, packagings；However as most polymers, nylon-6 itself
Thermal conductivity is bad, and thermal conductivity coefficient is about 0.3Wm-1·K-1, less than the one thousandth of copper, this makes nylon-6 in heat conduction material
Application in material field is restricted；Graphene has high thermally conductive system as a kind of novel two-dimentional carbon nanomaterial
Number, the room temperature thermal coefficient of single-layer graphene are up to 5300Wm-1·K-1, it is a kind of ideal that this can be used as graphene
Heat filling；Existing graphene/nylon-6 composite material preparation is cumbersome, at high cost to be unfavorable for industrial production, and leads
Hot coefficient is not high.
Summary of the invention
The present invention provides a kind of simple process, graphene/nylon-6 composite material preparation side that at low cost, thermal coefficient is high
Method.
The technical solution adopted by the present invention is that: a kind of graphene/nylon-6 composite material and preparation method thereof, including following step
It is rapid:
(1) after caprolactam being heated to melting, 6-aminocaprolc acid is added, stirring until the reaction is complete, is pre-processed
Caprolactam solution afterwards；Wherein the mass ratio of caprolactam and 6-aminocaprolc acid is 9:1 ~ 10:1；
(2) in the solution for obtaining graphite addition step (1), ultrasonication obtains mixture suspension；Wherein graphite and
The mass ratio of solution is 1:100 ~ 1:10；
(3) suspension obtained by step (2) is warming up to 150 ~ 180 DEG C and keeps the temperature 1 ~ 2 hour, then heats to 200 ~ 260 DEG C of heat preservations 6
~ 9 as a child natural coolings；
(4) up to required graphene/nylon-6 composite material after the product washing that step (3) obtains is dry.
Further, the graphite is 300 ~ 400 mesh crystalline flake graphites.
Further, heating temperature is 70 ~ 100 DEG C in the step (1), and mixing time is 30 ~ 90 minutes.
Further, ultrasonic treatment time is 10 ~ 120 minutes in the step (2), and ultrasonic power is 400 ~ 500W.
Further, apply stirring in step (3) reaction process, and be passed through nitrogen protection.
Further, it is washed in the step (4) water washing 3 ~ 5 times using 80 ~ 100 DEG C.
Further, it is carried out under conditions of 80 ~ 100 DEG C in the step (4) using air dry oven, dry 18 ~ 24
Hour.
The beneficial effects of the present invention are:
(1) method and process that the present invention uses is simple, it is only necessary to introduce on the basis of nylon-6 cationic polymerization to day
The pre- intercalation processing of right graphite, is not present pollution emission problem；
(2) present invention is at low cost, using common crystalline flake graphite as raw material；
(3) good heat conductivity of the present invention causes polymerization exfoliated graphite layer using natural graphite interlayer, realizes graphene
It is evenly dispersed between polymeric matrix, it can effectively promote the heating conduction of composite material.
Detailed description of the invention
Fig. 1 is flow diagram of the present invention.
Fig. 2 is the SEM figure of embodiment 1 in the present invention, embodiment 6, embodiment 7.
Specific embodiment
The present invention will be further described in the following with reference to the drawings and specific embodiments.
Embodiment 1
(1) monomer pre-processes: 5g 6-aminocaprolc acid, mechanical stirring is added after 45g caprolactam is heated to 80 DEG C of meltings
30 minutes, obtain colourless transparent liquid；
(2) the pre- intercalation of graphite and swelling: by 5g, 325 mesh natural graphites are added in transparency liquid obtained by step (1), warp
Progress monomer obtains mixture suspension to the pre- intercalation of graphite and swelling within 450W ultrasonication 1 hour；
(3) in-situ polymerization is removed with graphite linings: applying mechanical stirring and in nitrogen protection to suspension is mixed obtained by step (2)
Under be warming up to 180 DEG C keep the temperature 1 hour, further heat up later to 250 DEG C keep the temperature 9 hours after natural cooling.
(4) product cleaning and drying: being washed 5 times after reaction product in step (3) is cooled to solid with 80 DEG C of hot water, it
Dry 24 hours are placed in 80 DEG C of electric heating constant-temperature blowing drying box to get graphene/nylon-6 composite material.
Graphene/nylon-6 composite material obtained by step (4) is placed in mold, after 220 DEG C, 5MPa hot pressing 2 minutes,
Then graphene/nylon-6 composite material print is made in room temperature pressure maintaining 10 minutes under the conditions of 20MPa；Detected the composite wood
Material thermal coefficient reaches 2.2016Wm-1·K-1。
Embodiment 2
(1) monomer pre-processes: 5g 6-aminocaprolc acid, mechanical stirring is added after 45g caprolactam is heated to 80 DEG C of meltings
30 minutes, obtain colourless transparent liquid；
(2) the pre- intercalation of graphite and swelling: by 2.5g, 400 mesh natural graphites are added in transparency liquid obtained by step (1), warp
Progress monomer obtains mixture suspension to the pre- intercalation of graphite and swelling within 450W ultrasonication 1.5 hours；
(3) in-situ polymerization is removed with graphite linings: applying mechanical stirring and in nitrogen protection to suspension is mixed obtained by step (2)
Under be warming up to 180 DEG C keep the temperature 1 hour, further heat up later to 250 DEG C keep the temperature 9 hours after natural cooling.
(4) product cleaning and drying: being washed 5 times after reaction product in step (3) is cooled to solid with 80 DEG C of hot water, it
Dry 24 hours are placed in 80 DEG C of electric heating constant-temperature blowing drying box to get graphene/nylon-6 composite material.
Graphene/nylon-6 composite material obtained by step (4) is placed in mold, after 220 DEG C, 5MPa hot pressing 2 minutes,
Then graphene/nylon-6 composite material print is made in room temperature pressure maintaining 10 minutes under the conditions of 20MPa；Detected the composite wood
Material thermal coefficient reaches 1.8406Wm-1·K-1。
Embodiment 3
(1) monomer pre-processes: 5g 6-aminocaprolc acid, mechanical stirring is added after 45g caprolactam is heated to 80 DEG C of meltings
30 minutes, obtain colourless transparent liquid；
(2) the pre- intercalation of graphite and swelling: by 0.5g, 400 mesh natural graphites are added in transparency liquid obtained by step (1), warp
Progress monomer obtains mixture suspension to the pre- intercalation of graphite and swelling within 450W ultrasonication 1 hour；
(3) in-situ polymerization is removed with graphite linings: applying mechanical stirring and in nitrogen protection to suspension is mixed obtained by step (2)
Under be warming up to 180 DEG C keep the temperature 1 hour, further heat up later to 250 DEG C keep the temperature 9 hours after natural cooling.
(4) product cleaning and drying: being washed 5 times after reaction product in step (3) is cooled to solid with 80 DEG C of hot water, it
Dry 24 hours are placed in 80 DEG C of electric heating constant-temperature blowing drying box to get graphene/nylon-6 composite material.
Graphene/nylon-6 composite material obtained by step (4) is placed in mold, after 220 DEG C, 5MPa hot pressing 2 minutes,
Then graphene/nylon-6 composite material print is made in room temperature pressure maintaining 10 minutes under the conditions of 20MPa；Detected the composite wood
Material thermal coefficient reaches 1.4298Wm-1·K-1。
Embodiment 4
(1) monomer pre-processes: 5g 6-aminocaprolc acid, mechanical stirring is added after 50g caprolactam is heated to 80 DEG C of meltings
30 minutes, obtain colourless transparent liquid；
(2) the pre- intercalation of graphite and swelling: by 5.5g, 325 mesh natural graphites are added in transparency liquid obtained by step (1), warp
Progress monomer obtains mixture suspension to the pre- intercalation of graphite and swelling within 500W ultrasonication 1.5 hours；
(3) in-situ polymerization is removed with graphite linings: applying mechanical stirring and in nitrogen protection to suspension is mixed obtained by step (2)
Under be warming up to 180 DEG C keep the temperature 1 hour, further heat up later to 250 DEG C keep the temperature 9 hours after natural cooling.
(4) product cleaning and drying: being washed 5 times after reaction product in step (3) is cooled to solid with 80 DEG C of hot water, it
Dry 24 hours are placed in 80 DEG C of electric heating constant-temperature blowing drying box to get graphene/nylon-6 composite material.
Graphene/nylon-6 composite material obtained by step (4) is placed in mold, after 220 DEG C, 5MPa hot pressing 2 minutes,
Then graphene/nylon-6 composite material print is made in room temperature pressure maintaining 10 minutes under the conditions of 20MPa；Detected the composite wood
Material thermal coefficient reaches 2.1582 Wm-1·K-1。
Embodiment 5
(1) monomer pre-processes: 5g 6-aminocaprolc acid, mechanical stirring is added after 50g caprolactam is heated to 80 DEG C of meltings
30 minutes, obtain colourless transparent liquid；
(2) the pre- intercalation of graphite and swelling: by 2.525g, 325 mesh natural graphites are added in transparency liquid obtained by step (1),
Through 450W ultrasonication 0.5 hour progress monomer to the pre- intercalation of graphite and swelling, mixture suspension is obtained；
(3) in-situ polymerization is removed with graphite linings: applying mechanical stirring and in nitrogen protection to suspension is mixed obtained by step (2)
Under be warming up to 180 DEG C keep the temperature 1 hour, further heat up later to 250 DEG C keep the temperature 9 hours after natural cooling.
(4) product cleaning and drying: being washed 5 times after reaction product in step (3) is cooled to solid with 80 DEG C of hot water, it
Dry 24 hours are placed in 80 DEG C of electric heating constant-temperature blowing drying box to get graphene/nylon-6 composite material.
Graphene/nylon-6 composite material obtained by step (4) is placed in mold, after 220 DEG C, 5MPa hot pressing 2 minutes,
Then graphene/nylon-6 composite material print is made in room temperature pressure maintaining 10 minutes under the conditions of 20MPa；Detected the composite wood
Material thermal coefficient reaches 1.7269Wm-1·K-1。
Embodiment 6
(1) monomer pre-processes: 5g 6-aminocaprolc acid, mechanical stirring is added after 45g caprolactam is heated to 80 DEG C of meltings
30 minutes, obtain colourless transparent liquid；
(2) cationic polymerization: in transparency liquid obtained by step (1), applying mechanical stirring and under nitrogen protection
It heats up 180 DEG C and reacts 1 hour, further heat up to 250 DEG C natural cooling after reacting 9 hours later；
(3) product cleaning and drying: being washed 5 times after reaction product in step (2) is cooled to solid with 80 DEG C of hot water, it
Dry 24 hours are placed in 80 DEG C of electric heating constant-temperature blowing drying box to get nylon-6.
Nylon-6 obtained by step (3) is placed in mold, through 220 DEG C, after 5 MPa hot pressing 2 minutes, then in 20 MPa items
Nylon-6 print is made in room temperature pressure maintaining 10 minutes under part；Being detected the material thermal conductivity is 0.3230Wm-1·K-1。
Embodiment 7
(1) monomer pre-processes: 5g 6-aminocaprolc acid, mechanical stirring is added after 45g caprolactam is heated to 80 DEG C of meltings
30 minutes, obtain colourless transparent liquid；
(2) cationic polymerization: in transparency liquid obtained by step (1), applying mechanical stirring and under nitrogen protection
It heats up 180 DEG C and reacts 1 hour, further heat up to 250 DEG C natural cooling after reacting 9 hours later；
(3) 5g is added into liquid obtained by step (2), 325 mesh natural graphites continue stirring 30 minutes；
(4) product cleaning and drying: being washed 5 times after reaction product in step (3) is cooled to solid with 80 DEG C of hot water, it
Dry 24 hours are placed in 80 DEG C of electric heating constant-temperature blowing drying box to get graphite/nylon-6 melt blended material.
Graphite/nylon-6 melt blended material obtained by step (4) is placed in mold, after 220 DEG C, 5MPa hot pressing 2 minutes,
Then graphite/nylon-6 melt blended material print is made in room temperature pressure maintaining 10 minutes under the conditions of 20MPa；Detected the composite wood
Material thermal coefficient is 0.8966Wm-1·K-1。
Graphite and nylon-6 individualism, graphene/nylon-in graphite/nylon-6 melt blended material as can be seen from Figure 2
Graphene layer distributed, nylon-6 are distributed between graphene layer in 6 composite materials, and graphene dispersion is uniform.
Graphite can be regarded as from structure to be formed by graphene stacking, therefore available by way of removing graphite
Graphene；Monomer molecule attraction is intercalation into natural graphite interlayer by special role, and causes home position polymerization reaction in interlayer,
It is moved using reaction heat and long-chain molecule, the removing of graphene and its evenly dispersed in polymeric matrix may be implemented, from
And nylon-6/graphene composite material is made in a step；The removing of graphene and its good dispersibility are then conducive to significantly mention
Rise the heating conduction of nylon-6 composite material；Preparation method of the present invention by caprolactam heating melting and is added as catalysis first
The 6-aminocaprolc acid of agent；After appropriate natural graphite is added, by ultrasonication and churned mechanically collective effect, oneself is realized
Swelling and pre- intercalation of the lactams to expanded graphite；Then carried out by the caprolactam that control reaction condition causes graphite layers
Home position polymerization reaction removes natural graphite while synthetic nylon -6 and is graphene and divides it uniformly in a polymer matrix
It dissipates, so that graphene/nylon-6 high-heat-conductive composite material be made；Compared to pure nylon-6 or graphite mixing filled nylon-6,
Thermal coefficient can promote 4.4 times or more, 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 nylon-6 synthesis, removing natural graphite is graphene, thus obtained graphene/
Nylon-6 high-heat-conductive composite material；Composite material heat filling graphene dispersion prepared by the present invention is uniform, preparation flow is short, at
This is low, preparation flow is short, control is simple, and the graphene/nylon-6 composite material prepared compared with existing preparation method is thermally conductive
Performance is good, and is suitable for commercially producing and applying；Can further expansion nylon series composite materials such as electronic apparatus,
The extensive use in the fields such as communication product, mechanical industry.
Claims (7)
1. a kind of graphene/nylon-6 composite material and preparation method thereof, which comprises the following steps:
(1) after caprolactam being heated to melting, 6-aminocaprolc acid is added, stirring until the reaction is complete, obtains pretreated
Caprolactam solution；Wherein the mass ratio of caprolactam and 6-aminocaprolc acid is 9:1~10:1；
(2) in the solution for obtaining graphite addition step (1), ultrasonication obtains mixture suspension；Wherein graphite and solution
Mass ratio be 1:100~1:10；
(3) suspension obtained by step (2) is warming up to 150~180 DEG C and keeps the temperature 1~2 hour, then heats to 200~260 DEG C of heat preservations 6
~9 as a child natural coolings；
(4) up to required graphene/nylon-6 composite material after the product washing that step (3) obtains is dry.
2. a kind of graphene/nylon-6 composite material and preparation method thereof according to claim 1, which is characterized 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, which is characterized in that the step
Suddenly heating 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, which is characterized 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, which is characterized in that the step
Suddenly apply stirring in (3) reaction process, and be passed through nitrogen protection.
6. a kind of graphene/nylon-6 composite material and preparation method thereof according to claim 1, which is characterized in that the step
Suddenly it is washed in (4) water washing 3~5 times using 80~100 DEG C.
7. a kind of graphene/nylon-6 composite material and preparation method thereof according to claim 1, which is characterized in that the step
Suddenly it is carried out under conditions of 80~100 DEG C in (4) using air dry oven, it is 18~24 hours dry.
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| 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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