CN102977533B - Conductive high-polymer composite material and preparation method thereof - Google Patents
Conductive high-polymer composite material and preparation method thereof Download PDFInfo
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- CN102977533B CN102977533B CN201210493855.3A CN201210493855A CN102977533B CN 102977533 B CN102977533 B CN 102977533B CN 201210493855 A CN201210493855 A CN 201210493855A CN 102977533 B CN102977533 B CN 102977533B
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- polyaniline
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 229920000642 polymer Polymers 0.000 title claims abstract 4
- 238000002360 preparation method Methods 0.000 title claims description 18
- 229920000767 polyaniline Polymers 0.000 claims abstract description 47
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 33
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 33
- 239000004800 polyvinyl chloride Substances 0.000 claims abstract description 33
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 26
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 26
- 239000011159 matrix material Substances 0.000 claims description 26
- 239000003960 organic solvent Substances 0.000 claims description 26
- 229920001940 conductive polymer Polymers 0.000 claims description 25
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 18
- 238000013019 agitation Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000007669 thermal treatment Methods 0.000 claims description 6
- 238000011282 treatment Methods 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910021392 nanocarbon Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 16
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000007772 electrode material Substances 0.000 abstract description 3
- 230000007935 neutral effect Effects 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- -1 carbon nano tube compound Chemical class 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- OIRDTQYFTABQOQ-UHTZMRCNSA-N Vidarabine Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](CO)[C@@H](O)[C@@H]1O OIRDTQYFTABQOQ-UHTZMRCNSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 210000000617 arm Anatomy 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001246 colloidal dispersion Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SMPAPEKFGLKOIC-UHFFFAOYSA-N oxolane;hydrochloride Chemical compound Cl.C1CCOC1 SMPAPEKFGLKOIC-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a method for preparing a conductive high-polymer composite material. The method is a method for preparing a polyaniline carbon nano tube composite material based on polyvinyl chloride (PVC) and polymethyl methacrylate (PAMM). The conductive high-polymer composite material prepared by the method is simple in forming process, high in mechanical performance and high in electric conductivity and can serve as an electrode material in a neutral and acidic environment or serve as a corrosion-resistant conductive coating material.
Description
Technical field
The present invention relates to a kind of conductive polymer composite and preparation method thereof, especially the blended base polyaniline of PVC and PAMM, carbon nano tube compound material and preparation method thereof.
Background technology
Polyaniline is a kind of conducting polymer composite having application prospect most, because it has good thermostability, and chemical stability and electrochemical reversibility, excellent microwave absorption performance, raw material is easy to get, simple synthetic method, also has the characteristics such as unique doping phenomenon.At present in the progress attracted people's attention that the Synthesis and applications research of polyaniline all obtains, but be no matter be all powder body material by chemical oxidation or the polyaniline of electrochemical production, be difficult in actual applications form processing.Around polyaniline shaping applied research, people have carried out a lot of effort.Successively polyaniline film material, polyaniline modified electrode material, Polyaniline-modified sensor, electromagnetic screen coating, metal device protective system are there is, these researchs concentrate on and do not consider polyaniline material to make large volume electro-conductive material from the physical properties of powder body material powder, and only consider that it is as modifying and the application of mould material.In consideration large volume polyaniline formation treatment process, occurred the methods such as blended, altogether molten, the congruent melting of water-soluble polyaniline, polyaniline and conventional macromolecular material, copolymerization, the target of these methods is that prepare can the polyaniline large volume material of practical application; In addition, some investigators are investigated static pressure shaped material and are applied to anhydrous system.In addition, Vincent and Armes etc. also put forward to develop aqueous phase colloidal dispersion system is solve the important method being difficult to forming process shortcoming.Be developed polyaniline-coated inorganic nanoparticles (such as SiO
2, TiO
2, WC etc.) etc. material, the materials such as polyaniline-coated organic nanometer granule (such as PS, PMMA etc.).These have the material of polyaniline-coated can solve the processibility of polyaniline to a certain extent.For conducting polymer composite, a shortcoming is also had to be exactly that electric conductivity still can not match in excellence or beauty with metallographic phase.
The shortcoming of formed machining this self is difficult to for polyaniline, the invention provides a kind of method can preparing large volume and large-area polyaniline composite material, the method can not only solve the Problems in forming of polyaniline, the matrix material obtained can also be made to have higher electric conductivity, and the composite conducting material of preparation is owing to having the skeleton structure of organic macromolecule, matrix material effectively can overcome the distortion because polyaniline water suction volume growth causes, so this matrix material can be applied to the system of water.
Summary of the invention
The object of the invention is the preparation method providing a kind of conductive polymer composite, this is the preparation method of a kind of polyvinyl chloride (PVC) and the blended base polyaniline of polymethylmethacrylate (PAMM), carbon nano tube compound material, and the conductive polymer composite adopting method of the present invention to prepare has that physical properties is stable, electric conductivity is high, be easy to the features such as formed machining.
Present invention process flow process and process control condition as follows:
1. carbon nanotube and polyaniline ultrasonic disperse are formed stable dispersion system in organic solvent, ultrasonic time is: 30 ~ 45min, dispersion system to be sealed in ultrasonic disperse process, in case organic solvent volatilization, the dispersion system that ultrasonic disperse is good keeps for subsequent use under agitation, wherein the consumption of carbon nanotube accounts for 1 ~ 30% of final obtained matrix material quality, the addition of polyaniline accounts for 20 ~ 65% of final obtained matrix material quality, and organic solvent addition is the fully effective dispersing Nano carbon tubes of energy and polyaniline;
2. polymethylmethacrylate and polyvinyl chloride are dissolved obtained mixing solutions in organic solvent, wherein the consumption of polymethylmethacrylate and polyvinyl chloride (PVC) Compound is to account for 30% ~ 70% of final obtained matrix material quality, and the mass ratio of polymethylmethacrylate and polyvinyl chloride is 1:4 ~ 4:1; Choosing of organic solvent is identical with step kind 1., and organic solvent addition is for can dissolve polymethylmethacrylate and polyvinyl chloride completely;
3. the solution that 2. 1. step prepared with step is mixed under whipped state, and be heated to 45 DEG C ~ 60 DEG C volatile organic solvent under agitation, obtain the viscous state mixture that viscosity is higher, viscous state mixture is carried out room temperature repeatedly casting forming in forming molds, the thickness of every layer of casting is less than 0.5cm, after having cast, sample is heated to 100 DEG C ~ 150 DEG C thermal treatments 2 ~ 3 hours, namely obtains conductive polymer composite.
Described in the present invention, 1., 2. the processing step of part can also be: first by polyaniline and carbon nanotube dispersed dissolved polymethylmethacrylate (PMMA) or polyvinyl chloride (PVC) organic solution (selection of organic solvent and step 1. with 2. in identical) in, mixing solutions obtains stable dispersion system through ultrasonic disperse, again by dispersion system and the polyvinyl chloride dissolved (PVC) or polymethylmethacrylate (PMMA) organic solution (selection of organic solvent and step 1. with 2. in identical) blended, stirring heating, shaping, after heat treated, namely conductive polymer composite is obtained, the amount preparing the raw material of matrix material in this process and step 1. with 2. in the amount chosen identical.
Organic solvent described in the present invention is a kind of in tetrahydrofuran (THF), chloroform, N-Methyl pyrrolidone.
Carbon nanotube described in the present invention is commercial carbon nanotube through volume ratio is that the vitriol oil of 3:1 and concentrated nitric acid mixing acid obtain 50 DEG C ~ 60 DEG C activation treatment for 3 ~ 5 hours.
Another object of the present invention is to provide a kind of conductive polymer composite.
The present invention is relative to the advantage of prior art and technique effect:
(1) PVC and PAMM blended base polyaniline, the carbon nano tube compound material forming technology prepared of the present invention is simple, by situ aggregation method by polyaniline-coated in carbon nano tube surface, good mechanical property, the electric conductivity of the matrix material prepared by present method are high, also possess the advantages such as the catalytic activity of polyaniline, can as the electrode materials of neutral and acid environment or as anticorrosion, conductive coating materials use;
(2) the inventive method can not only solve the Problems in forming of polyaniline, the matrix material obtained can also be made to have higher electric conductivity, large volume and large-area polyaniline composite material can be obtained by present method, and the composite conducting material of preparation has the skeleton structure of organic macromolecule, matrix material effectively can overcome the distortion because polyaniline water suction volume growth causes, so this matrix material can be applied to the system of water.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but scope is not limited to described content.
embodiment 1: thisthe preparation method of conductive polymer composite, particular content is as follows:
1. 0.3g carbon nanotube and 1.2g polyaniline ultrasonic disperse are formed stable dispersion system in 20ml tetrahydrofuran (THF), ultrasonic frequency is 40KHZ, ultrasonic time 40min, ultrasonic disperse process is carried out under air-proof condition, the dispersion system that ultrasonic disperse is good is for subsequent use under agitation, wherein the addition of carbon nanotube is 10% of final obtained matrix material quality, the addition of polyaniline is 40% of final obtained matrix material quality, and organic solvent addition is energy dissolved carbon nanotube and polyaniline completely;
2. 1.0g polymethylmethacrylate and 0.5g polyvinyl chloride are dissolved in 50ml tetrahydrofuran (THF), magnetic agitation obtains mixing solutions, wherein the consumption of polymethylmethacrylate and polyvinyl chloride (PVC) Compound is 50% of final obtained matrix material quality, the mass ratio of polymethylmethacrylate and polyvinyl chloride is 2:1, and organic solvent addition is for can dissolve polymethylmethacrylate and polyvinyl chloride completely;
3. the solution that 2. 1. step prepared with step is mixed under whipped state, and be heated to 50 DEG C of volatile organic solvent under agitation, obtain the viscous state mixture that viscosity is higher, by viscous state mixture at room temperature, casting forming in the bulge that diameter is 4cm, the thickness of every layer of casting is less than 0.5cm, sample is heated to 130 DEG C of thermal treatments 2 hours after having cast, namely conductive polymer composite is obtained, gained sample electric conductivity 12S/cm, thickness: 1.5mm.
embodiment 2: thisthe preparation method of conductive polymer composite, particular content is as follows:
1. 0.96g carbon nanotube (be that the vitriol oil of 3:1 and concentrated nitric acid mixing acid 60 DEG C activation treatment 3 hour obtain through volume ratio) and 0.64g polyaniline ultrasonic disperse are formed stable dispersion system in 20ml chloroform, ultrasonic frequency is 40KHZ, ultrasonic time 30min, ultrasonic disperse process is carried out under air-proof condition, the dispersion system that ultrasonic disperse is good is for subsequent use under agitation, wherein the addition of carbon nanotube is 30% of final obtained matrix material quality, the addition of polyaniline is 20% of final obtained matrix material quality, organic solvent addition is energy dissolved carbon nanotube and polyaniline completely,
2. 1.2g polymethylmethacrylate and 0.4g polyvinyl chloride are dissolved in 50ml chloroform, magnetic agitation obtains mixing solutions, wherein the consumption of polymethylmethacrylate and polyvinyl chloride (PVC) Compound is 50% of final obtained matrix material quality, the mass ratio of polymethylmethacrylate and polyvinyl chloride is 3:1, and organic solvent addition is for can dissolve polymethylmethacrylate and polyvinyl chloride completely;
3. the solution that 2. 1. step prepared with step is mixed under whipped state, and be heated to 45 DEG C of volatile organic solvent under agitation, obtain the viscous state mixture that viscosity is higher, by viscous state mixture at room temperature, casting forming in the bulge that diameter is 4cm, the thickness of every layer of casting is less than 0.5cm, sample is heated to 100 DEG C of thermal treatments 3 hours after having cast, namely conductive polymer composite is obtained, gained sample electric conductivity 19S/cm, thickness: 1.7mm.
embodiment 3: thisthe preparation method of conductive polymer composite, particular content is as follows:
1. 0.04g carbon nanotube (be that the vitriol oil of 3:1 and concentrated nitric acid mixing acid 55 DEG C activation treatment 4 hour obtain through volume ratio) and 2.6g polyaniline ultrasonic disperse are formed stable dispersion system in 20ml N-Methyl pyrrolidone, ultrasonic frequency is 40KHZ, ultrasonic time 45min, ultrasonic disperse process is carried out under air-proof condition, the dispersion system that ultrasonic disperse is good is for subsequent use under agitation, wherein the addition of carbon nanotube is 1% of final obtained matrix material quality, the addition of polyaniline is 65% of final obtained matrix material quality, organic solvent addition is energy dissolved carbon nanotube and polyaniline completely,
2. 0.272g polymethylmethacrylate and 1.088g polyvinyl chloride are dissolved in 50ml N-Methyl pyrrolidone, magnetic agitation obtains mixing solutions, wherein the consumption of polymethylmethacrylate and polyvinyl chloride (PVC) Compound is 34% of final obtained matrix material quality, the mass ratio of polymethylmethacrylate and polyvinyl chloride is 1:4, and organic solvent addition is for can dissolve polymethylmethacrylate and polyvinyl chloride completely;
3. the solution that 2. 1. step prepared with step is mixed under whipped state, and be heated to 60 DEG C of volatile organic solvent under agitation, obtain the viscous state mixture that viscosity is higher, by viscous state mixture at room temperature, casting forming in the bulge that diameter is 4cm, the thickness of every layer of casting is less than 0.5cm, sample is heated to 150 DEG C of thermal treatments 2.5 hours after having cast, namely obtain conductive polymer composite, gained sample is electric conductivity 7S/cm, thickness: 3mm.
embodiment 4:the preparation method of this conductive polymer composite, particular content is as follows:
1. polyaniline and carbon nanotube (be that the vitriol oil of 3:1 and concentrated nitric acid mixing acid 55 DEG C activation treatment 4 hour obtain through volume ratio) are first dispersed in and have dissolved (addition of tetrahydrofuran (THF) is for dissolving polymethylmethacrylate completely) in the tetrahydrofuran solution of polymethylmethacrylate, mixing solutions obtains dispersion system after ultrasonic sealing dispersion 35min, again dispersion system is mixed under whipped state with the polyvinyl chloride tetrahydrofuran solution dissolved (addition of tetrahydrofuran (THF) is for dissolving polyvinyl chloride completely), wherein the addition of carbon nanotube is 10% of final obtained matrix material quality, the addition of polyaniline is 30% of final obtained matrix material quality, the consumption of polymethylmethacrylate and polyvinyl chloride (PVC) Compound is 60% of final obtained matrix material quality, the mass ratio of polymethylmethacrylate and polyvinyl chloride is 4:1,
2. the mixing solutions that 1. step obtains is heated to 55 DEG C of volatile organic solvent under agitation, obtain the viscous state mixture that viscosity is higher, by viscous state mixture at room temperature casting forming, the thickness of every layer of casting is less than 0.5cm, sample is heated to 140 DEG C of thermal treatments 2 hours after having cast, namely conductive polymer composite is obtained, gained sample electric conductivity 10S/cm, thickness: 2mm.
Claims (5)
1. a preparation method for conductive polymer composite, is characterized in that carrying out as follows:
1. carbon nanotube and polyaniline ultrasonic disperse are formed stable dispersion system in organic solvent, ultrasonic time 30 ~ 45min, ultrasonic disperse process is carried out under air-proof condition, the dispersion system that ultrasonic disperse is good is for subsequent use under agitation, wherein the addition of carbon nanotube is 1 ~ 30% of final obtained matrix material quality, the addition of polyaniline is 20 ~ 65% of final obtained matrix material quality, and organic solvent addition is the fully effective dispersing Nano carbon tubes of energy and polyaniline;
2. polymethylmethacrylate and polyvinyl chloride are dissolved in organic solvent, stir obtained mixing solutions, wherein the consumption of polymethylmethacrylate and polyvinyl chloride (PVC) Compound is 30% ~ 70% of final obtained matrix material quality, the mass ratio of polymethylmethacrylate and polyvinyl chloride is 1:4 ~ 4:1, and organic solvent addition is for can dissolve polymethylmethacrylate and polyvinyl chloride completely;
3. the solution that 2. 1. step prepared with step is mixed under whipped state, and be heated to 45 ~ 60 DEG C of volatile organic solvent under agitation, obtain the viscous state mixture that viscosity is higher, by viscous state mixture at room temperature casting forming, the thickness of every layer of casting is less than 0.5cm, after having cast, sample is heated to 100 DEG C ~ 150 DEG C thermal treatments 2 ~ 3 hours, namely obtains conductive polymer composite.
2. the preparation method of conductive polymer composite according to claim 1, it is characterized in that: during preparation, polyaniline and carbon nanotube are first dispersed in the organic solution of having dissolved the first polymkeric substance, mixing solutions obtains dispersion system through ultrasonic disperse, again dispersion system is mixed with the second polymer organic solution dissolved, stirring heating, shaping, after heat treated, namely obtain conductive polymer composite;
When the first polymkeric substance is polymethylmethacrylate, the second polymkeric substance is polyvinyl chloride;
When the first polymkeric substance is polyvinyl chloride, the second polymkeric substance is polymethylmethacrylate.
3. the preparation method of conductive polymer composite according to claim 1 and 2, is characterized in that: organic solvent is a kind of in tetrahydrofuran (THF), chloroform, N-Methyl pyrrolidone.
4. the preparation method of conductive polymer composite according to claim 1 and 2, is characterized in that: carbon nanotube is carbon nanotube through volume ratio is that the vitriol oil of 3:1 and concentrated nitric acid mixing acid obtain 50 DEG C ~ 60 DEG C activation treatment for 3 ~ 5 hours.
5. the conductive polymer composite that the preparation method of the conductive polymer composite described in claim 1 or 2 obtains.
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| CN103232781A (en) * | 2013-05-03 | 2013-08-07 | 昆明理工大学 | Preparation method of carbon-nanotube-reinforced polyaniline metal anticorrosive paint |
| CN104452298B (en) * | 2014-12-09 | 2016-08-24 | 丹东优耐特纺织品有限公司 | Anti-electromagnetic radiation WP and preparation method thereof |
| CN104667425B (en) * | 2015-02-28 | 2016-02-24 | 山东省千佛山医院 | A kind of defibrillator conduction electrocoagulation film |
| CN105200848B (en) * | 2015-08-09 | 2017-04-12 | 浙江理工大学 | Nanometer composite conductive paint and preparation method thereof |
| CN106810807A (en) * | 2017-02-13 | 2017-06-09 | 天津科技大学 | Polyaniline/composite material of polymethyl methacrylate and preparation method thereof |
| CN115364704B (en) * | 2022-10-25 | 2023-01-03 | 天津工业大学 | Polyacrylonitrile-carbon nano tube electroactive film with selective oxidation function and application |
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