CN107739504A - A kind of preparation method of graphene/nylon enhancing composite - Google Patents
A kind of preparation method of graphene/nylon enhancing composite Download PDFInfo
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- CN107739504A CN107739504A CN201711007680.XA CN201711007680A CN107739504A CN 107739504 A CN107739504 A CN 107739504A CN 201711007680 A CN201711007680 A CN 201711007680A CN 107739504 A CN107739504 A CN 107739504A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
Abstract
The invention discloses a kind of preparation method of graphene/nylon enhancing composite, comprise the following steps:(1) dry nylon (2) and Dispersion on surface processing is carried out to graphene with surfactant and coupling agent;(3) graphene after processing and nylon and heat stabilizer are added to extruding pelletization in double screw extruder after high-speed mixer and mixing, the particle of extrusion uses as master batch;(4) master batch, nylon, heat stabilizer and toughener are added to extruding pelletization in double screw extruder after high-speed mixer and mixing and prepare graphene/nylon enhancing composite;Graphene of the present invention/nylon enhancing composite has high intensity, excellent low-temperature flexibility, high-wearing feature, there is load capacity and the parts of relative motion available for automobile, center plate for lorry abrasion disc, wearing plate etc. is prepared, graphene/excellent combination property of nylon enhancing composite can reduce the breakage rate of parts, extend its service life, improve the car body safety in operation of automobile and railway freight-car;Therefore, the graphene that prepared by the inventive method/nylon enhancing composite has wide market application foreground.
Description
Technical field
The present invention relates to polymer/inorganic compound High performance nanometer composite material field, specifically, lived by surface
Property agent and coupling agent are surface-treated to graphene, are then borrowed nylon and graphene and other auxiliary agents with double screw extruder
Help mechanical external force and carry out melt blending, obtain a kind of preparation method of graphene/nylon enhancing composite.
Background technology
Nylon as engineering plastics has high mechanical strength, and coefficient of friction is low, self lubricity, shock absorption and sound-deadening properties
Good, excellent barrier, it is heat-resisting, wear-resistant, chemical proofing is good the advantages that, automobile industry, electronics can be widely used in
The field such as electrical communication field, film packaging field, military affairs and aerospace industry, track traffic industry;But nylon also has simultaneously
Have that water imbibition is big, it is sensitive to wet temp, and the shortcomings of influence dimensional stability, cryogenic property and electrical property.To adapt to industry hair
The demand of exhibition, the performance of nylon is improved by adding various auxiliary agents, as mechanical property, chemical property, electromagnetic performance,
The performances such as decay resistance, ageing-resistant performance, resistance to low temperature, wearability, hot property, anti-flammability, barrier, processability.
Graphene has unique structure, and intensity is high, specific surface area is big, chemical property is stable, excellent electrical and thermal conductivity
Can, the application field of graphene is gradually extended at present, the problem of easily reunion due to graphene, have impact on graphene in macromolecule
The application of Material Field, it is, thus, sought for suitable scattered and technology, enables graphene in high polymer material
It is preferably scattered, turn into the current technical issues that need to address to improve the combination property of material.
The content of the invention
The invention provides a kind of preparation method of graphene/nylon enhancing composite, by adding graphene to Buddhist nun
Imperial material carries out enhancing modification, while graphene can also reduce the water absorption rate and frictional resistance of nylon resin, and it is strong to improve material
Degree and cryogenic property;
For purpose as realization, in the inventive solutions, there is provided a kind of graphene/nylon activeness and quietness is compound
The preparation method of material, the graphene containing different graphene concentration/nylon enhancing composite wood can be obtained by adjusting addition
Material, this method is relative to situ aggregation method and solution mixing method, and this method is more suitable for industrialized production.In order to realize above-mentioned mesh
, the present invention adopts the following technical scheme that:
A kind of preparation method of graphene/nylon enhancing composite, comprises the following steps:
(1) nylon resin is put into 80-110 DEG C of baking oven and dries 4-6h.
(2) surfactant and coupling agent are added separately in graphene slurries, in ultrasonic device and high speed shear breast
Surfactant and coupling agent carry out Dispersion on surface processing, ultrasonic power 100-8000W, ultrasound to graphene respectively in change machine
Time is 10min-12h;Shear rate is 2000-12000r/min, time 1-2h, then carries out being dried under vacuum to constant weight,
Drying temperature is 80-100 DEG C;The percentage by weight of graphene solid content is 1-10% in graphene slurries, surfactant
Addition is the 0.1-1% of the percentage by weight of graphene solid content, and the addition of coupling agent is the weight of graphene solid content
The 0.5-2% of percentage.
(3) in the nylon for being 79.5-98.9% by percentage by weight, the graphene that percentage by weight is 1-20% is added,
0.1-0.5% heat stabilizer, double screw extruder is added after being well mixed on the high mixer that rotating speed is 500-7000r/min
Middle extruding pelletization prepares graphene/nylon master batch.
(4) in the nylon for being 39.5-98.9% by percentage by weight, 1-60% master batch is added, 0.1-0.5% heat is steady
Determine agent to stir in high mixer high speed, be then added to extruding pelletization in double screw extruder and prepare graphene/nylon enhancing again
Condensation material, extruder temperature control is for 180-310 DEG C, rotating speed 100-500r/min, and the material of extrusion is through cooling, pelletizing, so
4-6h is dried in 90 DEG C of baking ovens afterwards.
Nylon resin of the present invention is nylon 6, nylon66 fiber, nylon 46, NYLON610, nylon 612, nylon 11, nylon
12nd, at least one of nylon 1010, nylon 1212, nylon 6T, nylon 9 T, nylon 10T.
Surfactant of the present invention includes 1-METHYLPYRROLIDONE, gamma-butyrolacton, 1,3- dimethyl 2- imidazolines
At least one of ketone, 2- propyl alcohol, sodium taurocholate, lauryl sodium sulfate, neopelex, polyvinyl alcohol.
Coupling agent of the present invention is silane coupler, at least one of titanate coupling agent, silane coupler bag
Containing γ (2,3- glycidoxy) propyl trimethoxy silicane, gamma-aminopropyl-triethoxy-silane, N- (aminoethyls of β mono-)-γ-
Aminopropyl front three (second) TMOS, γ-(methacryloxypropyl) propyl trimethoxy silicane, γ-diethylenetriamine propylene three
The silane couplers such as Ethoxysilane;Titanate coupling agent includes the oleic acid acyloxy of isopropyl two (dioctyl phosphoric acid acyloxy) titanium
Acid esters, isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters, three iso stearate isopropyl titanates, double (two octyloxy pyrophosphoric acids
Ester group) titanate coupling agent such as ethylene titanate esters, tetra isopropyl two (dioctyl phosphito acyloxy) titanate esters.
Graphene slurries of the present invention are graphene slurries, graphene oxide slurries, biomass graphene slurries, stone
One or more of mixing in the slurries of black ene derivative, graphene film footpath≤5.0 μm, thickness≤1.0nm.
Heat stabilizer of the present invention is 3,5- di-t-butyl 4- hydroxy benzenes propionyl-hexamethylene diamine, phosphorous acid three (2,4- bis-
Tert-butyl benzene) ester, four [β-(3,5- di-t-butyl 4- hydroxy phenyls) propionic acid] pentaerythritol esters, one kind in cuprous iodide or more
Kind.
The method have the characteristics that:Graphene is preferably disperseed in nylon through a variety of mechanical external forces, pass through surface
Activating agent and coupling agent are surface-treated to graphene, graphene and nylon is had more preferable interface cohesion, surfactant
The aggregation of graphene can be prevented, coupling agent, which improves graphene and the interface cohesion of nylon, prevents graphene from assembling, and improves stone
The compatibility of black alkene and nylon, by refining the process of graphene and nylon blending, using high speed shear active force by graphene
Evenly spreading in nylon and obtain graphene/nylon enhancing composite of excellent performance, this method step is simple, easy to operate,
It is more suitable for industrialized production.
Embodiment
With reference to embodiment, the invention will be further described, rather than limitation the scope of the present invention.
Embodiment 1
A kind of preparation method of graphene of the present embodiment/nylon enhancing composite, comprises the following steps:
(1) nylon resin is put into 100 DEG C of baking oven and dries 4h;
(2) by surfactant 1-METHYLPYRROLIDONE and coupling agent γ (2,3- glycidoxy) propyl trimethoxy silicon
Alkane is added separately in graphene slurries, and surfactant and coupling agent are right respectively in ultrasonic device and high-speed shearing emulsion machine
Graphene carries out decentralized processing, and ultrasonic power 6000W, ultrasonic time 1.5h, shear rate 8000r/min, the time is
2h, then carry out being dried under vacuum to constant weight, drying temperature is 80 DEG C;The percentage by weight of graphene solid content in graphene slurries
For 10%, the addition of surfactant is the 0.5% of the percentage by weight of graphene solid content, and the addition of coupling agent is stone
The 1% of the percentage by weight of black alkene solid content.
(3) in the nylon 6 for being 74.6% by percentage by weight, the graphene after the processing of addition 25%, 0.4% 3,5- bis-
Tertiary butyl-4-hydroxy phenylpropyl alcohol acyl-hexamethylene diamine heat stabilizer, added after being well mixed on the high mixer that rotating speed is 5500r/min
Extruding pelletization prepares graphene/nylon master batch in double screw extruder.
(4) in the nylon 6 for being 97.7% by percentage by weight, 2% master batch, 0.3% phosphorous acid three (2,4- bis- are added
Tert-butyl benzene) ester heat stabilizer high mixer high speed stir, be then added to extruding pelletization in double screw extruder and prepare stone
Black alkene/nylon enhancing composite, extruder temperature control is for 210-240 DEG C, rotating speed 100-500r/min, the material of extrusion
Through cooling, pelletizing, 4-6h is then dried in 90 DEG C of baking ovens.
Test result is:Tensile strength >=80MPa, bending strength >=95MPa, compressive strength >=120MPa.
Embodiment 2
A kind of preparation method of graphene of the present embodiment/nylon enhancing composite, comprises the following steps:
(1) nylon resin is put into 100 DEG C of baking oven and dries 4h;
(2) by surfactant 1-METHYLPYRROLIDONE and coupling agent γ (2,3- glycidoxy) propyl trimethoxy silicon
Alkane is added separately in graphene slurries, and surfactant and coupling agent are right respectively in ultrasonic device and high-speed shearing emulsion machine
Graphene carries out decentralized processing, ultrasonic power 6000W, ultrasonic time 1.5h;Shear rate is 8000r/min, and the time is
2h, then carry out being dried under vacuum to constant weight, drying temperature is 80 DEG C;The percentage by weight of graphene solid content in graphene slurries
For 10%, the addition of surfactant is the 0.5% of the percentage by weight of graphene solid content, and the addition of coupling agent is stone
The 1% of the percentage by weight of black alkene solid content.
(3) in the nylon 6 for being 89.6% by percentage by weight, the graphene after the processing of addition 10%, 0.4% 3,5- bis-
Tertiary butyl-4-hydroxy phenylpropyl alcohol acyl-hexamethylene diamine heat stabilizer, added after being well mixed on the high mixer that rotating speed is 5500r/min
Extruding pelletization prepares graphene/nylon master batch in double screw extruder.
(4) in the nylon 6 for being 94.7% by percentage by weight, 5% master batch, 0.3% phosphorous acid three (2,4- bis- are added
Tert-butyl benzene) ester heat stabilizer high mixer high speed stir, be then added to extruding pelletization in double screw extruder and prepare stone
Black alkene/nylon activeness and quietness composite, extruder temperature control for 210-240 DEG C, rotating speed 100-500r/min, extrusion
Then material dries 4-6h through cooling, pelletizing in 90 DEG C of baking ovens.
Test result is:Tensile strength >=82MPa, bending strength >=95MPa, compressive strength >=125MPa.
Description of the invention and application are illustrative, are not wishing to limit the scope of the invention in above-described embodiment,
Therefore, the present invention is not limited by the present embodiment, what any technical scheme obtained using equivalence replacement was protected in the present invention
In the range of.
Claims (6)
1. the preparation method of a kind of graphene/nylon enhancing composite, it is characterised in that comprise the following steps:
(1) nylon resin is put into 80-110 DEG C of baking oven and dries 4-6h.
(2) surfactant and coupling agent are added separately in graphene slurries, in ultrasonic device and high-speed shearing emulsion machine
Middle surfactant and coupling agent carry out Dispersion on surface processing, ultrasonic power 100-8000W, ultrasonic time to graphene respectively
For 10min-12h;Shear rate is 2000-12000r/min, time 1-2h, then carries out being dried under vacuum to constant weight, is dried
Temperature is 80-100 DEG C;The percentage by weight of graphene solid content is 1-10% in graphene slurries, the addition of surfactant
The 0.1-1% of the percentage by weight for graphene solid content is measured, the addition of coupling agent is the weight percent of graphene solid content
The 0.5-2% of ratio.
(3) in the nylon for being 79.5-98.9% by percentage by weight, the graphene that percentage by weight is 1-20%, 0.1- are added
0.5% heat stabilizer, add in double screw extruder and squeeze after being well mixed on the high mixer that rotating speed is 500-7000r/min
Go out granulation and prepare graphene/nylon master batch.
(4) in the nylon for being 39.5-98.9% by percentage by weight, 1-60% master batch, 0.1-0.5% heat stabilizer are added
Stirred in high mixer high speed, be then added to extruding pelletization in double screw extruder and prepare graphene/nylon enhancing composite wood
Material, extruder temperature control is for 180-310 DEG C, rotating speed 100-500r/min, and the material of extrusion is through cooling, pelletizing, Ran Hou
4-6h is dried in 90 DEG C of baking ovens.
A kind of 2. preparation method of graphene as claimed in claim 1/nylon enhancing composite, it is characterised in that:Step
(1) nylon resin described in is nylon 6, nylon66 fiber, nylon 46, NYLON610, nylon 612, nylon 11, nylon 12, nylon
1010th, at least one of nylon 1212, nylon 6T, nylon 9 T, nylon 10T.
A kind of 3. preparation method of graphene/nylon enhancing composite according to claim 1, it is characterised in that:Step
(2) surfactant described in includes 1-METHYLPYRROLIDONE, gamma-butyrolacton, DMI, 2- third
At least one of alcohol, sodium taurocholate, lauryl sodium sulfate, neopelex, polyvinyl alcohol.
A kind of 4. preparation method of graphene/nylon enhancing composite according to claim 1, it is characterised in that:Step
(2) coupling agent described in is at least one of silane coupler, titanate coupling agent, and silane coupler includes γ (2,3-
Glycidoxy) propyl trimethoxy silicane, gamma-aminopropyl-triethoxy-silane, N- (aminoethyls of β mono-)-γ-aminopropyl front three
(second) TMOS, γ-(methacryloxypropyl) propyl trimethoxy silicane, γ-diethylenetriamine propylene triethoxysilane
Deng silane coupler;Titanate coupling agent includes the oleic acid acyloxy of isopropyl two (dioctyl phosphoric acid acyloxy) titanate esters, isopropyl
Base three (dioctyl phosphoric acid acyloxy) titanate esters, three iso stearate isopropyl titanates, double (two octyloxy pyrophosphoric acid ester groups) ethylenes
The titanate coupling agents such as titanate esters, tetra isopropyl two (dioctyl phosphito acyloxy) titanate esters.
A kind of 5. preparation method of graphene/nylon enhancing composite according to claim 1, it is characterised in that:Step
(2) the graphene slurries described in are graphene slurries, graphene oxide slurries, biomass graphene slurries, graphene derive
One or more of mixing in the slurries of thing, graphene film footpath≤5.0 μm, thickness≤1.0nm.
A kind of 6. preparation method of graphene/nylon enhancing composite according to claim 1, it is characterised in that:Step
(3) heat stabilizer and described in step (4) is 3,5- di-t-butyl -4- hydroxy benzenes propionyl-hexamethylene diamine, phosphorous acid three (2,4-
Di-tert-butyl) ester, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, one kind in cuprous iodide
It is or a variety of.
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Cited By (6)
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CN108329532A (en) * | 2018-03-26 | 2018-07-27 | 山东冬瑞高新技术开发有限公司 | A kind of bioengineering plastics and preparation method thereof |
CN109054365A (en) * | 2018-07-11 | 2018-12-21 | 青岛万林橡塑科技有限公司 | A kind of preparation method of solid phase graphene nylon Heat Conduction Material |
CN109898334A (en) * | 2019-03-21 | 2019-06-18 | 安徽工程大学 | A kind of thermally conductive dipped canvas and preparation method thereof |
CN110628213A (en) * | 2019-11-08 | 2019-12-31 | 中北大学 | PA11/RGO composite material and preparation method thereof |
CN112126124A (en) * | 2020-08-24 | 2020-12-25 | 安徽未来表面技术有限公司 | Graphene material and preparation method thereof |
CN112724666A (en) * | 2019-10-14 | 2021-04-30 | 上海杰事杰新材料(集团)股份有限公司 | graphene/PA 10T nanocomposite and preparation method thereof |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108329532A (en) * | 2018-03-26 | 2018-07-27 | 山东冬瑞高新技术开发有限公司 | A kind of bioengineering plastics and preparation method thereof |
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CN109898334A (en) * | 2019-03-21 | 2019-06-18 | 安徽工程大学 | A kind of thermally conductive dipped canvas and preparation method thereof |
CN109898334B (en) * | 2019-03-21 | 2021-05-04 | 安徽工程大学 | Heat-conducting impregnated canvas and preparation method thereof |
CN112724666A (en) * | 2019-10-14 | 2021-04-30 | 上海杰事杰新材料(集团)股份有限公司 | graphene/PA 10T nanocomposite and preparation method thereof |
CN110628213A (en) * | 2019-11-08 | 2019-12-31 | 中北大学 | PA11/RGO composite material and preparation method thereof |
CN110628213B (en) * | 2019-11-08 | 2021-10-22 | 中北大学 | PA11/RGO composite material and preparation method thereof |
CN112126124A (en) * | 2020-08-24 | 2020-12-25 | 安徽未来表面技术有限公司 | Graphene material and preparation method thereof |
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Application publication date: 20180227 |