CN105131408A - Graphene semiconductor shield material - Google Patents
Graphene semiconductor shield material Download PDFInfo
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- CN105131408A CN105131408A CN201510439101.3A CN201510439101A CN105131408A CN 105131408 A CN105131408 A CN 105131408A CN 201510439101 A CN201510439101 A CN 201510439101A CN 105131408 A CN105131408 A CN 105131408A
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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
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention relates to a shield material of high-voltage electrical cables and particularly relates to a graphene semiconductor shield material. The raphene semiconductor shield material is prepared from graphene nano sheets and ethylene-vinyl acetate and is prepared through the following steps: preparing a uniformly-dispersed graphene nano sheets (GR) water solution; adding an ethylene-vinyl acetate (EVA) emulsion with stirring; mixing the two liquids and performing flocculation to obtain a GR/EVA solid; filtering and washing the GR/EVA solid to neutralization with deionized water; vacuum freeze-drying the GR/EVA solid to prepare GR/EVA mother rubber; fully mixing the GR/EVA mother rubber in a double-roller open mill and treating the mother rubber with a vulcanizing agent; and performing moulding on a plate vulcanization machine to obtain the graphene semiconductor shield material. The preparation process is simple, is low in cost and energy consumption and is easy to control. The graphene semiconductor shield material is low in density, is excellent in semiconduction performance, is high in pressure resistance and tensile strength, is ultra-smooth and water tree-resistant, and is an excellent shield material of the middle- and high-voltage electrical cables.
Description
[technical field]
The present invention relates to a kind of shielding material of high voltage power cable, specifically relate to a kind of graphene semiconductor shielding material.
[background technology]
Graphene is by SP
2carbon atom close-packed arrays a kind of carbon simple substance with bi-dimensional cellular shape lattice structure together of hybrid form, has started unprecedented research boom due to performances such as the chemical structure of its uniqueness, the specific surface area of super large and impayable electricity, mechanics, calorifics in the field of compound material of new energy materials (energy storage material, ultracapacitor, solar cell etc.), photocatalyst material, biomaterial and each quasi-tradition.
Ethylene-vinyl acetate, contracting claims EVA, is by ethene and vinyl acetate copolymerized and obtained thermoplastic resin, and it and many materials have bonds well performance, and it is pliable and tough and have elasticity, can be used as sole sealed strip, foam plastic product and power cable goods etc.
Graphene and EVA material all can be applicable to improve power cable product properties, the achievement in research of current polymer/graphene composite material emerges in an endless stream, and Graphene is increased body as new high-performance can bring many-sided performances such as mechanics, electricity, calorifics and tribology to get a promotion for polymer composites.Its preparation method is mainly situ aggregation method, melt-blending process and emulsion hybrid system.
Original graphite is oxidized by melt-blending process usually, makes Graphene, with polymkeric substance blended obtained matrix material in the molten state through peeling off and reducing.Graphene and polymkeric substance can be prepared respectively in melt blending, therefore the size of Graphene and form controlled, but Graphene not easily disperses in polymeric matrix, poor with the interface interaction of polymkeric substance.Unstable in the molten state by the organic group in the Graphene of chemical modification, can not melt-blending process be applied to.The Graphene that current melt-blending process adopts is obtained by thermal reduction mostly, and the density of this Graphene is less, usually also can increase the difficulty of melting mixing.
Situ aggregation method is mixed with polymer monomer by Graphene, adds initiator initiation reaction, finally obtained matrix material.Graphene uniform can be dispersed in polymeric matrix by situ aggregation method, and shortcoming is that the viscosity of the polymkeric substance adding Graphene (or graphene oxide) increases, and makes polyreaction become complicated.
Emulsion hybrid system utilizes graphene oxide in water, have good dispersiveness, the aqueous liquid dispersion of graphene oxide can be mixed with polymer latex, prepares Graphene/polymer composites by reduction.Also tensio-active agent can be adopted to carry out surface modification to Graphene, improve its dispersiveness in water, be then mixed with matrix material with latex.This method can avoid the harm of organic solvent, the polymer composites of obtained high conduction performance.
In solution blended process, usually first prepare graphene oxide, the dispersion liquid that modification obtains can disperseing in organic solvent is carried out to it, obtain Graphene by reduction, then carry out solution blending with polymkeric substance and prepare Graphene/polymer composites.The advantage of solution mixing method is that the preparation of Graphene (or graphene oxide) and the synthesis of polymkeric substance are carried out respectively, can control size and the form of Graphene, and Graphene ratio is easier to dispersion.Shortcoming needs with an organic solvent, harm environment, and when adopting local reduction way, the difference due to type of polymer and reductive agent may cause the degraded of polymkeric substance.
But the prior aries such as a kind of graphene oxide nanobelt/polar rubber reported, graphene nanobelt/rubber composite only report mechanical property and the conductivity of same kind material, lack about specializing in Graphene and EVA material connected applications in the report of power cable goods correlation technique.Therefore the shield semiconductors material that shielding material in a kind of high-tension cable is provided is needed, to meet the needs of prior art.
[summary of the invention]
A kind of graphene semiconductor is the object of the present invention is to provide to shield material, with graphene nanometer sheet and ethylene-vinyl acetate for main raw material synthesizing graphite alkene shield semiconductors material, graphene semiconductor shielding material density provided by the invention is low, semiconduction superior performance, withstand voltage height, tensile strength are high, smooth and water-fast tree, can apply widely and cable screen material, the fields such as anti-electrostatic, have huge application prospect.
The present invention is by the following technical solutions for achieving the above object:
The invention provides a kind of graphene semiconductor shielding material, graphene semiconductor shielding material is made up of graphene nanometer sheet and ethylene-vinyl acetate, and graphene nanometer sheet accounts for 0.5 ~ 30% of shielding material mass percent.
In graphene semiconductor shielding material provided by the invention, graphene nanometer sheet accounts for 1 ~ 10% of shielding material mass percent.
In graphene semiconductor shielding material provided by the invention, graphene nanometer sheet accounts for 1.5 ~ 3.3% of shielding material mass percent.
Present invention also offers the preparation method of a kind of graphene semiconductor shielding material, comprise the steps:
1) frequency is 20 ~ 25kHz, power is the aqueous solution 15-30min that 70 ~ 90% times supersound process graphene nanometer sheets are made into;
2) under 300 ~ 500rpm speed, ethylene-vinyl acetate emulsion is added step 1) graphene solution in stir 30 ~ 60min, obtain cotton-shaped compound;
3) with compound described in deionized water rinsing, filter, vacuum lyophilization, obtain the masterbatch of graphene semiconductor shielding material;
4) open refining mixing 10 ~ 15h, 160 ~ 180 DEG C, pressure be 8 ~ 15MPa under vulcanisation step 3) the masterbatch 8 ~ 12min of gained, obtain graphene semiconductor shielding material.
Preparation method's step 1 provided by the invention) in, the concentration of graphene solution is 5 ~ 20g/L.
Preparation method's step 3 provided by the invention) in, compound is extremely neutral with deionized water rinsing.
Preparation method's step 3 provided by the invention) in, freezing temp is-50 ~-15 DEG C, and the time is 3 ~ 5day, vacuum tightness < 10Pa.
Preparation method's step 4 provided by the invention) in, curing temperature is 170 ~ 175 DEG C, and curing time is 10 ~ 12min, and sulfide stress is 8 ~ 12MPa.
With immediate prior art ratio, technical scheme provided by the invention has following beneficial effect:
1, graphene semiconductor provided by the invention shielding material has high, the smooth and characteristics such as water-fast tree of withstand voltage height, tensile strength;
2, the shielding material density that obtains of the present invention is lower, and resistivity reduces to have superior semiconducting behavior;
3, preparation method of the present invention is simple, processing ease, cost are low, energy consumption is low, is easy to control, and can be mass.
[accompanying drawing explanation]
Fig. 1 is the profile scanning electromicroscopic photograph of Graphene/ethylene-vinyl acetate shield semiconductors material, show the graphene nanometer sheet that technical scheme provides and ethylene-vinyl acetate interface cohesion good.
[embodiment]
With each embodiment, the present invention is described in further details below.
Embodiment 1 prepares Graphene/ethylene-vinyl acetate shield semiconductors material
With deionized water, 5g graphene nanometer sheet is settled to 3000ml, ultrasonic frequency be 25kHz, power processes 20min under being 80% condition, then the ethylene-vinyl acetate solution just adding 495g is stirred on limit, stir speed (S.S.) is 350r/min, churning time is 30min, and filtration washing obtains neutral cotton-shaped compound; Lyophilize process 3day at-50 DEG C, obtains masterbatch subsequently; By dried masterbatch through two roller mill mixing 10h.Then carry out sulfidization molding: curing temperature 160 DEG C, curing time 8min, sulfide stress 8MPa, obtain Graphene/ethylene-vinyl acetate shield semiconductors material, its performance is as shown in table 1, productive rate 90%.
Embodiment 2 prepares Graphene/ethylene-vinyl acetate shield semiconductors material
With deionized water, 15g graphene nanometer sheet is settled to 3000ml, ultrasonic frequency be 25kHz, power processes 20min under being 80% condition, then the ethylene-vinyl acetate solution just adding 485g is stirred on limit, stir speed (S.S.) is 350r/min, churning time is 30min, and filtration washing obtains neutral cotton-shaped compound; Lyophilize process 3day at-15 DEG C, obtains masterbatch subsequently; By dried masterbatch through two roller mill mixing 10h.Then carry out sulfidization molding: curing temperature 160 DEG C, curing time 8min, sulfide stress 8MPa, obtain Graphene/ethylene-vinyl acetate shield semiconductors material, its performance is as shown in table 1, productive rate 91%.
Table 1 is the Performance comparision of embodiment 1 and embodiment 2 Graphene of different content under same experimental conditions, can find out that Graphene content is increased to 3.0wt% from 1.0wt%, the mechanical properties such as its tensile strength, elongation at break, shore hardness A are basicly stable constant, but the density of shielding material reduces, 20 DEG C of volume specific resistances reduce 28.5%, and improved performance is remarkable.
The performance data of table 1 Graphene/ethylene-vinyl acetate shield semiconductors material
| Sample sequence number | Embodiment 1 | Embodiment 2 |
| Graphene content | 1.0wt％ | 3.0wt％ |
| Tensile strength | 11.2Mpa | 12.4Mpa |
| Elongation at break | 302％ | 305％ |
| Shore hardness A | 83 | 82 |
| 20 DEG C of volume specific resistances | 31.6Ω·cm | 22.6Ω·cm |
| Density | 1.12 | 1.11 |
Embodiment 3 prepares Graphene/ethylene-vinyl acetate shield semiconductors material
With deionized water, 25g graphene nanometer sheet is settled to 3000ml, ultrasonic frequency be 25kHz, power processes 30min under being 85% condition, then the ethylene-vinyl acetate solution just adding 475g is stirred on limit, stir speed (S.S.) is 350r/min, churning time is 30min, and filtration washing obtains neutral cotton-shaped compound; Lyophilize process 5day at interval-50 DEG C of freezing temp, obtains masterbatch subsequently; By dried masterbatch through two roller mill mixing 12h.Then carry out sulfidization molding: curing temperature 180 DEG C, curing time 10min, sulfide stress 10MPa, obtain Graphene/ethylene-vinyl acetate shield semiconductors material, productive rate 93%.
Embodiment 4 prepares Graphene/ethylene-vinyl acetate shield semiconductors material
With deionized water, 25g graphene nanometer sheet is settled to 3000ml, ultrasonic frequency be 25kHz, power processes 50min under being 90% condition, then the ethylene-vinyl acetate solution just adding 475g is stirred on limit, stir speed (S.S.) is 350r/min, churning time is 30min, and filtration washing obtains neutral cotton-shaped compound; Lyophilize process 5day at-50 DEG C, obtains masterbatch subsequently; By dried masterbatch through two roller mill mixing 15h.Then carry out sulfidization molding: curing temperature 170 DEG C, curing time 12min, sulfide stress 12Mpa, obtain Graphene/ethylene-vinyl acetate shield semiconductors material, productive rate 88%.
Embodiment 5 prepares Graphene/ethylene-vinyl acetate shield semiconductors material
With deionized water, 50g graphene nanometer sheet is settled to 3000ml, ultrasonic frequency be 25kHz, power processes 30min under being 90% condition, then the ethylene-vinyl acetate solution just adding 450g is stirred on limit, stir speed (S.S.) is 350r/min, churning time is 30min, and filtration washing obtains neutral cotton-shaped compound; Lyophilize process 4day at-50 DEG C, obtains masterbatch subsequently; By dried masterbatch through two roller mill mixing 12h, then carry out sulfidization molding, curing temperature 180 DEG C, sulfuration 8min, sulfide stress 12MPa, obtain Graphene/ethylene-vinyl acetate shield semiconductors material, productive rate 95%.
Embodiment 6 prepares Graphene/ethylene-vinyl acetate shield semiconductors material
With deionized water, 16g graphene nanometer sheet is settled to 3000ml, ultrasonic frequency be 25kHz, power processes 30min under being 90% condition, then the ethylene-vinyl acetate solution just adding 484g is stirred on limit, stir speed (S.S.) is 350r/min, churning time is 30min, and filtration washing obtains neutral cotton-shaped compound; Lyophilize process 4day at-50 DEG C, obtains masterbatch subsequently; By dried masterbatch through two roller mill mixing 12h.Then carry out sulfidization molding: curing temperature 180 DEG C, curing time 8min, sulfide stress 12MPa, obtain Graphene/ethylene-vinyl acetate shield semiconductors material, productive rate 95%.
Embodiment 7 prepares Graphene/ethylene-vinyl acetate shield semiconductors material
With deionized water, 8g graphene nanometer sheet is settled to 3000ml, ultrasonic frequency be 25kHz, power processes 30min under being 90% condition, then the ethylene-vinyl acetate solution just adding 492g is stirred on limit, stir speed (S.S.) is 350r/min, churning time is 30min, and filtration washing obtains neutral cotton-shaped compound; Lyophilize process 4day at-50 DEG C, obtains masterbatch subsequently; By dried masterbatch through two roller mill mixing 12h.Then carry out sulfidization molding: curing temperature 180 DEG C, curing time 8min, sulfide stress 12MPa, obtain Graphene/ethylene-vinyl acetate shield semiconductors material, productive rate 92%.
Embodiment 8 prepares Graphene/ethylene-vinyl acetate shield semiconductors material
With deionized water, 5g graphene nanometer sheet is settled to 3000ml, ultrasonic frequency be 25kHz, power processes 30min under being 90% condition, then the ethylene-vinyl acetate solution just adding 495g is stirred on limit, stir speed (S.S.) is 350r/min, churning time is 30min, and filtration washing obtains neutral cotton-shaped compound; Lyophilize process 4day at-50 DEG C, obtains masterbatch subsequently; By dried masterbatch through two roller mill mixing 12h.Then carry out sulfidization molding: curing temperature 180 DEG C, curing time 8min, sulfide stress 12MPa, obtain Graphene/ethylene-vinyl acetate shield semiconductors material.
Embodiment 9 prepares Graphene/ethylene-vinyl acetate shield semiconductors material
With deionized water, 50g graphene nanometer sheet is settled to 3000ml, ultrasonic frequency be 25kHz, power processes 30min under being 90% condition, then the ethylene-vinyl acetate solution just adding 450g is stirred on limit, stir speed (S.S.) is 350r/min, churning time is 30min, and filtration washing obtains neutral cotton-shaped compound; Lyophilize process 4day at-50 DEG C, obtains masterbatch subsequently; By dried masterbatch through two roller mill mixing 12h.Then carry out sulfidization molding: curing temperature 180 DEG C, curing time 8min, sulfide stress 12MPa, obtain Graphene/ethylene-vinyl acetate shield semiconductors material.
The Graphene shielding material density that the present invention obtains reduces, and 20 DEG C of lower volume resistivity reduce 28.5%, and semiconducting behavior significantly improves.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; those of ordinary skill in the field are to be understood that; can modify to the specific embodiment of the present invention with reference to above-described embodiment or equivalent replacement; these do not depart from any amendment of spirit and scope of the invention or equivalent replacement, and it all should be encompassed within claims of the present invention.
Claims (8)
1. a graphene semiconductor shielding material, is characterized in that described graphene semiconductor shielding material is made up of graphene nanometer sheet and ethylene-vinyl acetate, and graphene nanometer sheet accounts for 0.5 ~ 30% of described shielding material mass percent.
2. graphene semiconductor shielding material according to claim 1, is characterized in that graphene nanometer sheet accounts for 1 ~ 10% of described shielding material mass percent.
3. graphene semiconductor shielding material according to claim 1, is characterized in that graphene nanometer sheet accounts for 1.5 ~ 3.3% of described shielding material mass percent.
4. a preparation method for the graphene semiconductor shielding material as described in any one of claims 1 to 3, described preparation method comprises the steps:
1) frequency is 20 ~ 25kHz, power is the aqueous solution 15-30min that 70 ~ 90% times supersound process graphene nanometer sheets are made into;
2) under 300 ~ 500rpm speed, ethylene-vinyl acetate emulsion is added step 1) graphene solution in stir 30 ~ 60min, obtain cotton-shaped compound;
3) with compound described in deionized water rinsing, filter, vacuum lyophilization, obtain the masterbatch of graphene semiconductor shielding material;
4) open refining mixing 10 ~ 15h, 160 ~ 180 DEG C, pressure be 8 ~ 15MPa under vulcanisation step 3) the masterbatch 8 ~ 12min of gained, obtain graphene semiconductor shielding material.
5. preparation method according to claim 4, is characterized in that step 1) described in the concentration of graphene solution be 5 ~ 20g/L.
6. preparation method according to claim 4, is characterized in that step 3) described in compound deionized water rinsing to neutral.
7. preparation method according to claim 4, is characterized in that step 3) described in freezing temp be-50 ~-15 DEG C, the time is 3 ~ 5day, vacuum tightness < 10Pa.
8. preparation method according to claim 4, is characterized in that step 4) described in curing temperature be 170 ~ 175 DEG C, curing time is 10 ~ 12min, and sulfide stress is 8 ~ 12MPa.
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| CN201510439101.3A CN105131408A (en) | 2015-06-26 | 2015-06-26 | Graphene semiconductor shield material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105895242A (en) * | 2016-06-22 | 2016-08-24 | 中国航空综合技术研究所 | Graphene-contained flame-retardant insulating cable |
| CN106750862A (en) * | 2016-12-16 | 2017-05-31 | 吴中区穹窿山天仲高分子材料技术研究所 | A kind of preparation method of Graphene EVA composites |
| CN107564618A (en) * | 2017-09-30 | 2018-01-09 | 河北华通线缆集团股份有限公司 | A kind of water-proof cable containing graphene |
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| CN105895242A (en) * | 2016-06-22 | 2016-08-24 | 中国航空综合技术研究所 | Graphene-contained flame-retardant insulating cable |
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Application publication date: 20151209 |