CN110358309A - A kind of silica gel/carbon nanotube dielectric elastomer composite material and preparation method thereof - Google Patents
A kind of silica gel/carbon nanotube dielectric elastomer composite material and preparation method thereof Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/392—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing sulfur
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- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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Abstract
The present invention relates to a kind of silica gel/carbon nanotube dielectric elastomer composite materials and preparation method thereof, belong to dielectric elastomer composite material.The composite material is prepared by following raw material: 100 parts by weight of carboxyl graft modification silicon rubber, 0.5~5 parts by weight of more benzene ring compounds, 0.1~1 parts by weight of 0.5~5 parts by weight of array carbon nano tube, 0.1~1 parts by weight of crosslinking agent and catalyst, wherein carboxyl graft modification silicon rubber is obtained and being grafted carboxylic small organic molecule on silicon rubber.The present invention can increase substantially the dielectric constant of composite material under low loading, while not significantly improve its elasticity modulus and dielectric loss.
Description
Technical field
The invention belongs to dielectric material fields, further, are related to a kind of silica gel/carbon nanotube dielectric elastomer composite wood
Material and preparation method thereof.
Background technique
Dielectric elastomer (dielectric elastomer, DE) is electroactive polymer.When applying external electrical field to DE,
Due to the effect of Maxwell stress, DE can generate the expansion of in-plane and the compression of thickness direction, convert electrical energy into machinery
Energy；When removing extra electric field, DE can be restored to original shape and volume again.DE is big with electroluminescent deformation, the response time is fast,
The advantages that dielectric loss is small, elastic energy density is high, high conversion efficiency is widely used in artificial-muscle, prosthetics, miniature
Aircraft, sensor (such as blind person's touch screen), plane loudspeaker field.But most of dielectric elastomer material room temperatures are not tied
Crystalline substance, polarity is small, and dielectric constant is lower, and the strain for often leading to that very high driving voltage is needed to can be only achieved practical application is wanted
It asks, seriously hinders the application of dielectric elastomer, therefore the dielectric constant for how improving dielectric elastomer becomes the research field
A major challenge.
Chinese patent application " dielectric elastomer material and preparation method thereof " (number of patent application 200810064238.5) mentions
Go out and dielectric elastomer is mixed and made into using relaxor ferroelectric ceramics material and silicone rubber solution, dielectric constant can achieve
80-360.University of Pennsylvania, the U.S. is by adding lead magnesio-niobate in solution normal direction polyvinyldifluoride-poly- trifluoro-ethylene (PVDF-TrFE)
(PMN) ceramic powders, when the volume fraction of the ceramic powders of addition is 50%, the dielectric constant of composite material can be promoted
200, but the poor compatibility between ceramic powders and rubber matrix, the additions of a large amount of ceramic powders so that composite material brittleness
Increase, modulus is obviously improved, and reduces the toughness of material, big electroluminescent shape can be obtained by needing to apply very high driving voltage
Become, limits the application of composite material.
Chinese patent application " high-dielectric composite material and preparation method thereof containing carbon nanotube " (number of patent application:
03104776.9) it proposes using carbon nanotube CNT, barium titanate BaTiO3With it is compound made of organic Kynoar (PVDF)
Material, dielectric constant can be up to 450.But since the raising of dielectric constant depends primarily on BaTiO3, however it is a large amount of
BaTiO3Filling, lead to filler difficulties in dispersion.And common CNTs has the shortcomings that height is tangled, hardly possible is dispersed, it can only be with aggregation
State figure is rambling to be scattered in polymer, and to improving, dielectric properties are unfavorable.In order to solve point of carbon pipe in the polymer
The problem of dissipating usually carries out surface chemical modification to carbon pipe and surface coats organic layer." a kind of carbon nano-tube/polymer is high for patent
The preparation method of dielectric constant compound film " (number of patent application: 200810018851.3) is first acidified carbon nanotube, amine
Change or plasma surface modification, then prepare carbon nano-tube/polymer laminated film using solution casting method.Patent is high
Dielectric property polyaryl ether ketone/polyaniline-carbon nano tube compound material and preparation method thereof (number of patent application:
201110233290.0) carbon nanotube of polyaniline-coated is used to improve its dispersibility in poly(aryl ether ketone).These methods can
So that carbon nanotube obtains good dispersion in the polymer, but also causes centainly to destroy to the complete structure of carbon pipe itself,
Influence the dielectric properties or reduction interfacial polarization effect of carbon pipe, it is therefore desirable to which higher carbon pipe additive amount could obtain height
Dielectric constant.
Summary of the invention
Thought and innovative point of the invention is embodied in: being introduced more benzene ring structures on silica gel first, is generated interfacial polarization, increases
Add the dielectric constant of modified silica-gel；Secondly one-dimension oriented array carbon nano tube is used, is sheared by two-roll mill in rubber
It is middle to form good dispersion, and by the pi-pi accumulation effect between phenyl ring, further increase that its is uniformly dispersed, thus into
The dielectric constant of one step raising composite material.
An object of the present invention is to provide a kind of silica gel/carbon nanotube dielectric elastomer composite material, by including following
The raw material of component is prepared, based on parts by weight:
Wherein, the carboxyl graft modification silicon rubber is by being grafted having with carboxyl polar functional group on silicon rubber
Machine small molecule and obtain, the carboxyl grafting rate of the preferably described carboxyl graft modification silicon rubber is 0.5%~5%.
The contents of ethylene of the silicon rubber is 0.5%~5%, and silicon rubber preferably is selected from methyl vinyl silicone rubber, methyl
At least one of ethenylphenyl silicon rubber, methyl ethylene trifluoro propyl silicon rubber.
At least one of the preferred mercaptopropionic acid of the polarity small organic molecule, thioacetic acid.
The carboxyl graft modification silicon rubber can be used method in the prior art and be prepared, preferably using clickization
Learn (a method of improve elastomer dielectric properties, number of patent application 201510462798.6), in the condition of UV illumination
Under in rubber side group grafted polar small organic molecule.
Specifically prepared using following steps:
100 parts of silicon rubber, 1~3 part of photoinitiator, 300~500 parts of polarity small organic molecule are taken, silica gel is dissolved in solvent
In, it is added polarity small organic molecule into silicone rubber solution, logical nitrogen 3~photoinitiator is added after five minutes, is 100 in power
Illumination 2min~2h under~500W ultraviolet lamp obtains the carboxyl graft modification silicon rubber.
The photoinitiator is selected from photoinitiator commonly used in the art, preferably benzil derivatives (such as: styrax diformazan
Ether, DMPA), Dialkoxy acetophenones, benzoin (Benzoin) and its derivative etc..
By taking thioacetic acid as an example, the reaction equation of Silicage-polymer- bonded phase polar micromolecules is as follows:
The array carbon nano tube length is 50~100 μm, and caliber is 6~8nm, and preferred length is 70~90 μm, caliber
For 6~7nm.
Compared with common carbon pipe, array carbon nano tube has the characteristics that one-dimension oriented arrangement, is sheared by open mill, and carbon is received
The array structure of mitron beam is destroyed, and the single-root carbon nano-tube isolated is evenly dispersed in a polymer matrix, obtains dispersing good
Good carbon nano tube compound material.
More benzene ring compounds be the compound with more benzene ring structures, preferably 5,5,10,10,15,15- Hexaethyls-
- three polyindene (compound A) of 2,7,12- triamido can be used method in the prior art and (Lin T C, Tsai B be prepared
K,Huang T Y,et al.Synthesis and two-photon absorption properties of truxene-
cored chromophores with functionalized pyrazine units fused as the end-groups
[J].Dyes&Pigments,2015,120(28):99-111.)。
The catalyst is selected from catalyst commonly used in the art, preferably N, N'- Dicyclohexylcarbodiimide (DCC), 1- (3-
At least one of dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride (EDC).
The crosslinking agent is selected from peroxide cross-linking agent commonly used in the art, preferably dibenzoyl peroxide (BPO), peroxide
Change diisopropylbenzene (DIPB) (DCP) or 2,5- dimethyl -2,5- two (t-butylperoxy) hexane (at least one of double 2,5).
The second object of the present invention is to provide a kind of preparation method of silica gel/carbon nanotube dielectric elastomer composite material,
The following steps are included:
Carboxyl graft modification silicon rubber is dissolved in solvent by step 1, forms uniform silica gel solution a by stirring；
More benzene ring compounds are added in solution a by step 2, and catalyst is added, is heated to 30-65 DEG C, and reaction 3h~
8h occurs condensation reaction, through drying, obtains the modified silica-gel b for being grafted more benzene ring compounds after purification；
Step 3 plasticates silica gel b, and the array carbon nano tube and crosslinking agent is added, is kneaded uniform after cure, obtains institute
State silica gel/carbon nanotube dielectric elastomer composite material.
Preferably, specific step is as follows for step 3: at room temperature, silica gel b being plasticated on the double roll mill, array is added
Carbon nanotube and crosslinking agent, slice parks 7~9h after being kneaded uniformly, according to the curing temperature (150 DEG C~180 DEG C) of measured in advance
Vulcanized on vulcanizing press with vulcanization time (1~2min), the silica gel/carbon nanotube for obtaining low content carbon nanotube is situated between
Electric elastic composite.
Solvent similar in the solubility parameter values such as the preferred tetrahydrofuran of the solvent, benzene, toluene, chloroform, ethyl acetate,
Dosage is conventional amount used, or requirement according to the actual situation is adjusted.The dosage of the preferred solvent is with 100 parts by weight
Carboxyl graft modification silicon rubber is to count, 200~500 parts of solvent.
Carboxyl graft modification silicon rubber and the reaction equation of compound A are as follows:
For being directly blended compared to traditional elastomer with carbon pipe, the present invention introduces more on silicone elastomer
Benzene ring structure compound, since with the electron conjugated effect of big pi bond, electronics can dissociate in big pi bond, and silica gel has insulation
Property, that just forms interfacial polarization between more benzene ring compounds and silica gel, and array carbon nano tube is added later, passes through the six of carbon pipe
π-the π that member ring and phenyl ring generate piles up the uniformity that effect increases the dispersion of carbon pipe, so as to improve composite material dielectric constant.
The present invention can obtain the composite material of fine dispersion, and the dielectric of composite material is increased substantially under low loading
Constant, while not significantly improving its elasticity modulus and dielectric loss.
Specific embodiment
Below in conjunction with the embodiments, the present invention is described in further details.
Raw materials used in the embodiment of the present invention is commercially available.
Dependence test explanation:
The dielectric properties measuring method of silica gel/carbon nanotube dielectric elastomer composite material, comprising the following steps: choose thick
Degree is 1mm, and diameter is the dielectric elastomer electrode test piece of 2cm, with acetone clean the surface；Using Novocontrol wideband dielectric
Impedance spectrometer, at room temperature, according to the dielectric constant of vulcanized rubber and the reference standard GB/T 1693- of dielectric loss angle tangent
2007, test 10-1-107Dielectric constant and dielectric loss in the frequency range of Hz.Test result is shown in Table 1.
At room temperature, using the puller system (CMT4104) of Shenzhen SANs company with the rate of extension pair of 50mm/min
Composite material batten carries out tension test, measures elasticity modulus and elongation at break.Wherein composite material diaphragm is cut into survey
The dumbbell shape batten that area is 20mm*4mm is tried, film thickness 0.5mm or so will strain preceding 5% corresponding strain data and carry out Linear Quasi
Conjunction obtains elasticity modulus.Referring to the modulus and elongation at break of GB/T528-2009 standard testing rubber composite material.Correlative measurement
Examination data are shown in Table 1.
Embodiment 1:
(1) it weighs the methyl vinyl silicone rubber that 100 parts by weight of ethylene base contents are 5% to be placed in conical flask, and adds
Enter 500 parts of tetrahydrofurans (THF) as solvent；400 parts of thioacetic acid are added after completely dissolution to silicon rubber, are filled to thioacetic acid
Lead to addition 3 parts of photoinitiator (dimethoxybenzoin) after nitrogen 4min after dividing dissolution, conical flask is placed under ultraviolet lamp (function later
Rate is 100W) illumination 8min, the silica gel solution after reaction is subjected to wadding glue with deionized water；It is then that the silica gel wadded a quilt with cotton out is molten again
It in 500 parts of tetrahydrofurans, is repeated three times, as far as possible removes the small molecules such as thioacetic acid in graft modification silica gel dry
Only；Obtained silica gel is dried to 72h in a vacuum drying oven at 50 DEG C later, obtaining more pure carboxyl grafting rate is
4.5% or so methyl vinyl silicone rubber.
(2) 4 part of three polyindene is added in anhydrous tetrahydro furan, stirs into after suspension and slowly adds under conditions of ice bath
Enter the hexane solution that 14 parts of concentration are 2.4M n-BuLi to be added drop-wise to 13 parts of bromoethanes after reacting 30min at room temperature
System is stated, after reacting 4h at room temperature, then the hexane solution that 14 parts of concentration are 2.4M n-BuLi is added dropwise, 13 parts is then added dropwise again
Bromoethane reacts at room temperature 8h or more, reaction solution is poured into water after being extracted with dichloromethane into above-mentioned solution after being added dropwise,
Solvent is removed with anhydrous sodium sulfate is dry, crude product obtains 5,5,10,10,15,15- Hexaethyls-three by silica gel chromatograph column purification
Polyindene (compound B)；0.2 part of concentrated nitric acid is added into 1, the 2- dichloroethane solution of compound B, by gained mixed solution in ice
Stirred in water bath 20min, solution becomes light brown at this time, and reaction mixture is poured into mixture of ice and water, and with NaOH tune pH
It to neutrality, is then extracted with ethyl acetate, anhydrous sodium sulfate is dry, and solvent is removed in vacuum, and crude product is pure by silica gel chromatographic column
Change, obtains 5,5,10,10,15,15- Hexaethyls -2,7,-three polyindene (compound C) of 12- trinitro-；By 2 parts of compound C and 4
Part stannic chloride dihydrate mixes in ethyl acetate, is stirred liquid and is heated to reflux 8h, unsaturated carbonate is used in ice bath
Hydrogen sodium is quenched, and is extracted with ethyl acetate after filtering, and dry with anhydrous sodium sulfate, solvent is removed in vacuum, crude product passes through silica gel
Chromatography obtains compound A.
(3) by 100 parts by weight carboxyl grafting rates be 4.5% methyl vinyl silicone rubber to be dissolved in 500 parts of tetrahydrofurans molten
In liquid, 0.5 part of compound A is added thereto, 0.5 part of DCC catalyst is added, and be stirred to react 3h at 50 DEG C, with anhydrous sulphur
Sour sodium is dry, solvent is removed in vacuum, crude product obtains the silica gel of graft compound A by silica gel chromatograph column purification.
(4) at room temperature, the silica gel of graft compound A is plasticated on the double roll mill, being gradually added into 0.5 part of length is
70 μm or so, the array carbon nano tube and 0.5 part of DCP crosslinking agent that caliber is 6nm or so, slice parks 7h after being kneaded uniformly,
Vulcanized on vulcanizing press, curing temperature is 160 DEG C, and vulcanization time 1min obtains the silica gel of low content carbon nanotube
Dielectric elastomer composite material.
Dependence test is carried out, test result is shown in Table 1.
Embodiment 2:
Preparation method and test method are with embodiment 1, but unlike the first embodiment: 1 part of chemical combination being added in step (3)
Object A, is heated to reflux 4h.Test result is shown in Table 1.
Embodiment 3:
Preparation method and test method are with embodiment 1, but unlike the first embodiment: 2 parts of chemical combination being added in step (3)
Object A, is heated to reflux 6h.Test result is shown in Table 1.
Embodiment 4:
Preparation method and test method are with embodiment 3, but as different from Example 3: 1 part of carbon being added in step (4) and receives
Mitron.Test result is shown in Table 1.
Embodiment 5:
Preparation method and test method are with embodiment 3, but as different from Example 3: 2 parts of carbon being added in step (4) and receive
Mitron.Test result is shown in Table 1.
Comparative example 1:
Preparation method and test method are with embodiment 1, but unlike the first embodiment: by 100 parts in step (1) of carboxylic
The methyl vinyl silicone rubber that base grafting rate is 4.5% is directly plasticated on a mill, and 0.5 part of DCP crosslinking is then added
Agent obtains silica gel base dielectric elastomer material after vulcanization.Test result is shown in Table 1.
Comparative example 2:
Preparation method and test method are with embodiment 1, but unlike the first embodiment: 100 parts in step (3) are connect
The silicon rubber of branch compound A is directly plasticated on a mill, and 0.5 part of DCP crosslinking agent is then added, obtains silica gel after vulcanization
Base dielectric elastomer material.Test result is shown in Table 1.
Comparative example 3:
Preparation method and test method are with embodiment 1, but unlike the first embodiment: by 100 parts in step (1) of carboxylic
The methyl vinyl silicone rubber that base grafting rate is 4.5% is directly plasticated on a mill, and 0.5 part of carbon nanotube is then added
With 0.5 part of DCP crosslinking agent, silica gel dielectric elastomer material is obtained after vulcanization.Test result is shown in Table 1.
1 embodiment of table is compared with the performance of comparative example
From the data analysis in table 1: to the silica gel of carboxyl graft modification by chemical reaction be grafted three polyindenes or
After physical blending adds carbon nanotube, dielectric constant is obviously improved, and dielectric loss and elastic modulus change are little.Addition
The silica gel of equal parts carbon nanotube, with the increase of the grafting amount of Silicage-polymer- bonded phase compound A, the dielectric constant of composite material exists
It is constantly promoted, this is because interfacial polarization is produced between silica gel and phenyl ring after being grafted compound A, so that being situated between
Electric constant increases；On the other hand, the pi-pi accumulation between carbon nanotube and benzene ring compound acts on the dispersion of increased carbon nanotube
Property, so that the dielectric constant of homogeneous composite material is further promoted.The dosage of fixed compound A, the carbon for adding different numbers are received
After mitron, the dielectric constant of composite material is further promoted.Although compound A has plane rigid structure, due to grafting
Measure simultaneously few, so dielectric loss and elastic modulus change and little, modulus is still less than 1MPa.
Claims (10)
1. a kind of silica gel/carbon nanotube dielectric elastomer composite material, it is characterised in that the composite material is by including following
The raw material of component is prepared, based on parts by weight:
Wherein, the carboxyl graft modification silicon rubber is obtained by the grafted polar small organic molecule on silicon rubber, silicon rubber
The contents of ethylene of glue is 0.5%~5%.
2. silica gel/carbon nanotube dielectric elastomer composite material according to claim 1, it is characterised in that the composite wood
Material is by including that the raw material of following components is prepared, based on parts by weight:
3. dielectric elastomer composite material according to claim 1, it is characterised in that:
More benzene ring compounds are-three polyindene of 5,5,10,10,15,15- Hexaethyl -2,7,12- triamido.
4. dielectric elastomer composite material according to claim 1, it is characterised in that:
The silicon rubber is methyl vinyl silicone rubber, methyl vinyl phenyl silicon rubber, methyl ethylene trifluoro propyl silicon rubber
At least one of glue.
5. dielectric elastomer composite material according to claim 1, it is characterised in that:
The polarity small organic molecule is selected from mercaptopropionic acid or thioacetic acid.
6. dielectric elastomer composite material according to claim 1, it is characterised in that:
The carboxyl grafting rate of the carboxyl graft modification silicon rubber is 0.5%~5%.
7. dielectric elastomer composite material according to claim 1, it is characterised in that:
The array carbon nano tube length is 50~100 μm, and caliber is 6~8nm.
8. dielectric elastomer composite material according to claim 1, it is characterised in that:
The catalyst is selected from N, N'- Dicyclohexylcarbodiimide, 1- (3- dimethylamino-propyl) -3- ethyl carbodiimide hydrochloride
At least one of salt.
9. a kind of preparation of described in any item silica gel/carbon nanotube dielectric elastomer composite materials according to claim 1~8
Method, it is characterised in that the following steps are included:
Carboxyl graft modification silicon rubber is dissolved in solvent by step 1, forms uniform silica gel solution a by stirring；
More benzene ring compounds are added in solution a by step 2, and catalyst is added, and are heated to 30~65 DEG C, react 3~8h, hair
Raw condensation reaction, by drying, the modified silica-gel b for purifying to be grafted more benzene ring compounds；
Step 3 plasticates silica gel b, and the array carbon nano tube and crosslinking agent is added, is kneaded uniform after cure, obtains the silicon
Glue/carbon nanotube dielectric elastomer composite material.
10. the preparation method of silica gel/carbon nanotube dielectric elastomer composite material according to claim 9, feature exist
In:
In step 3, slice is parked 7~9h and is vulcanized again after being kneaded uniformly, and curing temperature is 150~180 DEG C, and vulcanization time is
1~2min.
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|---|---|---|---|---|
| CN103214707A (en) * | 2013-04-17 | 2013-07-24 | 北京化工大学 | High-dielectric elastomer composite material with low content of carbon nanometer tubes and preparation method of composite material |
| CN105131218A (en) * | 2015-07-31 | 2015-12-09 | 北京化工大学 | Method for improving dielectric property of elastomer |
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