CN107325520B - A kind of preparation method of antistatic modified plastics - Google Patents
A kind of preparation method of antistatic modified plastics Download PDFInfo
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Abstract
A kind of preparation method of antistatic modified plastics, is related to the production technical field of Antistatic type plastics.Organic-silicon-modified ethyl orthosilicate is pre-condensed presoma to be added with spray pattern in the dilute microplate of graphite of high-speed stirred and the mixed system of carbon nanotube, is then sufficiently mixed again with plastic pellet, then through extruding pelletization, obtains collaboration anti-electrostatic modified plastic.The present invention solves the aggregation problem of the dilute microplate of graphite and carbon nanotube, OM-SiO2The introducing of organic group in P, can assign the interface binding power of nano carbon material and plastic substrate, realize the low target of the loading needed when reaching antistatic property index, and obtained nanocomposite also has ideal mechanics, thermodynamics and wear-resisting property.
Description
Technical field
The present invention relates to the production technical fields of Antistatic type plastics.
Background technique
Plastics occupy consequence, resistivity with higher and good insulation in people's daily life and production
Property, it is widely used usually as insulating materials, but plastics are easy to produce electrostatic in production, transport and use process, make
At malignant events such as dust suction, electric shocks even explosion.Therefore, the antistatic technology demand of plastics is increasing, and many carbon materials by
In its high conductivity, it is frequently used to as the antistatic modified additive of plastics.
Graphene has excellent electricity, heat and mechanical performance, is optimal two-dimension nano materials now, is expected to apply
In the preparation of the electrode material of hydrogen storage equipment, solar battery and lithium battery, the fields such as biosensor and engineering plastics.Carbon
After nanotube (CNTs) is found and is reported for the first time by Lijima since 1991 as a kind of quasi- one-dimensional carbon nano material, due to
Its unique structure and excellent performance have rapidly become the research hotspot of field of nanometer material technology.
In recent years, numerous studies report gathers graphene and CNTs with the compound high-performance conductive for preparing of polymer respectively
Object based nano composite material is closed, and achieves gratifying progress.Complete graphene have high electron mobility [2 ×
105cm2/ (VS)], and CNTs is made of being crimped as graphene, so having good conductive property as graphene.
Since two-dimensional graphene and the composite construction of one-dimensional carbon nanotube have big specific surface and three dimensional network structure, more favorably
Conductive network structure will necessarily be more effectively constructed in polymer matrix body in the common addition of the transfer of electronics, the two, in turn
Reduce its conductivity threshold.
However, either graphene or CNTs, on the one hand due to their distinctive small-size effects and skin effect, with
And itself strong model ylid bloom action power makes them easily reunite, and causes to disperse in the base uneven；On the other hand, stone
The surface of black alkene and CNTs have stronger hydrophobicity and chemical inertness, lead to the poor compatibility of they and polymeric matrix, multiple
The interface bond strength of condensation material is low.This cannot not only play the characteristic of nanofiller, can reduce the property of polymeric matrix instead
Energy.So how promoting graphene and CNTs dispersion in a polymer matrix, improving its interface between polymeric matrix
In conjunction with being currently to prepare high-performance polymer/graphene/(CNTs) nanocomposite bottleneck problem.
It is a kind of poly- carbon of conduction containing multi-dimensional nanomaterial in technical solution disclosed in patent document CN201510181084
Perester radical pellet adds inorganic dispersion aids using conductive black/carbon nano tube/graphene as conductive material to help it
Dispersion in polycarbonate.But it is good using the dispersion effect of Organic-inorganic composite dispersing agent that its effect is not so good as, and needs to fill out
The carbon nanomaterial for filling high-content is not easy to be uniformly mixed.
It is a kind of gathering for graphene/carbon nanotube hybrid in technical solution disclosed in patent document CN200510046681.6
Compound composite material and its manufacturing method are added to polymer body using graphene oxide and oxide/carbon nanometer tube
In, the polymer composites of graphene/carbon nanotube hybrid are prepared by the method for solution blending or mechanical blending.But
It is the graphene oxide and oxide/carbon nanometer tube using functionalization, original structure may be destroyed during functionalization, is made
The decline of its electric conductivity, and price improves.
Summary of the invention
Easy to reunite and aiming at the problem that with plastic interface poor adhesion carbon nanotube and graphene, the present invention provides one kind
The preparation method of antistatic modified plastics.
The technical scheme is that: organic-silicon-modified ethyl orthosilicate is pre-condensed presoma (OM-SiO2P) with spraying square
Formula is added in the dilute microplate of graphite of high-speed stirred and the mixed system of carbon nanotube, is then sufficiently mixed again with plastic pellet, then
Through extruding pelletization, collaboration anti-electrostatic modified plastic is obtained.
Organic-silicon-modified ethyl orthosilicate pre-condensation presoma normality is liquid, and the present invention is first by organic-silicon-modified positive silicon
Acetoacetic ester is pre-condensed presoma (OM-SiO2P the graphene microchip of high-speed stirred) is added to spray pattern and carbon nanotube is mixed
In zoarium system, then high-speed stirred, as a result organically-modified nano-silica is equably generated in graphene microchip and carbon nano tube surface
SiClx can effectively weaken the interaction between graphene microchip and between carbon nanotube, efficiently avoid nano size particles
Aggregation problem, one-dimensional carbon pipe and two-dimensional sheet graphene are constructed into conductive network structure, OM-SiO in plastic substrate2In P
Organic group can increase the interaction with plastic substrate, to assign the interface binding power of nano carbon material and plastics, with
Improve the mechanics of antistatic modified composite material, creep resistant and the performances such as wear-resisting.This is because organically-modified nano-silica
The basic structural unit of silicon is made of silicon-oxygen chain link, and side chain then passes through silicon atom and is connected with organic group.
The beneficial effects of the present invention are:
1, the present invention is pre-condensed presoma (OM-SiO using organic-silicon-modified ethyl orthosilicate2P) carry out disperse modified graphite
Alkene microplate and carbon nanotube, in graphene microchip and carbon nano tube surface equably generation organically-modified nano-silica in situ
Silicon dexterously solves the aggregation problem of the dilute microplate of graphite and carbon nanotube, OM-SiO2The introducing of organic group, Ke Yifu in P
Give the interface binding power of nano carbon material and plastic substrate.
2, method of modifying provided by the invention can construct what carbon nanotube was combined with graphene microchip in plastic substrate
Three-dimensional conductive network structure realizes the low target of the loading needed when reaching antistatic property index.
3, the nanocomposite that antistatic modified method provided by the invention obtains also has ideal mechanics, thermodynamics
And wear-resisting property.
Further, organic-silicon-modified ethyl orthosilicate of the present invention is pre-condensed presoma (OM-SiO2P), graphite is dilute
Microplate and the additive amount of carbon nanotube account for the 0.1~0.5wt%, 1~8wt%, 0.5~3wt% of total addition level respectively.
The antistatic property of plastics not only can be improved in this additive amount, moreover it is possible to improve the mechanical property of plastics.
And when organic-silicon-modified ethyl orthosilicate is pre-condensed presoma (OM-SiO2P) additive amount of solution is very little, then rises
It is such as too many less than the effect of interface disperse modified, then it can reduce the antistatic effect of nanocomposite.
In addition, graphene of the present invention is in single-layer graphene, bilayer graphene, few layer graphene or multi-layer graphene
At least any one.Graphene can not only improve the electric conductivity of plastics, can also improve the mechanical properties of plastics with it is wear-resisting
Performance.
The carbon nanotube be in single-walled carbon nanotube or multi-walled carbon nanotube at least any one.Carbon nanotube and stone
The synergistic effect of black alkene has big specific surface and three dimensional network structure, is more advantageous to the transmission of electronics, can be more effectively poly-
It closes in object matrix and constructs conductive network structure, increase the antistatic property of plastics.
The plastics are any one in polyethylene, polypropylene, polycarbonate, nylon or polyether-ether-ketone.These types modeling
Material covers general-purpose plastics, engineering plastics and special plastic, is widely used, studies its antistatic property and be of great significance.
Specific embodiment
In following embodiment, unless otherwise stated, all percentage compositions are by weight.
One, organic-silicon-modified ethyl orthosilicate pre-condensation presoma is prepared:
By 7.7g ethyl orthosilicate (TEOS), 0.545g γ-methacryloxypropyl trimethoxy silane
(KH570), 1g water, the mixing of 3.4g ethyl alcohol, in 60 DEG C of reaction 6h, obtain organosilicon after the pH to 6 of hydrochloric acid adjustment mixed system
Modified ethyl orthosilicate is pre-condensed presoma, abbreviation OM-SiO2P, is liquid under room temperature normality.
Two, the modification of plastics and antistatic result:
Embodiment 1:
(1) graphene microchip 20g, carbon nanotube 60g are weighed, organic-silicon-modified ethyl orthosilicate is pre-condensed presoma (OM-
SiO2P) solution 2g, by OM-SiO2P solution is mixed with the graphene microchip that spray pattern is added to high-speed stirred with carbon nanotube
In system, then high-speed stirred 10min.
(2) 1918g polycarbonate is weighed, with modified Nano material in step (1) with high mixer mixing 10min, by double
Graphene/carbon nano-tube/polycarbonate composite material is made in screw machine extruding pelletization, vulcanizes pressure on 260 DEG C of vulcanizing presses
Piece 10min, measuring volume resistivity is 2 × 106Ω·cm。
Embodiment 2:
(1) graphene microchip 80g, carbon nanotube 20g are weighed, organic-silicon-modified ethyl orthosilicate is pre-condensed presoma (OM-
SiO2P) solution 4g, by OM-SiO2P solution is mixed with the graphene microchip that spray pattern is added to high-speed stirred with carbon nanotube
In system, then high-speed stirred 10min.
(2) 1896g polyether-ether-ketone is weighed, with modified Nano material in step (1) with high mixer mixing 10min, by double
Graphene/carbon nano-tube/polyether-ether-ketone composite material is made in screw machine extruding pelletization, vulcanizes pressure on 400 DEG C of vulcanizing presses
Piece 10min, measuring volume resistivity is 4 × 106Ω cm, coefficient of friction drop to 0.340 from 0.424, and frictional behaviour obtains
It improves.
Embodiment 3:
(1) graphene microchip 160g, carbon nanotube 10g are weighed, organic-silicon-modified ethyl orthosilicate is pre-condensed presoma
(OM-SiO2P) solution 10g, by OM-SiO2P solution is added to the graphene microchip and carbon nanotube of high-speed stirred with spray pattern
In mixed system, then high-speed stirred 10min.
(2) 1820g polyethylene is weighed, with modified Nano material in step (1) with high mixer mixing 10min, by double spiral shells
Bar machine extruding pelletization is made graphene/carbon nano-tube/composite polyethylene material, vulcanizes tabletting on 180 DEG C of vulcanizing presses
10min, measuring volume resistivity is 2 × 106Ω·cm。
Comparative example 1:
(1) graphene microchip 20g, carbon nanotube 60g are weighed, organic-silicon-modified ethyl orthosilicate is pre-condensed presoma (OM-
SiO2P) solution 20g, by OM-SiO2P solution is mixed with the graphene microchip that spray pattern is added to high-speed stirred with carbon nanotube
In system, then high-speed stirred 10min.
(2) 1900g polycarbonate is weighed, with modified Nano material in step (1) with high mixer mixing 10min, by double
Graphene/carbon nano-tube/polycarbonate composite material is made in screw machine extruding pelletization, vulcanizes pressure on 260 DEG C of vulcanizing presses
Piece 10min, measuring volume resistivity is 2 × 1011Ω·cm。
This comparative example increases organic-silicon-modified ethyl orthosilicate pre-condensation presoma (OM-SiO2P) the dosage of solution, leads
Volume resistivity is caused to substantially increase, antistatic effect is deteriorated.
Comparative example 2:
(1) graphene microchip 80g, carbon nanotube 20g are weighed, organic-silicon-modified ethyl orthosilicate is pre-condensed presoma (OM-
SiO2P) solution 1g, by OM-SiO2P solution is mixed with the graphene microchip that spray pattern is added to high-speed stirred with carbon nanotube
In system, then high-speed stirred 10min.
(2) 1899g polyether-ether-ketone is weighed, with modified Nano material in step (1) with high mixer mixing 10min, by double
Graphene/carbon nano-tube/polyether-ether-ketone composite material is made in screw machine extruding pelletization, vulcanizes pressure on 400 DEG C of vulcanizing presses
Piece 10min, measuring volume resistivity is 2 × 1011Ω·cm。
This comparative example reduces organic-silicon-modified ethyl orthosilicate pre-condensation presoma (OM-SiO2P) the dosage of solution, leads
Volume resistivity is caused to substantially increase, antistatic effect is deteriorated.
Comparative example 3:
Weigh 40g carbon nanotube, 1960g polyether-ether-ketone, high mixer mixing 10min, by dual-screw-stem machine extruding pelletization system
Carbon nano-tube/poly polyetherether ketone composite is obtained, vulcanizes tabletting 10min on 400 DEG C of vulcanizing presses, measuring volume resistivity is
2×108Ω cm, tensile strength 77Mpa.
This comparative example is only added to unmodified carbon nanotube, compound although electric conductivity reaches antistatic requirement
The tensile strength of material is reduced to 77MPa compared to the 95MPa of polyether-ether-ketone, reduces significant.
Comparative example 4:
(1) graphene microchip 100g is weighed, organic-silicon-modified ethyl orthosilicate is pre-condensed presoma (OM-SiO2P) solution
20g, by OM-SiO2P solution is added in the graphene microchip and carbon nanotube hybrid system of high-speed stirred with spray pattern, then
High-speed stirred 10min.
(2) 1880g polyether-ether-ketone is weighed, with modified Nano material in step (1) with high mixer mixing 10min, by double
Graphene/carbon nano-tube/polyether-ether-ketone composite material is made in screw machine extruding pelletization, vulcanizes pressure on 400 DEG C of vulcanizing presses
Piece 10min, measuring volume resistivity is 2 × 1012Ω·cm。
More organic-silicon-modified nanometer titanium dioxide silicon precursor (OM-SiO is added in this comparative example2P) solution, resistance compared with
Greatly, antistatic requirement cannot be reached.
Claims (4)
1. a kind of preparation method of antistatic modified plastics, it is characterised in that: organic-silicon-modified ethyl orthosilicate to be pre-condensed
Presoma with spray pattern be added high-speed stirred graphene microchip and carbon nanotube mixed system in, then again with plastics
Particle is sufficiently mixed, then through extruding pelletization, obtains collaboration anti-electrostatic modified plastic；The organic-silicon-modified ethyl orthosilicate preshrunk
The additive amount for closing presoma, graphene microchip and carbon nanotube accounts for 0.1~0.5wt% of total addition level, 1~8wt%, 0.5 respectively
~3wt%；The method for preparing the organic-silicon-modified ethyl orthosilicate pre-condensation presoma is: by 7.7g ethyl orthosilicate,
0.545g γ-methacryloxypropyl trimethoxy silane, 1g water, the mixing of 3.4g ethyl alcohol, adjust mixed system with hydrochloric acid
PH to 6 after, in 60 DEG C of reaction 6h, obtain organic-silicon-modified ethyl orthosilicate pre-condensation presoma, abbreviation OM-SiO2P, room temperature
It is liquid under normality.
2. preparation method according to claim 1, it is characterised in that: the graphene is single-layer graphene, double-layer graphite
In alkene, few layer graphene or multi-layer graphene at least any one.
3. preparation method according to claim 1, it is characterised in that: the carbon nanotube is single-walled carbon nanotube or multi wall
In carbon nanotube at least any one.
4. preparation method according to claim 1, it is characterised in that: the plastics are polyethylene, polypropylene, poly- carbonic acid
Any one in ester, nylon or polyether-ether-ketone.
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| CN109796545B (en) * | 2017-11-17 | 2021-08-27 | 中国石油天然气股份有限公司 | Preparation method of antistatic ultrahigh molecular weight polyethylene |
| CN108084686B (en) * | 2017-12-27 | 2020-11-27 | 上海统慧科技发展有限公司 | Polyester-based conductive master batch based on carbon nanotube and graphene compound system and preparation method thereof |
| CN108373559A (en) * | 2018-02-02 | 2018-08-07 | 桂林理工大学 | A kind of graphene/carbon nano-tube collaboration enhancing polyethylene pipe and preparation method thereof |
| CN109627580B (en) * | 2018-12-10 | 2024-04-26 | 上海玉城高分子材料股份有限公司 | Light-colored permanent antistatic modified polypropylene material and preparation method thereof |
| CN112976741A (en) * | 2021-03-15 | 2021-06-18 | 瑞安市东威塑胶有限公司 | BOPP antistatic stretching film |
| CN117024873A (en) * | 2023-06-15 | 2023-11-10 | 广州力合新材料科技有限公司 | Preparation method of modified polypropylene plastic |
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| CN103525014B (en) * | 2013-10-31 | 2015-05-20 | 华南理工大学 | Three-phase composite high-dielectric-property material, manufacturing method and processing method |
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