CN102558586A - Preparation method of polyethylene-vinyl acetate composite film - Google Patents
Preparation method of polyethylene-vinyl acetate composite film Download PDFInfo
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- CN102558586A CN102558586A CN2011104177492A CN201110417749A CN102558586A CN 102558586 A CN102558586 A CN 102558586A CN 2011104177492 A CN2011104177492 A CN 2011104177492A CN 201110417749 A CN201110417749 A CN 201110417749A CN 102558586 A CN102558586 A CN 102558586A
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Abstract
The invention relates to a preparation method of a polyethylene-vinyl acetate composite film, belonging to the field of modification and preparation of high-conductivity materials. Conducting polymers and graphene are utilized to modify polyethylene-vinyl acetate (EVA), and an in-situ polymerization method is utilized to obtain the high-conductivity composite material. Compared with the existing modified high molecular material (including doping carbon nanotubes, carbon fibers and the like), the graphene-polyaniline codoped EVA material has the advantages of much higher conductivity and lower manufacturing cost.
Description
Technical field
The present invention relates to a kind of preparation method of plastic of poly vinyl acetate composite package; Promptly utilize conductive polymers and Graphene modified poly ethylene vinyl acetate (EVA); The employing situ aggregation method obtains the matrix material of high conductivity, belongs to the modification preparation field of high conducting material.
Background technology
Compare with the intrinsically conducting macromolecular material; The conductive polymeric composite that is composited by conducting medium and macromolecular material because of the polymer kind extensively, be easy to suitability for industrialized production, be easy to advantage such as machine-shaping, be widely used in conduction, antistatic, planar heat producing body, anti-EMI, field such as explosion-proof.Present alternative conducting medium mainly contains metal system and charcoal system; At traditional charcoal is in the conducting medium; The application of carbon black (CCB) and thomel (CF) is the most extensive; But these carbon element media generally need bigger addition just can make macromolecular material reach the ideal conductivity; Therefore, when conducting mediums such as using carbon black and graphite carries out property modification to macromolecular material, tend to produce degradation problem under material mechanical performance, heat-resistant stability ability and the processing characteristics.Since finding carbon nanotube, carbon nanotube is also developed conductive polymers as main doping agent; The doping 30% sooty plastic of poly vinyl acetate of on CARBON, reporting in 2011 (EVA), the EVA of 15% thomel that mixes, the EVA of 5% carbon nanotube that mixes, its specific conductivity is respectively 2.5 * 10
-6S/cm, 5.0 * 10
-5S/cm, 2.5 * 10
-4S/cm.
After Graphene in 2004 is prepared successfully by geim seminar of Univ Manchester UK through " micromechanics is peeled off " method, become the most attracting research focus of material circle, chemical boundary and Condensed Matter Physics circle; Graphene relies on its excellent electroconductibility and extremely low add-on; Become a kind of conductive modified agent that has potentiality; Carry out the Graphene and the aqueous polyurethane of thermal treatment gained compound like Anjanapura etc. through solution combined and situ aggregation method; When the Graphene content that adds was 3 wt%, the specific conductivity of aqueous polyurethane/graphene complex was 2.24 * 10
-4S/cm [A. V. Raghu; Y. R. Lee; H. M. Jeong, C. M. Shin, et al. Preparation and Physical Properties of Waterborne Polyurethane/Functionalized Graphene Sheet Nanocomposites. Macromol. Chem. Phys. 2008; 209,2487-2493].
Electron propagation ducts pattern different from the past is like line-line connecting passage pattern: conductive doped polymkeric substance (like polyacetylene, polypyrrole, Polythiophene); Post--post connecting passage pattern: doped carbon nanometer pipe; Face--face connecting passage pattern: doped graphene; The object of the present invention is to provide a kind of mentality of designing of brand-new composite conductive polymer material, designed a kind of brand-new heterogeneous composite conducting material that launches to make up conductive network with line-facial bone shut die type; Promptly utilize Graphene and conducting polymer as doping agent, the preparation composite conducting material.Such mixture, the microchannel form of its transmission electronic has: line-line, line-face, face-face, thus conductive channel quantity increases greatly, causes conductivity to promote greatly.And utilize this mentality of designing, and having prepared the EVA material of Graphene and Polyaniline Doped, its specific conductivity has reached 0.1S/cm.
Summary of the invention
The present invention designs a kind of line-face-line bonded novel conductive model; With Graphene (GNS); Polyaniline (PANI) is the matrix material that main doping agent increase conductive channel and the method for utilizing in-situ polymerization successfully synthesize GNS/ PANI/ EVA high conductivity, can be widely used in the cable shield material, antistatic material; Area of solar cell etc. have great application prospect.
The invention has the beneficial effects as follows:
With respect to existing modified polymer material (comprising doping vario-properties such as utilizing carbon nanotube, thomel), the electroconductibility of the EVA material that Graphene and polyaniline are composite mixed improves a lot, and low cost of manufacture.
The present invention specifically implements by following step:
The first step: prepare graphene oxide through chemical oxidation;
Second step: the graphene oxide of preparing thermal reduction is at high temperature become Graphene;
The 3rd step: select for use suitable solvent to adopt situ aggregation method to prepare the composite solution of Graphene and polyaniline at low temperatures; The mass ratio of Graphene and polyaniline is 1:2 ~ 1:4 in the composite solution of Graphene and polyaniline, and the mass percentage concentration of Graphene is controlled at 5% ~ 30% in the composite solution of Graphene and polyaniline;
The 4th step: plastic of poly vinyl acetate is mixed with solution, mixes, stir with the composite solution of Graphene and polyaniline, ultrasonic;
The 5th step: pour above-mentioned mixing solutions into mould, vacuum-drying, film forming.
The said method the first step is prepared graphite oxide with the graphite oxidation intercalation, and these methods include but not limited to: hummer method, staudenmair method.
In said second step of method, note under protection of inert gas 700 ℃ ~ 1100 ℃ of characteristic temperature scopes.
The 3rd step of said method, employing be situ aggregation method, keep pH value to be not more than 3, polymerization temperature is less than 20 ℃; Said suitable solvent is the N SL 1332.
The concrete preparation method in the 3rd step of said method is: adding mass percentage concentration to three-necked bottle under 0 ~ 10 ℃ is 1 ~ 2% X 2073 solution, drips aniline monomer, adds the skimmer propyl carbinol, adds 2mg/ml
Graphene solution, add hydrochloric acid and regulate pH value to 1 ~ 3, stir, dripping mass percentage concentration is the ammonium persulphate of 5 ~ 15 %; Reaction 4 ~ 8 h filter, and use acetone respectively; Distilled water wash is neutral to PH, 50 ~ 80 ℃ of following vacuum-drying 24 ~ 48 h, and dissolve with N-Methyl pyrrolidone; The add-on of skimmer and aniline monomer volume ratio are 300:1 ~ 500:1; X 2073 and aniline monomer mol ratio are 1.5:1 ~ 1.8:1; Graphene add-on and aniline monomer mass ratio are 1:2 ~ 1:4, and the add-on of ammonium persulphate and aniline monomer mol ratio are 2.5:1 ~ 3:1.
Said the 4th step of method; With the mixed solvent dissolving of plastic of poly vinyl acetate with YLENE and N-Methyl pyrrolidone; The YLENE of per 60 ~ 90 ml and the mixed solvent of N-Methyl pyrrolidone dissolving 1.88 ~ 2.2 gram plastic of poly vinyl acetate; The volume ratio of YLENE and N-Methyl pyrrolidone is 1:1 ~ 3:1 in YLENE and the N-Methyl pyrrolidone mixed solvent, with the composite solution stirring of Graphene and polyaniline, ultrasonic 2 ~ 5h.
In said the 5th step of method, temperature is controlled at 50 ~ 80 ℃, vacuum-drying 24 ~ 48 h.
Description of drawings
Fig. 1 is the AFM figure of used Graphene in instance one, instance three, the instance four, and AFM figure display piece layer thickness is about 0.6 nm, and interpret sample is a single-layer graphene;
Fig. 2 is the optical photograph of composite conductive film in the instance four, has as can be seen from the figure prepared complete laminated film, its smooth surface, even;
Fig. 3 is the SEM figure of composite conductive film in the instance four, can find out that from SEM figure Graphene, polyaniline are relatively good at the EVA dispersive, does not significantly reunite;
A among Fig. 4; B and c curve are respectively the change curve of the AC conductivity of Comparative Examples 1, instance three and instance four composite packages with frequency; Sample in Comparative Examples 2 sample test curves and the instance one is similar; As can be seen from the figure the laminated film specific conductivity in the instance one increases along with the increase of frequency; Explanation does not form conductive network in laminated film, and instance three is constant basically along with frequency with the laminated film specific conductivity in the instance four, explains to have formed conductive network in the laminated film; Thereby explain that being mixed with altogether of Graphene and PANI is beneficial to the formation conductive network, thereby also can make up conductive network by side light Graphene/PANI/EVA matrix material with line-facial bone shut die type.
Embodiment
Further specify content of the present invention below in conjunction with instance:
Vinyl acetate content is 14 % among the EVA that is adopted, and specific conductivity is 5 * 10
-15S/cm.
Comparative Examples 1:
The preparation of Graphene/EVA (mass ratio 2:98) laminated film
1, the preparation of graphite oxide: utilize improved staudenmair method, in 98% the vitriol oil, add natural flake graphite, HNO
3And KClO
3, 10 ℃ of control reacting liquid temperatures behind stirring reaction 5 h, refilter the reaction solution dilution with deionized water, and the ionized water thorough washing is until neutrality, and is dry then.
2, with graphene oxide under the condition of nitrogen protection, rise to 1000 ℃ of thermal reduction 30 s.
3,40 mg Graphenes are made into the solution of 2 mg/ml with 20 ml N-Methyl pyrrolidone; Join wiring solution-forming in the 60 ml YLENE to 1.98g EVA; Above-mentioned two kinds of solution are mixed, stir 2 h, ultrasonic 4 h.
4, pour ultrasonic uniform solution into mould under 50 ℃, vacuum-drying 48 h, the demoulding, recording specific conductivity is 3.26 * 10
-5S/cm.
Comparative Examples 2:
The preparation of PANI/EVA (mass ratio 5:95) laminated film
1, the preparation of polyaniline: 5
oThree-necked bottle adding mass concentration to 250ml under the C is 1.25% X 2073 (DBSA), 60 ml, drips the 0.002mol aniline monomer, adds skimmer propyl carbinol 40ml; Add hydrochloric acid and regulate pH value to 2, stir, dripping mass concentration is 15% ammonium persulphate (APS) 70ml reaction 9h; Filter; Use acetone respectively, distilled water wash is neutral to PH, 60
oVacuum-drying 24h under the C.
2, take by weighing 0.1g PANI is made into 10mg/ml with the 10mlN-SL 1332 solution; Join wiring solution-forming in the 60ml YLENE to 1.98g EVA; These two kinds of solution are mixed, stir 2h, ultrasonic 4h.
3, pour ultrasonic uniform solution into mould under 75 ℃, vacuum-drying 30h, the demoulding, recording specific conductivity is 7.52 * 10
-5S/cm.
Instance three: Graphene/PANI/EVA laminated film (mass ratio is 2:5:93)
1, with the step 1 in the instance one.
2, with the step 2 in the instance one.
3, the preparation of the composite solution of Graphene and polyaniline:
5
oThree-necked bottle adding mass concentration to 250 ml under the C is 1.25 % X 2073es (DBSA), 30 ml, drips 0.1 ml aniline monomer, adds skimmer propyl carbinol 40ml; Add 2 mg/ml Graphene solution, 20 ml, add hydrochloric acid and regulate pH value to 2, stir; Dripping mass concentration is that 15% ammonium persulphate (APS), 40 ml react 9 h, filters, and uses acetone respectively; Distilled water wash is neutral to PH, 60
oVacuum-drying 24 h under the C, and dissolve with 100 ml N-Methyl pyrrolidone.
4, with 1.88g EVA with YLENE and N-Methyl pyrrolidone mixed solvent wiring solution-forming; The volume of YLENE and N-Methyl pyrrolidone mixed solvent is 60 ml; The volume ratio of YLENE and N-Methyl pyrrolidone is 2:1 in YLENE and the N-Methyl pyrrolidone mixed solvent; Mixed mechanical stirring 3 h, and ultrasonic 4 h with the Graphene in last step and the composite solution of polyaniline.
5, pour ultrasonic uniform solution into mould under 75 ℃, vacuum-drying 30 h, the demoulding, recording specific conductivity is 7.52 * 10
-3S/cm.
Instance four: the preparation of Graphene/PANI/EVA laminated film (mass ratio is 4:8:88)
1, with the step 1 in the instance one
2, with the step 2 in the instance one
3, the preparation of the composite solution of Graphene and polyaniline: 0
oThree-necked bottle adding mass concentration to 250 ml under the C is 1.25 % X 2073es (DBSA), 60 ml, drips 0.002 mol aniline monomer, adds skimmer propyl carbinol 40 ml; Add 2 mg/ml Graphene solution, 50 ml, add hydrochloric acid and regulate pH value to 2, stir; Dripping mass concentration is that 15 % ammonium persulphates (APS), 70 ml react 9 h, filters, and uses acetone respectively; Distilled water wash is neutral to PH, 60
oVacuum-drying 24 h under the C, and dissolve with 75 ml N-Methyl pyrrolidone.
4, with 2.2g EVA with YLENE and N-Methyl pyrrolidone mixed solvent wiring solution-forming; The volume of YLENE and N-Methyl pyrrolidone mixed solvent is 90 ml; The volume ratio of YLENE and N-Methyl pyrrolidone is 3:1 in YLENE and the N-Methyl pyrrolidone mixed solvent, mixes mechanical stirring 3h with the Graphene in the 3rd step and the composite solution of polyaniline; And ultrasonic 2 h, the content of Graphene in the matrix material of preparation: polyaniline: EVA is respectively 4wt%:8wt%: 88wt%.
5, pour the composite solution that mixes into mould under 50 ℃, vacuum-drying 48 h, the demoulding, prepared composite conducting film specific conductivity is 1.07 * 10
-1S/cm.
Claims (7)
1. the preparation method of a plastic of poly vinyl acetate composite package comprises the steps:
(1) prepares graphene oxide through chemical oxidation;
(2) graphene oxide of preparing thermal reduction is at high temperature become Graphene;
(3) select for use suitable solvent to adopt situ aggregation method to prepare the composite solution of Graphene and polyaniline at low temperatures; The mass ratio of Graphene and polyaniline is 1:2 ~ 1:4 in the composite solution of Graphene and polyaniline, and the mass percentage concentration of Graphene is controlled at 5% ~ 30% in the composite solution of Graphene and polyaniline;
(4) plastic of poly vinyl acetate is mixed with solution, mixes, stir with the composite solution of Graphene and polyaniline, ultrasonic;
(5) pour above-mentioned mixing solutions into mould, vacuum-drying, film forming.
2. the preparation method of a kind of plastic of poly vinyl acetate composite package as claimed in claim 1 is characterized in that: in the said step 1, the method for the graphite oxidation intercalation being prepared graphite oxide includes but not limited to: hummer method, staudenmair method.
3. the preparation method of a kind of plastic of poly vinyl acetate composite package as claimed in claim 1 is characterized in that: said step 2 should be carried out under protection of inert gas, 700 ℃ ~ 1100 ℃ of TRs.
4. the preparation method of a kind of plastic of poly vinyl acetate composite package as claimed in claim 1 is characterized in that: what said step 3 adopted is situ aggregation method, keeps pH value to be not more than 3, and polymerization temperature is less than 20 ℃; Said suitable solvent is the N SL 1332.
5. like the preparation method of claim 1 or 4 described a kind of plastic of poly vinyl acetate composite packages; It is characterized in that: the concrete preparation method of said step 3 is: adding mass percentage concentration to three-necked bottle under 0 ~ 10 ℃ is 1 ~ 2% X 2073 solution; Drip aniline monomer; Add the skimmer propyl carbinol, add 2mg/ml
Graphene solution, add hydrochloric acid and regulate pH value to 1 ~ 3, stir, dripping mass percentage concentration is the ammonium persulphate of 5 ~ 15 %; Reaction 4 ~ 8 h filter, and use acetone respectively; Distilled water wash is neutral to PH, 50 ~ 80 ℃ of following vacuum-drying 24 ~ 48 h, and dissolve with N-Methyl pyrrolidone; The add-on of skimmer and aniline monomer volume ratio are 300:1 ~ 500:1; X 2073 and aniline monomer mol ratio are 1.5:1 ~ 1.8:1; Graphene add-on and aniline monomer mass ratio are 1:2 ~ 1:4, and the add-on of ammonium persulphate and aniline monomer mol ratio are 2.5:1 ~ 3:1.
6. the preparation method of a kind of plastic of poly vinyl acetate composite package as claimed in claim 1; It is characterized in that: the concrete preparation method of said step 4 is: with the mixed solvent dissolving of plastic of poly vinyl acetate with YLENE and N-Methyl pyrrolidone; The YLENE of per 60 ~ 90 ml and the mixed solvent of N-Methyl pyrrolidone dissolving 1.88 ~ 2.2 gram plastic of poly vinyl acetate; The volume ratio of YLENE and N-Methyl pyrrolidone is 1:1 ~ 3:1 in YLENE and the N-Methyl pyrrolidone mixed solvent; Stir ultrasonic 2 ~ 5h with the composite solution of Graphene and polyaniline.
7. the preparation method of a kind of plastic of poly vinyl acetate composite package as claimed in claim 1 is characterized in that: said step 5 temperature is controlled at 50 ~ 80 ℃, vacuum-drying 24 ~ 48 h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104448303A (en) * | 2014-11-20 | 2015-03-25 | 河南城建学院 | Ethylene-vinyl acetate copolymer/polyaniline composite conductive material and preparation method thereof |
| CN105131408A (en) * | 2015-06-26 | 2015-12-09 | 中国航空工业集团公司北京航空材料研究院 | Graphene semiconductor shield material |
| CN105461948A (en) * | 2015-11-23 | 2016-04-06 | 南京航空航天大学 | Preparation method of conductive macromolecule non-covalent functionalized graphene modified electrokinetic energy conversion polymer material |
| CN107011568A (en) * | 2017-04-19 | 2017-08-04 | 上海电气集团股份有限公司 | Composite graphite alkene/carbon black is the semi-conducting polymer and preparation method of conducting medium |
| CN108878796A (en) * | 2017-05-16 | 2018-11-23 | 天津大学 | Graphene modified conductive polymer gel and its preparation method and application |
| CN109370226A (en) * | 2018-10-24 | 2019-02-22 | 嘉兴市海德姆智能电气有限公司 | A kind of preparation method of electromagnetic shielding material |
| CN109627562A (en) * | 2018-12-20 | 2019-04-16 | 中山大学 | A kind of preparation method and application of conducing composite material |
| CN113265090A (en) * | 2021-05-14 | 2021-08-17 | 东北大学 | Preparation method for coating polyaniline-doped graphene surface |
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| EP2036941A1 (en) * | 2007-09-13 | 2009-03-18 | Stichting Dutch Polymer Institute | Process for the preparation of a conductive polymer composition |
| CN101798462A (en) * | 2010-03-26 | 2010-08-11 | 武汉工程大学 | Graphene/conductive polymer composite film and preparation method thereof |
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2011
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2036941A1 (en) * | 2007-09-13 | 2009-03-18 | Stichting Dutch Polymer Institute | Process for the preparation of a conductive polymer composition |
| CN101798462A (en) * | 2010-03-26 | 2010-08-11 | 武汉工程大学 | Graphene/conductive polymer composite film and preparation method thereof |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104448303A (en) * | 2014-11-20 | 2015-03-25 | 河南城建学院 | Ethylene-vinyl acetate copolymer/polyaniline composite conductive material and preparation method thereof |
| CN104448303B (en) * | 2014-11-20 | 2016-09-21 | 河南城建学院 | A kind of ethylene-vinyl acetate copolymer/polyaniline composite conducting material and preparation method thereof |
| CN105131408A (en) * | 2015-06-26 | 2015-12-09 | 中国航空工业集团公司北京航空材料研究院 | Graphene semiconductor shield material |
| CN105461948A (en) * | 2015-11-23 | 2016-04-06 | 南京航空航天大学 | Preparation method of conductive macromolecule non-covalent functionalized graphene modified electrokinetic energy conversion polymer material |
| CN107011568A (en) * | 2017-04-19 | 2017-08-04 | 上海电气集团股份有限公司 | Composite graphite alkene/carbon black is the semi-conducting polymer and preparation method of conducting medium |
| CN107011568B (en) * | 2017-04-19 | 2019-12-20 | 上海电气集团股份有限公司 | Semiconductor polymer with composite graphene/carbon black as conductive medium and preparation method thereof |
| CN108878796A (en) * | 2017-05-16 | 2018-11-23 | 天津大学 | Graphene modified conductive polymer gel and its preparation method and application |
| CN109370226A (en) * | 2018-10-24 | 2019-02-22 | 嘉兴市海德姆智能电气有限公司 | A kind of preparation method of electromagnetic shielding material |
| CN109627562A (en) * | 2018-12-20 | 2019-04-16 | 中山大学 | A kind of preparation method and application of conducing composite material |
| CN109627562B (en) * | 2018-12-20 | 2020-05-26 | 中山大学 | Preparation method and application of conductive composite material |
| CN113265090A (en) * | 2021-05-14 | 2021-08-17 | 东北大学 | Preparation method for coating polyaniline-doped graphene surface |
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