CN106832733A - A kind of preparation method of dielectric polyaniline/elastic composite high - Google Patents
A kind of preparation method of dielectric polyaniline/elastic composite high Download PDFInfo
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Abstract
A kind of preparation method of dielectric polyaniline/elastic composite high, belong to technical field of composite preparation, the present invention is with oil-soluble elastomer as matrix material, the oil-soluble doped polyaniline solution of emulsion polymerization synthesis is dielectric enhancement material, homogeneous phase solution is formed after both are well mixed according to certain ratio, evaporative removal solvent, the method that material shaping obtains dielectric polyaniline/elastic composite high.It is characteristic of the invention that low production cost, process is simple, convenient formation, and the composite has dielectric constant and pliability higher.
Description
Technical field
The invention belongs to technical field of composite preparation, and in particular to a kind of dielectric polyaniline/elastomer composite material high
The preparation method of material.
Background technology
Dielectric elastomer is a kind of electroactive polymer, driving deformation can be produced under electric field action, with electroluminescent shape
Become big, energy density is high, the response time is short, pliability good and the features such as high conversion efficiency, can be widely applied to pocket or micro-
The fields such as humanoid robot, micro-air-vehicles, disc driver, plane loudspeaker and prosthetics.But, dielectric elastomer material
Dielectric constant it is relatively low, it is necessary to larger electroluminescent deformation could be produced under higher electric field, this severely limits dielectric elastomer
Development and application.Therefore, the dielectric constant for how improving dielectric elastomer is the primary study in current dielectric elastomer field
Problem.
Elastomer has unique high resiliency（Reaction time is short, viscoplasticity is delayed small）, the good and high filling energy of pliability
Power, but most of elastomers are not crystallized at room temperature, type is small, and dielectric constant is small, outfield is sensed weaker, it is impossible to directly as
Electroactive polymer.In order to obtain bigger electroluminescent deformation, many researchers by by elastomer and high dielectric ceramic filler or
The conductive fillers such as metal, carbon material are combined to improve the dielectric constant of dielectric elastomer.But, larger loading certainty
The modulus of elastomer can be caused to increase considerably, had a strong impact on the range of application and application field of composite.In recent years, with
Polyaniline（PANI）For the dielectric composite material of conductive filling material has obtained very big development.Compared with other fillers, PANI
With structure diversification, electrical conductivity is high, mechanism of doping effect is unique, high-k, environmental stability good, and raw material is inexpensively easy
, simple synthetic method the advantages of, obtained the favor of Many researchers.But, exist in polyaniline molecule structure substantial amounts of
Benzene formula and quinoid rigid structure, polyaniline in eigenstate solubility certain in organic solvent, however, changing by inorganic acid doping
Property after, it is almost insoluble in most of conventional organic solvent, is only partially soluble in DMF and N- methyl pyrroles
Pyrrolidone etc., significantly limit application of the polyaniline as conductive additive.Polyaniline is mixed using organic proton acid
It is miscellaneous modified, while layer/polyaniline conductive performance is lifted, its solubility in organic solvent is significantly increased.Therefore, adopt
With the polyaniline of modified with organic acids as dielectric elastomer dielectric enhancement material, with highly important theory and actual application
Value.
The content of the invention
It is low for existing dielectric type elastic composite dielectric constant, and dielectric type elastomer after addition conductive filler
The problem of the reduction of pliability of composite, the present invention proposes a kind of dielectric polyphenyl high that can overcome above prior art defect
The preparation method of amine/elastic composite.
The technical scheme is that：Oil-soluble polyaniline solution and elastomer are mixed, is stirred at room temperature uniform rearmounted
In mould, evaporation solvent shaping obtains final product dielectric polyaniline/elastic composite high.
The present invention with oil-soluble elastomer as matrix material, emulsion polymerization synthesis oil-soluble doped polyaniline solution
Be dielectric enhancement material, by both according to certain ratio it is well mixed after form homogeneous phase solution, evaporative removal solvent, material into
The method that type obtains dielectric polyaniline/elastic composite high.It is characteristic of the invention that low production cost, process is simple, into
Type is convenient, and the composite has dielectric constant and pliability higher.
Wherein, the mass ratio of polyaniline and elastomer is 0.1~10: 100 in the oil-soluble polyaniline solution.The present invention
Oil-soluble doped polyaniline solution can dissolve each other with oil-soluble elastomer so that add a small amount of oil-soluble doped polyaniline
Solution can just obtain the polyaniline/elastic composite of high-k, and the polyaniline/elastic composite has
Preferable pliability.
The oil-soluble polyaniline is with benzene sulfonic acid, isopropyl sulfonic acid, toluene sulfonic acide, DBSA, diformazan
At least one polyaniline modified for dopant material of benzene sulfonic acid, camphorsulfonic acid and dibutyl naphthalenesulfonic acid, stearic acid or palmitic acid.
Polyaniline is modified using the acid of these organic protons, the conductive capability and its in organic solvent of polyaniline can be improved
Solubility.A small amount of modified with organic acids polyaniline is added in the elastomer, both can obtain the composite of high-k, and it is multiple
The elastic modelling quantity of condensation material does not increase significantly.
The elastomer is phenylethylene（SBS、SIS、SEBS、SEPS）, olefines（TPO、TPV）, diene class（TPB、
TPI）, polyvinyl chloride-base（TPVC、TCPE）, urethane class（TPU）, esters（TPEE）, amide-type（TPAE）, organic fluoride class（TPF）, have
Machine silicone rubber kinds (PDMS) or vinyl elastomer.The composite of preparation, it is stretchable and electric conductivity is good.
Solvent in the oil-soluble polyaniline solution is to be respectively provided with preferable compatibility with doped polyaniline and elastomer
Organic solvent, including pentane, hexane, hexamethylene, benzene,toluene,xylene, chlorobenzene, dichloro-benzenes, methylisobutylketone, dichloromethane
Alkane, tetrahydrofuran, 1-METHYLPYRROLIDONE, dimethylformamide, dimethyl sulfoxide or dichloroethanes.The composite of preparation,
It is stretchable and electric conductivity is good.
The present invention specifically has the advantage that：（1）Cost of material is low.Polyphenyl is prepared using the technique of aniline oxidation emulsion polymerization
Amine aqueous solution, conventional conductive filler is replaced with this, and cost of material can be greatly lowered；（2）Dielectric elastomer composite material is flexible
Property is good.The polyaniline of traditional handicraft synthesis, poor solubility in organic solvent, particularly non-polar solven, patent of the present invention
Polyaniline prepared by the emulsion polymerization of use has excellent solubility in organic solvent, adds in the elastomer a small amount of
Oil-soluble polyaniline solution is the elastic composite that can obtain high-k, and will not substantially reduce the soft of elastomer
Toughness；（3）Process is simple is convenient.The polyaniline of high-dissolvability, it is only necessary to elastomer simply in proportion mixing, evaporation solvent into
Type, you can easily prepare the polyaniline/elastic composite of dielectric high.
Specific embodiment
The following examples are illustrated the present invention in more detail, rather than limitation of the invention further.Unless
It is otherwise noted, wherein each percentage is mass percent.
Embodiment 1：
1st, the preparation of DBSA modified polyaniline toluene solution：
DBSA 36.28g, deionized water 200mL and toluene 50mL are added in 1L four-hole bottles, stirring is cooled to 2
DEG C when, add aniline 5.59g, and be incubated 1h.Insulation is finished, to being slowly added dropwise 9.13g ammonium persulfates and 50mL water in reaction system
Mixed solution, time for adding is 1h, then 0-5 DEG C of insulation reaction 17h.Insulation is finished, and 200mL toluene and 200g acetone are added
To in reactor material, and after stirring 1h, stratification obtains oil reservoir 198.36g, water layer 501.68.Oil reservoir carries out negative pressure and quickly takes out
Filter, removes a small amount of insoluble matter, and final to obtain clear green oil reservoir 196.25g, test solid content is 7.58%.
2nd, hydrogenated styrene-butadiene block copolymer（SEBS）The preparation of toluene liquid：
5.68g SEBS powder is added in 28.74g toluene, stirring is warming up to 90 DEG C or so, and SEBS is down to room after being completely dissolved
Temperature, obtains the SEBS toluene solutions that concentration is 16.5%.
3rd, polyaniline/hydrogenated styrene-butadiene block copolymer（PANI/SEBS）The preparation of high-dielectric composite material：
The SEBS first that the DBSA modified polyaniline toluene solution that will be obtained in 1.5g steps 1 is added in step 2
In benzole soln（Wherein polyaniline and the mass ratio of folding hundred of SEBS is 2: 100）, after 1h is stirred at room temperature, it is transferred in mould, it is placed in
In 30 DEG C of thermostatic drying chambers, 6h is heated, you can to dielectric PANI/SEBS composites high.
4th, test：
The composite wood is tested using the molded breadth frequency dielectric constants of German Novocontrol Technoligies companies Concept 80
The dielectric properties of material, its elastic modelling quantity is surveyed using standard dog bone batten.The dielectric PANI/SEBS composites high for obtaining
Dielectric constant（100Hz）677.12 and elastic modelling quantity 3.22MPa.
Embodiment 2~5：
With benzene sulfonic acid, isopropyl sulfonic acid, toluene sulfonic acide, xylene monosulfonic acid, camphorsulfonic acid, dibutyl naphthalenesulfonic acid, stearic acid or
Palmitic acid is dopant material, and polyaniline is modified, in the similar embodiment 1 of method, only be doping material by dodecyl
Benzene sulfonic acid is changed to each material of the above, investigates dielectric constant of the different organic acid doped materials to PANI/SEBS composites
With the influence of elastic modelling quantity, as a result see the table below.
Each example more than：Using benzene sulfonic acid, isopropyl sulfonic acid, toluene sulfonic acide, DBSA, dimethylbenzene
Composite prepared by sulfonic acid, camphorsulfonic acid and dibutyl naphthalenesulfonic acid, stearic acid or palmitic acid modified polyaniline is respectively provided with higher
Dielectric constant and preferable pliability.
Embodiment 6~9：
Using pentane, hexane, hexamethylene, benzene, dimethylbenzene, chlorobenzene, dichloro-benzenes, 1-METHYLPYRROLIDONE, methylisobutylketone, dichloro
Methane, tetrahydrofuran, dimethylformamide, dimethyl sulfoxide or dichloroethanes are solvent, replace the toluene in example 1, other
Part is constant, investigates influence of the organic solvent to the dielectric constant and elastic modelling quantity of PANI/SEBS composites, as a result see the table below.
Each example explanation more than：Influence of the organic solvent to the dielectric constant and elastic modelling quantity of PANI/SEBS composites
It is smaller, using pentane, hexane, hexamethylene, benzene,toluene,xylene, chlorobenzene, dichloro-benzenes, methylisobutylketone, dichloromethane, tetrahydrochysene
At least one in furans, dimethylformamide, 1-METHYLPYRROLIDONE, dimethyl sulfoxide or dichloroethanes is solvent, is prepared
Composite be respectively provided with dielectric constant and preferable pliability higher.
Embodiment 10~17：
On the basis of embodiment 1, polyaniline elastic composite is prepared using other kinds of elastomer, its dielectric constant
And elastic modelling quantity see the table below.
Each example more than：Using phenylethylene, olefines, diene class, polyvinyl chloride-base, urethane class, esters, acid amides
Polyaniline/elastic composite prepared by class, organic fluoride class, organic silicon rubber class or ethene analog thermoplastic elastomer is respectively provided with
Dielectric constant higher and preferable pliability.
Embodiment 18~25：
On the basis of example 1, dielectric properties and springform of the different polyaniline consumptions to PANI/SEBS composites are investigated
The influence of amount, as a result see the table below.
Illustrated by various embodiments above：The dielectric polyaniline high being made of the inventive method/elastic composite, energy
Enough overcome existing dielectric type elastic composite dielectric constant low, and addition conductive filler causes dielectric type elastomer composite
The problem of the reduction of pliability of material.
Claims (4)
1. a kind of preparation method of dielectric polyaniline/elastic composite high, it is characterised in that by oil-soluble polyaniline solution
With elastomer mixing, polyaniline and the mass ratio of elastomer mixing are 0.1~10: 100 in the oil-soluble polyaniline solution,
It is placed in mould after stirring at room temperature, evaporation solvent shaping obtains final product dielectric polyaniline/elastic composite high.
2. the preparation method of dielectric polyaniline/elastic composite high according to claim 1, it is characterised in that：It is described
Oil-soluble polyaniline is benzene sulfonic acid, isopropyl sulfonic acid, toluene sulfonic acide, DBSA, xylene monosulfonic acid, camphorsulfonic acid
With at least one polyaniline modified for dopant material of dibutyl naphthalenesulfonic acid, stearic acid or palmitic acid.
3. the preparation method of dielectric polyaniline/elastic composite high according to claim 1, it is characterised in that：It is described
Elastomer is phenylethylene, olefines, diene class, polyvinyl chloride-base, urethane class, esters, amide-type, organic fluoride class, organosilicon rubber
Glue class or vinyl elastomer.
4. the preparation method of dielectric polyaniline/elastic composite high according to claim 1, it is characterised in that：It is described
Solvent is pentane, hexane, hexamethylene, benzene,toluene,xylene, chlorobenzene, dichloro-benzenes, methyl tert-butyl in oil-soluble polyaniline solution
Ketone, dichloromethane, tetrahydrofuran, dimethylformamide, 1-METHYLPYRROLIDONE, dimethyl sulfoxide or dichloroethanes.
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Application publication date: 20170613 |