CN109721812A - The preparation method and its device of a kind of graphene/conductive black composite material and application - Google Patents
The preparation method and its device of a kind of graphene/conductive black composite material and application Download PDFInfo
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- CN109721812A CN109721812A CN201910144610.1A CN201910144610A CN109721812A CN 109721812 A CN109721812 A CN 109721812A CN 201910144610 A CN201910144610 A CN 201910144610A CN 109721812 A CN109721812 A CN 109721812A
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Abstract
A kind of preparation method of graphene/conductive black composite material, it is therefore an objective to prevent agglomeration and dieseling；Method is that solid graphite alkene or graphene water system suspension are configured in graphene batch tank with water to the graphene suspension that mass percent is 10%-15%, disperses to form stable suspension by mechanical stirring or ultrasonic wave；Conductive black is added in stable graphene suspension to be granulated in water, is uniformly mixed and forms mixed liquor；It is added in wet granulator, the surface that cladding is adsorbed onto powdery conductive black forms graphene/wet particle of conductive black composite material；It is dry in roller drier to slough moisture, form graphene/conductive black composite material；This material can be used for producing cable semiconductive shieldin material；Preparation facilities includes graphene suspension system, is granulated water system, mixer, wet granulator, powdered carbon black storage tank, roller drier and tail-gas combustion stove.
Description
Technical field
The present invention relates to a kind of graphene/conductive black composite material and preparation method thereof and its devices and the composite material
Using.
Background technique
Medium and high voltage cable mainly uses the evenly dispersed addition conductive black in high molecular polymer with semiconductive shieldin material
The mode of equal materials is made, and is influenced by conductive black electric conductivity and thermal stability are bad, leads to the volume of semiconductive shieldin material
Resistivity index is higher thus not ideal enough to cable shield effect, to improve conductive black electric conductivity and thermal stability,
Graphene need to be added to improve electric conductivity.At present cable manufacturer or semiconductive shieldin material manufacturer by graphene,
Mixer is added in conductive black and other materials, is mixed a variety of materials by mechanism, graphene is due to its biggish ratio
Easily there is agglomeration along with interaction is easy to produce between lamella and lamella in surface area, it is difficult to and it is evenly dispersed, it makes
Improve at electric conductivity bad, while solid a variety of materials high-speed stirred heat is high, dieseling easily occurs, formed waste and
Security risk.
Summary of the invention
Object of the present invention is to overcome the shortcomings of above-mentioned prior art, providing one kind, can to prevent agglomeration and spontaneous combustion existing
The graphene of elephant/conductive black composite material and preparation method thereof and its device and composite material application.
A kind of graphene/conductive black composite material and preparation method thereof, it is characterized in that:
(1) solid graphite alkene or graphene water system suspension are configured to mass percent with water in graphene batch tank is
The graphene suspension of 10%-15% disperses to form stable suspension by mechanical stirring or ultrasonic wave；Graphene suspension is matched
Set hardness≤3 μm ol/l, the basicity≤3 μm ol/l with water；
(2) conductive black is added in stable graphene suspension to be granulated in water, is uniformly mixed by mixer and forms mixed liquor；
The conductive black is granulated hardness≤3 μm ol/l, the basicity≤3 μm ol/l of water；It is 1%- that graphene, which accounts for mixed liquor mass percent,
6%；Preferred graphene accounting is 1%-5%.
(3) above-mentioned mixed liquor is added in wet granulator, cladding is adsorbed onto the surface of powdery conductive black, in wet process
Pelletizer stirs under the action of tooth, forms graphene/wet particle of conductive black composite material；Powdery conductive black is stored up by powdered carbon black
Tank is added by airtight valve, and the ratio between powdery conductive black and granulation water are 1:1.
The tooth position of stirring, by its high-speed rotating mechanical stirring power, makes tiny powdered material in machine inside pelletizer
Continuous rotation realizes mixing, granulating, nodularization, densification etc., to achieve the purpose that granulation.
(4) moisture is sloughed in the wet particle of carbon black drying in roller drier, eventually forms graphene/conductive black composite wood
Material；The mass percent that graphene accounts for the composite material is 1%-6%；
In the suspension that graphene and water are mixed to form, add according to the ratio of the total mass percent 0.1%-0.5% of suspension
Enter dispersing agent, improves stability of suspension.Graphene suspension is added to conductive black by constant displacement pump and flowmeter and is granulated water
In, then by be granulated Water flow adjusting valve and be granulated water ga(u)ge be quantitatively adding graphene into conductive black.
Graphene/wet particle of conductive black composite material in roller drier with the hot fume from tail-gas combustion stove into
Row exchanges heat and sloughs moisture, and 150-300 DEG C of outlet temperature of roller drier carbon black.Preferred 150-250 DEG C of outlet temperature of carbon black.
The preferred concentration of the graphene suspension that the mass percent is 10%-15% is 10%-13%.The preparation
The preferred softened water of graphene suspension water.Disperse to form stable suspension by mechanical stirring or ultrasonic wave, can add
A certain proportion of dispersing agent, preferred dispersing agent are anionic surfactant, adding proportion 0.1-0.5%.
Pelletizer feed zone is added by hydraulic giant in the mixed liquor, and uniformly cladding is adsorbed onto the surface of powdered carbon black, shape
At graphene/conductive black composite material, graphene/conductive black composite material forms charcoal under the action of pelletizer stirs tooth
Black wet particle.The raw materials used in the present invention is commercially available.
Above method graphene produced/conductive black composite material DBP absorption value: 120-180 10-5m3/Kg、
N2 adsorption specific surface area: 40-80 103m2/ Kg, volatile matter :≤0.8%, heating loss :≤0.3%, particle average hardness 15-
21cN, ash content≤0.20%.
The application of above method graphene produced/conductive black composite material is for cable semi-conductive screen
Material, semiconductive shieldin material is according to the formula that mass unit part is counted: EVA100 parts of ethylene-vinyl acetate copolymer；Graphene/lead
Electric carbon black composite material 40-45 parts；5-8 parts of lubricant；0.1-0.3 parts of antioxidant；1.5-1.8 parts of crosslinking agent；Pass through mixer
It is kneaded, screw extruder is granulated to form semiconductive shieldin material, 20 DEG C of volume resistivities≤20 Ω cm；90 DEG C of volume resistivities
≤50Ω·cm.Semiconductive shieldin material forms the shielded layer of cable by extruder, and graphene/conductive black composite material exists
Conductive path is formed in shielded layer, improves semiconductive shieldin material electric conductivity.
Graphene used in the above method/conductive black composite material preparation facilities, including graphene suspension system, make
Grain water system, mixer, wet granulator, powdered carbon black storage tank, roller drier and tail-gas combustion stove；Being granulated water system includes
It is granulated water pump and is granulated waterpipe；Graphene suspension system includes graphene batch tank, constant displacement pump, flowmeter and suspension liquid pipe
Road；Graphene suspension system is connect by suspension pipeline with waterpipe is granulated, and constant displacement pump, flowmeter are successively mounted in suspension
On pipeline；Mixer is mounted on suspension pipeline and is granulated the rear of water pipe pipeline joint；Mixer by mixed liquor pipeline with it is wet
The connection of method pelletizer；Powdered carbon black storage tank is connect by airtight valve with wet granulator；Roller drier by blanking pipe with
Wet granulator connection；Tail-gas combustion stove is connect by flue with roller drier periphery fire-box；It is set on roller drier
There is graphene/conductive black composite material outlet.
The mixer is static mixer.It is sequentially arranged at mixer rear for adjusting mixed liquor on mixed liquor pipeline
The flowmeter and flow control valve of flow.
The positive effect of the present invention is that: be less prone to agglomeration, easily it is evenly dispersed, electric conductivity improve compared with
It is good, while solid a variety of materials high-speed stirred heat height can be effectively prevented and dieseling occur, form waste and safety
Hidden danger.Graphene forms stable system in water phase, improves graphene agglomeration, improves graphene dispersion effect,
It is formed in shielded layer and causes conductive path, improve electric conductivity, 90 DEG C of volume resistivity≤50 of cable semi-conductive shield material
Ω·cm；Graphene/conductive black disperses in water phase, without security risk.
Detailed description of the invention
Fig. 1 is graphene of the present invention/conductive black composite material preparation facilities structural schematic diagram；
In figure: 1. graphene batch tank, 2. constant displacement pump, 3. flowmeter, is 4. granulated water pump, 5. mixer, 6. flowmeter, 7. flow
Regulating valve, 8. powdered carbon black storage tank, 9. airtight valve, 10. wet granulator, roller drier, tail-gas combustion stove, fire-box,
Graphene/conductive black composite material outlet.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.
Embodiment 1
A kind of graphene/conductive black composite material and preparation method thereof is:
(1) solid graphite alkene is used, is configured to the graphene that mass percent is 10%-15% in graphene batch tank and softened water
Water system suspension adds the anionic surfactant of 0.1%-0.5% as dispersing agent, forms stable hang by mechanical stirring
Supernatant liquid.Wherein, there are two graphene batch tanks, one to open one standby.
(2) graphene suspension is added conductive black and is granulated in water by constant displacement pump, flowmeter, passes through flowmeter and flow
Regulating valve is quantitatively adding graphene, graphene accounting 1%-6%.Graphene is uniformly mixed with granulation water by mixer.
(3) mixed liquor is uniformly added into pelletizer feed zone by 3-6 branch hydraulic giant, and cladding is adsorbed onto the surface of powdered carbon black,
Graphene/conductive black composite material is formed, graphene/conductive black composite material is formed under the action of pelletizer stirs tooth
The wet particle of carbon black.
(4) the wet particle of carbon black exchanges heat in drying machine with from tail-gas combustion stove hot fume, sloughs moisture, carbon black goes out
150-300 DEG C of temperature of mouth.
Graphene used in the above method/conductive black composite material preparation facilities, including graphene suspension system, make
Grain water system, mixer 5., wet granulator 10., powdered carbon black storage tank 8., roller drier and tail-gas combustion stove；It is granulated
Water system include be granulated water pump 4. be granulated waterpipe；Graphene suspension system include graphene batch tank 1., constant displacement pump 2.,
Flowmeter 3. with suspension pipeline；Graphene suspension system by suspension pipeline with granulation waterpipe connect, constant displacement pump 2.,
Flowmeter is 3. successively on suspension pipeline；5. mixer is mounted on suspension pipeline and is granulated the rear of water pipe pipeline joint；
5. mixer passes through mixed liquor pipeline and 10. connect with wet granulator；Powdered carbon black storage tank 8. pass through airtight valve 9. with wet granulation
10. machine connects；10. roller drier is connect by blanking pipe with wet granulator；Tail-gas combustion stove passes through flue
It is connect with roller drier periphery fire-box；Roller drier is equipped with graphene/conductive black composite material outlet.
5. the mixer is static mixer.
Above method graphene produced/conductive black composite material DBP absorption value: 120-180 10-5m3/Kg、
N2 adsorption specific surface area: 40-80 103m2/ Kg, volatile matter :≤0.8%, heating loss :≤0.3%, particle average hardness 15-
21cN, ash content≤0.20%.
The application of above method graphene produced/conductive black composite material is for cable semi-conductive screen
Material, semiconductive shieldin material is according to the formula that mass unit part is counted: EVA100 parts of ethylene-vinyl acetate copolymer；Graphene/lead
Electric carbon black composite material 40-45 parts；5-8 parts of lubricant；0.1-0.3 parts of antioxidant；1.5-1.8 parts of crosslinking agent；Pass through mixer
It is kneaded, screw extruder is granulated to form semiconductive shieldin material, 20 DEG C of volume resistivities≤20 Ω cm；90 DEG C of volume resistivities
≤50Ω·cm.Semiconductive shieldin material forms the shielded layer of cable by extruder, and graphene/conductive black composite material exists
Conductive path is formed in shielded layer, improves semiconductive shieldin material electric conductivity.
Embodiment 2
A kind of graphene/conductive black composite material and preparation method thereof is:
(1) 10%-15% graphene water system suspension is used, graphene batch tank is added, is dispersed by mechanical stirring or ultrasonic wave
Stable suspension is formed, wherein graphene batch tank two, one to open one standby.
(2) graphene suspension is added conductive black and is granulated in water by constant displacement pump, flowmeter, passes through flowmeter and flow
Regulating valve is quantitatively adding graphene, graphene accounting 1%-6%.Graphene is uniformly mixed with granulation water by mixer.
(3) mixed liquor is uniformly added into pelletizer feed zone by 3-6 branch hydraulic giant, and cladding is adsorbed onto the surface of powdered carbon black,
Graphene/conductive black composite material is formed, graphene/conductive black composite material is formed under the action of pelletizer stirs tooth
The wet particle of carbon black.
(4) the wet particle of carbon black exchanges heat in drying machine with from tail-gas combustion stove hot fume, sloughs moisture, carbon black goes out
150-300 DEG C of temperature of mouth.
Graphene used in the above method/conductive black composite material preparation facilities is same as Example 1.
Above method graphene produced/conductive black composite material DBP absorption value: 120-180 10-5m3/Kg、
N2 adsorption specific surface area: 40-80 103m2/ Kg, volatile matter :≤0.8%, heating loss :≤0.3%, particle average hardness 15-
21cN, ash content≤0.20%.
Embodiment 3
A kind of graphene/conductive black composite material and preparation method thereof is:
(1) graphene water system suspension is used, the graphene aqueous solution of 10%-15% is configured in graphene batch tank and water, adopts
It uses the anionic surfactant of 0.1%-0.2% as dispersing agent, forms stable suspension by mechanical stirring；Wherein graphite
Alkene batch tank two, one to open one standby.
(2) graphene suspension is added conductive black and is granulated in water by constant displacement pump, flowmeter, passes through flowmeter and flow
Regulating valve is quantitatively adding graphene, graphene accounting 1%-6%.Graphene suspension is uniformly mixed with granulation water by mixer.
(3) mixed liquor is uniformly added into pelletizer feed zone by 3-6 branch hydraulic giant, and cladding is adsorbed onto the surface of powdered carbon black,
Graphene/conductive black composite material is formed, graphene/conductive black composite material is formed under the action of pelletizer stirs tooth
The wet particle of carbon black.
(4) the wet particle of carbon black exchanges heat in drying machine with from tail-gas combustion stove hot fume, sloughs moisture, carbon black goes out
150-250 DEG C of temperature of mouth.
Graphene used in the above method/conductive black composite material preparation facilities is same as Example 1.
Above method graphene produced/conductive black composite material DBP absorption value: 120-180 10-5m3/Kg、
N2 adsorption specific surface area: 40-80 103m2/ Kg, volatile matter :≤0.8%, heating loss :≤0.3%, particle average hardness 15-
21cN, ash content≤0.20%.
Claims (8)
1. a kind of graphene/conductive black composite material and preparation method thereof, it is characterized in that:
(1) solid graphite alkene or graphene water system suspension are configured to mass percent with water in graphene batch tank is
The graphene suspension of 10%-15% disperses to form stable suspension by mechanical stirring or ultrasonic wave；Graphene suspension is matched
Set hardness≤3 μm ol/l, the basicity≤3 μm ol/l with water；
(2) conductive black is added in stable graphene suspension to be granulated in water, is uniformly mixed by mixer and forms mixed liquor,
The conductive black is granulated hardness≤3 μm ol/l, the basicity≤3 μm ol/l of water；It is 1%- that graphene, which accounts for mixed liquor mass percent,
6%；
(3) above-mentioned mixed liquor is added in wet granulator, cladding is adsorbed onto the surface of powdery conductive black, in wet granulation
Machine forms graphene/wet particle of conductive black composite material under the action of stirring tooth；The mass ratio of powdery conductive black and mixed liquor
For 1:1；
(4) graphene/wet particle of conductive black composite material is dry in roller drier sloughs moisture, formation graphene/lead
Electric carbon black composite material；The mass percent that graphene accounts for the composite material is 1%-6%.
2. graphene as described in claim 1/conductive black composite material and preparation method thereof, it is characterized in that graphene is mixed with water
Graphene suspension is formed, dispersing agent is added according to the 0.1%-0.5% of graphene suspension gross mass percentage, improves suspension
Stability.
3. graphene as claimed in claim 1 or 2/conductive black composite material and preparation method thereof, it is characterized in that the roller is dry
Dry machine is exchanged heat by the hot fume from tail-gas combustion stove with graphene/wet particle of conductive black composite material and de- discharging the water pathogen
Point, 150-300 DEG C of outlet temperature of roller drier carbon black.
4. graphene as described in claim 1/conductive black composite material and preparation method thereof, it is characterized in that graphite produced
Alkene/conductive black composite material DBP absorption value: 120-180 10-5m3/ Kg, N2 adsorption specific surface area: 40-80 103m2/Kg、
Volatile matter :≤0.8%, heating loss :≤0.3%, particle average hardness 15-21cN, ash content≤0.20%.
5. graphene as described in claim 1/conductive black composite material preparation facilities, it is characterized in that outstanding including graphene
Supernatant liquid system is granulated water system, mixer, wet granulator, powdered carbon black storage tank, roller drier and tail-gas combustion stove；It makes
Grain water system includes being granulated water pump and granulation waterpipe；Graphene suspension system includes graphene batch tank, constant displacement pump, flow
Meter and suspension pipeline；Graphene suspension system by suspension pipeline with granulation waterpipe connect, constant displacement pump, flowmeter according to
It is secondary to be mounted on suspension pipeline；Mixer is mounted on suspension pipeline and is granulated the rear of water pipe pipeline joint；Mixer passes through mixed
Liquid pipe road is closed to connect with wet granulator；Powdered carbon black storage tank is connect by airtight valve with wet granulator；Roller drier is logical
Blanking pipe is crossed to connect with wet granulator；Tail-gas combustion stove is connect by flue with roller drier periphery fire-box；Rolling
Drum drier is equipped with graphene/conductive black composite material outlet.
6. graphene as claimed in claim 5/conductive black composite material preparation facilities, it is characterized in that the mixer is
Static mixer.
7. such as graphene described in claim 5 or 6/conductive black composite material preparation facilities, it is characterized in that mixing liquid pipe
The flowmeter and flow control valve for adjusting mixing flow quantity are sequentially arranged at mixer rear on road.
8. graphene as claimed in claim 1 or 5/conductive black composite material application, it is characterized in that for producing cable
With semiconductive shieldin material, semiconductive shieldin material is according to the formula that mass unit part is counted: ethylene-vinyl acetate copolymer EVA100
Part；Graphene/40-45 parts of conductive black composite material；5-8 parts of lubricant；0.1-0.3 parts of antioxidant；Crosslinking agent 1.5-1.8
Part；Its production method is by mixer mixing, and screw extruder is granulated to form semiconductive shieldin material, and semiconductive shieldin material passes through
Extruder forms the shielded layer of cable, and graphene/conductive black composite material forms conductive logical in the semi-conductive screen bed of material
Road improves semiconductive shieldin material electric conductivity；20 DEG C of volume resistivities of the semiconductive shieldin material≤20 Ω cm；90 DEG C of volume electricity
Resistance rate≤50 Ω cm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110330010A (en) * | 2019-07-09 | 2019-10-15 | 杭州高烯科技有限公司 | A kind of efficiently graphene-based conductive additive and preparation method thereof |
| CN111171606A (en) * | 2019-12-30 | 2020-05-19 | 青岛科技大学 | Graphene-carbon black composite granules and preparation method and application thereof |
| CN111303526A (en) * | 2020-04-02 | 2020-06-19 | 成都鑫成鹏高分子科技股份有限公司 | Multilayer graphene modified semiconductive shielding material and preparation method thereof |
| CN112625342A (en) * | 2020-12-08 | 2021-04-09 | 广东聚石科技研究有限公司 | Graphene modified plastic and preparation method and application thereof |
| CN112898805A (en) * | 2021-01-21 | 2021-06-04 | 东莞市泰恩斯线缆有限公司 | Cable coating paint, cable preparation method and cable prepared by method |
| CN113150487A (en) * | 2021-02-07 | 2021-07-23 | 南方电网科学研究院有限责任公司 | Preparation method of thermoplastic shielding material |
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| CN107474376A (en) * | 2017-09-12 | 2017-12-15 | 哈尔滨理工大学 | A kind of cable semi-conductive shielding material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110330010A (en) * | 2019-07-09 | 2019-10-15 | 杭州高烯科技有限公司 | A kind of efficiently graphene-based conductive additive and preparation method thereof |
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| CN112898805A (en) * | 2021-01-21 | 2021-06-04 | 东莞市泰恩斯线缆有限公司 | Cable coating paint, cable preparation method and cable prepared by method |
| CN113150487A (en) * | 2021-02-07 | 2021-07-23 | 南方电网科学研究院有限责任公司 | Preparation method of thermoplastic shielding material |
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