CN101768316B - Preparation method of polyaniline/P (MMA-BA-HEA) conductive composite material - Google Patents
Preparation method of polyaniline/P (MMA-BA-HEA) conductive composite material Download PDFInfo
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Abstract
The invention relates to a preparation method of a polyaniline/P(MMA-BA-HEA) conductive composite material, which takes butyl acrylate, methyl methacrylate, hydroxyethyl acrylate and aniline as raw materials, and comprises the following steps: first, preparing a P(MMA-BA-HEA) emulsion by taking fatty alcohol-polyoxyethylene ether, sodium dodecyl benzene sulfonate and n-amyl alcohol as emulsifying agents and taking azo-diisopropyl-imidazoline as an initiator; and then obtaining the polyaniline (PANI)/P (MMA-BA-HEA) conductive composite material by the in situ polymerization of the aniline in the copolymer emulsion. The polyaniline conductive composite material of the invention has good conductivity and processability, the highest conductivity of the composite material is 1.472S. cm<-1>, the composite material PANI/P (MMA-BA-HEA) has good solubility in organic solvents, such as cyclohexanone, N-methylpyrrolidone and dimethyl sulfoxide, and the problems of processing difficulty and application of the polyaniline conductive material are solved.
Description
Technical field
The present invention relates to the preparation method of a kind of polyaniline/P (MMA-BA-HEA) conducing composite material.
Background technology
Polyaniline is a kind of novel high polymer electro-conductive material, and advantage such as have that cost of material is low, synthetic simple, electric conductivity is high, good in oxidation resistance, environmental stability are good becomes the focus of research.Up to the present obtain to use at aspects such as nano material, secondary cell, antistatic and electromagnetic shielding material, anticorrosive, ultracapacitor, selective permeation film, transmitter, molecular wire and molecular device, artificial-muscles.
But because polyaniline infusibility indissoluble, comprehensive mechanical property is poor, can't limit its application to a great extent with traditional method straight forming processing.At present, by mixing, prepare polyaniline derivative or copolymer polyaniline, the water base dispersoid of preparation polyaniline, preparing the processing characteristics that polyaniline composite material improves polyaniline.Be rigidity by the polyaniline material molecular chain that mixes made, do not have second-order transition temperature, material decomposes before fusion; Aniline and other monomer copolymerizations, prepared materials processing improves, but its specific conductivity obviously descends.The poor stability of the water base dispersoid of polyaniline in the aqueous solution, cohesion easily.
Summary of the invention
The object of the present invention is to provide a kind ofly have certain second-order transition temperature, good heat stability, solvability is good, specific conductivity is high, the preparation method of machinable polyaniline/P (MMA-BA-HEA) conducing composite material.
For achieving the above object, the technical solution used in the present invention is:
1) emulsion preparation: at first by mass fraction the Pentyl alcohol of 0.9～1.2 part fatty alcohol-polyoxyethylene ether, 0.9～1.2 part Sodium dodecylbenzene sulfonate and 0.05～0.1 part is joined keep constant temperature when under agitation being warmed up to 70～75 ℃ in 180～200 parts the deionized water and with two feed hoppers respectively to wherein dripping monomer mixture and initiator solution, the two all dripped off in 1.0～1.5 hours, drip off follow-up continuation of insurance temperature reaction 3 hours, cool to room temperature promptly gets the emulsion of P (MMA-BA-HEA) multipolymer then;
Said monomer mixture is that 45～50 parts butyl acrylate, 18～22 parts methyl methacrylate and 2～3 parts Hydroxyethyl acrylate mix by mass fraction;
Said initiator solution is the deionized water solution of azo di-isopropyl tetrahydroglyoxaline, and wherein the mass fraction of azo di-isopropyl tetrahydroglyoxaline is that 5～10 parts, the mass fraction of deionized water are 30 parts;
2) preparation of polyaniline composite material: the emulsion of getting P (MMA-BA-HEA) multipolymer of 25～30 parts aniline and 50～60 parts by mass fraction in reactor, mix and with the hydrochloric acid of 0.2mol/L regulate pH value be 1～1.5 mixed emulsion, get by mass fraction 10～15 parts ammonium persulphate mix with 25～30 parts deionized water ammonium persulfate aqueous solution, ammonium persulfate aqueous solution is added drop-wise in the mixed emulsion, the dropping time is 2～2.5 hours, control reaction temperature is 10～15 ℃, reaction times is 10～15 hours, with gained emulsion dehydrated alcohol breakdown of emulsion, sedimentation and filtration is also used absolute ethanol washing, up to filtrate pH value is 6, in 60 ℃ of vacuum-dryings, grind into powder is polyaniline/P (MMA-BA-HEA) matrix material.
The present invention is with aniline and compound processibility, the solvability of improving polyaniline of other plastic macromolecule materials, and the electric conductivity of this method p-poly-phenyl amine influence simultaneously is less.Gained polyaniline composite material of the present invention has favorable conductive and processing characteristics, and the matrix material specific conductivity is up to 1.472Scm
-1, matrix material PANI/P (MMA-BA-HEA) as having good solubility in pimelinketone, N-Methyl pyrrolidone, the dimethyl sulfoxide (DMSO), has solved the processing difficulties of layer/polyaniline conductive material and the problem of application facet in organic solvent.Therefore, the material of the present invention preparation and the comparison of existing polyaniline composite material have certain second-order transition temperature, good heat stability, solvability is good, specific conductivity is high, machinable polyaniline composite material, reaches domestic and international advanced level.
Embodiment
Embodiment 1:1) emulsion preparation: at first press mass fraction with 0.9 part fatty alcohol-polyoxyethylene ether (AEO
9), the Pentyl alcohol of 0.9 part Sodium dodecylbenzene sulfonate (SDBS) and 0.05 part join keep constant temperature when under agitation being warmed up to 70 ℃ in 180 parts the deionized water and with two feed hoppers respectively to wherein dripping monomer mixture and initiator solution, the two all dripped off in 1 hour, drip off follow-up continuation of insurance temperature reaction 3 hours, cool to room temperature promptly gets the emulsion of P (MMA-BA-HEA) multipolymer then;
Said monomer mixture is that 45 parts butyl acrylate (BA), 18 parts methyl methacrylate (MMA) and 2 parts Hydroxyethyl acrylate (HEA) mix by mass fraction;
Said initiator solution is the deionized water solution of azo di-isopropyl tetrahydroglyoxaline (AIP), and wherein the mass fraction of azo di-isopropyl tetrahydroglyoxaline is that 5 parts, the mass fraction of deionized water are 30 parts;
2) preparation of polyaniline composite material: the emulsion of getting P (MMA-BA-HEA) multipolymer of 25 parts aniline and 50 parts by mass fraction in reactor, mix and with the hydrochloric acid of 0.2mol/L regulate pH value be 1.5 mixed emulsion, get by mass fraction 10 parts ammonium persulphate mix with 25 parts deionized water ammonium persulfate aqueous solution, ammonium persulfate aqueous solution is added drop-wise in the mixed emulsion, the dropping time is 2 hours, control reaction temperature is 10 ℃, reaction times is 15 hours, with gained emulsion dehydrated alcohol breakdown of emulsion, sedimentation and filtration is also used absolute ethanol washing, up to filtrate pH value is 6, in 60 ℃ of vacuum-dryings, grind into powder is polyaniline/P (MMA-BA-HEA) matrix material.
Embodiment 2:1) emulsion preparation: at first press mass fraction with 1.1 parts fatty alcohol-polyoxyethylene ether (AEO
9), the Pentyl alcohol of 1.1 parts Sodium dodecylbenzene sulfonate (SDBS) and 0.08 part join keep constant temperature when under agitation being warmed up to 75 ℃ in 190 parts the deionized water and with two feed hoppers respectively to wherein dripping monomer mixture and initiator solution, the two all dripped off in 1.5 hours, drip off follow-up continuation of insurance temperature reaction 3 hours, cool to room temperature promptly gets the emulsion of P (MMA-BA-HEA) multipolymer then;
Said monomer mixture is that 48 parts butyl acrylate (BA), 20 parts methyl methacrylate (MMA) and 2.8 parts Hydroxyethyl acrylate (HEA) mix by mass fraction;
Said initiator solution is the deionized water solution of azo di-isopropyl tetrahydroglyoxaline (AIP), and wherein the mass fraction of azo di-isopropyl tetrahydroglyoxaline is that 8 parts, the mass fraction of deionized water are 30 parts;
2) preparation of polyaniline composite material: the emulsion of getting P (MMA-BA-HEA) multipolymer of 28 parts aniline and 58 parts by mass fraction in reactor, mix and with the hydrochloric acid of 0.2mol/L regulate pH value be 1.4 mixed emulsion, get by mass fraction 14 parts ammonium persulphate mix with 28 parts deionized water ammonium persulfate aqueous solution, ammonium persulfate aqueous solution is added drop-wise in the mixed emulsion, the dropping time is 2.5 hours, control reaction temperature is 15 ℃, reaction times is 10 hours, with gained emulsion dehydrated alcohol breakdown of emulsion, sedimentation and filtration is also used absolute ethanol washing, up to filtrate pH value is 6, in 60 ℃ of vacuum-dryings, grind into powder is polyaniline/P (MMA-BA-HEA) matrix material.
Embodiment 3:1) emulsion preparation: at first press mass fraction with 1.2 parts fatty alcohol-polyoxyethylene ether (AEO
9), the Pentyl alcohol of 1.2 parts Sodium dodecylbenzene sulfonate (SDBS) and 0.1 part join keep constant temperature when under agitation being warmed up to 73 ℃ in 200 parts the deionized water and with two feed hoppers respectively to wherein dripping monomer mixture and initiator solution, the two all dripped off in 1.2 hours, drip off follow-up continuation of insurance temperature reaction 3 hours, cool to room temperature promptly gets the emulsion of P (MMA-BA-HEA) multipolymer then;
Said monomer mixture is that 50 parts butyl acrylate (BA), 22 parts methyl methacrylate (MMA) and 3 parts Hydroxyethyl acrylate (HEA) mix by mass fraction;
Said initiator solution is the deionized water solution of azo di-isopropyl tetrahydroglyoxaline (AIP), and wherein the mass fraction of azo di-isopropyl tetrahydroglyoxaline is that 10 parts, the mass fraction of deionized water are 30 parts;
2) preparation of polyaniline composite material: the emulsion of getting P (MMA-BA-HEA) multipolymer of 30 parts aniline and 60 parts by mass fraction in reactor, mix and with the hydrochloric acid of 0.2mol/L regulate pH value be 1.2 mixed emulsion, get by mass fraction 15 parts ammonium persulphate mix with 30 parts deionized water ammonium persulfate aqueous solution, ammonium persulfate aqueous solution is added drop-wise in the mixed emulsion, the dropping time is 2.3 hours, control reaction temperature is 13 ℃, reaction times is 12 hours, with gained emulsion dehydrated alcohol breakdown of emulsion, sedimentation and filtration is also used absolute ethanol washing, up to filtrate pH value is 6, in 60 ℃ of vacuum-dryings, grind into powder is polyaniline/P (MMA-BA-HEA) matrix material.
Embodiment 4:1) emulsion preparation: at first press mass fraction with 1.0 parts fatty alcohol-polyoxyethylene ether (AEO
9), the Pentyl alcohol of 1.0 parts Sodium dodecylbenzene sulfonate (SDBS) and 0.06 part join keep constant temperature when under agitation being warmed up to 74 ℃ in 185 parts the deionized water and with two feed hoppers respectively to wherein dripping monomer mixture and initiator solution, the two all dripped off in 1.4 hours, drip off follow-up continuation of insurance temperature reaction 3 hours, cool to room temperature promptly gets the emulsion of P (MMA-BA-HEA) multipolymer then;
Said monomer mixture is that 46 parts butyl acrylate (BA), 19 parts methyl methacrylate (MMA) and 2.3 parts Hydroxyethyl acrylate (HEA) mix by mass fraction;
Said initiator solution is the deionized water solution of azo di-isopropyl tetrahydroglyoxaline (AIP), and wherein the mass fraction of azo di-isopropyl tetrahydroglyoxaline is that 7 parts, the mass fraction of deionized water are 30 parts;
2) preparation of polyaniline composite material: the emulsion of getting P (MMA-BA-HEA) multipolymer of 26 parts aniline and 53 parts by mass fraction in reactor, mix and with the hydrochloric acid of 0.2mol/L regulate pH value be 1.0 mixed emulsion, get by mass fraction 12 parts ammonium persulphate mix with 26 parts deionized water ammonium persulfate aqueous solution, ammonium persulfate aqueous solution is added drop-wise in the mixed emulsion, the dropping time is 2 hours, control reaction temperature is 11 ℃, reaction times is 14 hours, with gained emulsion dehydrated alcohol breakdown of emulsion, sedimentation and filtration is also used absolute ethanol washing, up to filtrate pH value is 6, in 60 ℃ of vacuum-dryings, grind into powder is polyaniline/P (MMA-BA-HEA) matrix material.
Claims (5)
1. the preparation method of a polyaniline/P (MMA-BA-HEA) conducing composite material is characterized in that:
1) emulsion preparation: at first by mass fraction the Pentyl alcohol of 0.9～1.2 part fatty alcohol-polyoxyethylene ether, 0.9～1.2 part Sodium dodecylbenzene sulfonate and 0.05～0.1 part is joined keep constant temperature when under agitation being warmed up to 70～75 ℃ in 180～200 parts the deionized water and with two feed hoppers respectively to wherein dripping monomer mixture and initiator solution, the two all dripped off in 1.0～1.5 hours, drip off follow-up continuation of insurance temperature reaction 3 hours, cool to room temperature promptly gets the emulsion of P (MMA-BA-HEA) multipolymer then;
Said monomer mixture is that 45～50 parts butyl acrylate, 18～22 parts methyl methacrylate and 2～3 parts Hydroxyethyl acrylate mix by mass fraction;
Said initiator solution is the deionized water solution of azo di-isopropyl tetrahydroglyoxaline, and wherein the mass fraction of azo di-isopropyl tetrahydroglyoxaline is that 5～10 parts, the mass fraction of deionized water are 30 parts;
2) preparation of polyaniline composite material: the emulsion of getting P (MMA-BA-HEA) multipolymer of 25～30 parts aniline and 50～60 parts by mass fraction in reactor, mix and with the salt acid for adjusting pH value of 0.2mol/L be 1～1.5 mixed emulsion, get by mass fraction 10～15 parts ammonium persulphate mix with 25～30 parts deionized water ammonium persulfate aqueous solution, ammonium persulfate aqueous solution is added drop-wise in the mixed emulsion, the dropping time is 2～2.5 hours, control reaction temperature is 10～15 ℃, reaction times is 10～15 hours, with gained emulsion dehydrated alcohol breakdown of emulsion, sedimentation and filtration is also used absolute ethanol washing, up to filtrate pH value is 6, in 60 ℃ of vacuum-dryings, grind into powder is polyaniline/P (MMA-BA-HEA) matrix material.
2. the preparation method of polyaniline/P according to claim 1 (MMA-BA-HEA) conducing composite material is characterized in that: 1) emulsion preparation: at first press mass fraction with 0.9 part fatty alcohol-polyoxyethylene ether AEO
9, 0.9 part Sodium dodecylbenzene sulfonate (SDBS) and 0.05 part Pentyl alcohol join keep constant temperature when under agitation being warmed up to 70 ℃ in 180 parts the deionized water and with two feed hoppers respectively to wherein dripping monomer mixture and initiator solution, the two all dripped off in 1 hour, drip off follow-up continuation of insurance temperature reaction 3 hours, cool to room temperature promptly gets the emulsion of P (MMA-BA-HEA) multipolymer then;
Said monomer mixture is that 45 parts butyl acrylate (BA), 18 parts methyl methacrylate (MMA) and 2 parts Hydroxyethyl acrylate (HEA) mix by mass fraction;
Said initiator solution is the deionized water solution of azo di-isopropyl tetrahydroglyoxaline (AIP), and wherein the mass fraction of azo di-isopropyl tetrahydroglyoxaline is that 5 parts, the mass fraction of deionized water are 30 parts;
2) preparation of polyaniline composite material: the emulsion of getting P (MMA-BA-HEA) multipolymer of 25 parts aniline and 50 parts by mass fraction in reactor, mix and with the salt acid for adjusting pH value of 0.2mol/L be 1.5 mixed emulsion, get by mass fraction 10 parts ammonium persulphate mix with 25 parts deionized water ammonium persulfate aqueous solution, ammonium persulfate aqueous solution is added drop-wise in the mixed emulsion, the dropping time is 2 hours, control reaction temperature is 10 ℃, reaction times is 15 hours, with gained emulsion dehydrated alcohol breakdown of emulsion, sedimentation and filtration is also used absolute ethanol washing, up to filtrate pH value is 6, in 60 ℃ of vacuum-dryings, grind into powder is polyaniline/P (MMA-BA-HEA) matrix material.
3. the preparation method of polyaniline/P according to claim 1 (MMA-BA-HEA) conducing composite material is characterized in that: 1) emulsion preparation: at first press mass fraction with 1.1 parts fatty alcohol-polyoxyethylene ether AEO
9, 1.1 parts Sodium dodecylbenzene sulfonate (SDBS) and 0.08 part Pentyl alcohol join keep constant temperature when under agitation being warmed up to 75 ℃ in 190 parts the deionized water and with two feed hoppers respectively to wherein dripping monomer mixture and initiator solution, the two all dripped off in 1.5 hours, drip off follow-up continuation of insurance temperature reaction 3 hours, cool to room temperature promptly gets the emulsion of P (MMA-BA-HEA) multipolymer then;
Said monomer mixture is that 48 parts butyl acrylate (BA), 20 parts methyl methacrylate (MMA) and 2.8 parts Hydroxyethyl acrylate (HEA) mix by mass fraction;
Said initiator solution is the deionized water solution of azo di-isopropyl tetrahydroglyoxaline (AIP), and wherein the mass fraction of azo di-isopropyl tetrahydroglyoxaline is that 8 parts, the mass fraction of deionized water are 30 parts;
2) preparation of polyaniline composite material: the emulsion of getting P (MMA-BA-HEA) multipolymer of 28 parts aniline and 58 parts by mass fraction in reactor, mix and with the salt acid for adjusting pH value of 0.2mol/L be 1.4 mixed emulsion, get by mass fraction 14 parts ammonium persulphate mix with 28 parts deionized water ammonium persulfate aqueous solution, ammonium persulfate aqueous solution is added drop-wise in the mixed emulsion, the dropping time is 2.5 hours, control reaction temperature is 15 ℃, reaction times is 10 hours, with gained emulsion dehydrated alcohol breakdown of emulsion, sedimentation and filtration is also used absolute ethanol washing, up to filtrate pH value is 6, in 60 ℃ of vacuum-dryings, grind into powder is polyaniline/P (MMA-BA-HEA) matrix material.
4. the preparation method of polyaniline/P according to claim 1 (MMA-BA-HEA) conducing composite material is characterized in that: 1) emulsion preparation: at first press mass fraction with 1.2 parts fatty alcohol-polyoxyethylene ether AEO
9, 1.2 parts Sodium dodecylbenzene sulfonate (SDBS) and 0.1 part Pentyl alcohol join keep constant temperature when under agitation being warmed up to 73 ℃ in 200 parts the deionized water and with two feed hoppers respectively to wherein dripping monomer mixture and initiator solution, the two all dripped off in 1.2 hours, drip off follow-up continuation of insurance temperature reaction 3 hours, cool to room temperature promptly gets the emulsion of P (MMA-BA-HEA) multipolymer then;
Said monomer mixture is that 50 parts butyl acrylate (BA), 22 parts methyl methacrylate (MMA) and 3 parts Hydroxyethyl acrylate (HEA) mix by mass fraction;
Said initiator solution is the deionized water solution of azo di-isopropyl tetrahydroglyoxaline (AIP), and wherein the mass fraction of azo di-isopropyl tetrahydroglyoxaline is that 10 parts, the mass fraction of deionized water are 30 parts;
2) preparation of polyaniline composite material: the emulsion of getting P (MMA-BA-HEA) multipolymer of 30 parts aniline and 60 parts by mass fraction in reactor, mix and with the salt acid for adjusting pH value of 0.2mol/L be 1.2 mixed emulsion, get by mass fraction 15 parts ammonium persulphate mix with 30 parts deionized water ammonium persulfate aqueous solution, ammonium persulfate aqueous solution is added drop-wise in the mixed emulsion, the dropping time is 2.3 hours, control reaction temperature is 13 ℃, reaction times is 12 hours, with gained emulsion dehydrated alcohol breakdown of emulsion, sedimentation and filtration is also used absolute ethanol washing, up to filtrate pH value is 6, in 60 ℃ of vacuum-dryings, grind into powder is polyaniline/P (MMA-BA-HEA) matrix material.
5. the preparation method of polyaniline/P according to claim 1 (MMA-BA-HEA) conducing composite material is characterized in that: 1) emulsion preparation: at first press mass fraction with 1.0 parts fatty alcohol-polyoxyethylene ether AEO
9, 1.0 parts Sodium dodecylbenzene sulfonate (SDBS) and 0.06 part Pentyl alcohol join keep constant temperature when under agitation being warmed up to 74 ℃ in 185 parts the deionized water and with two feed hoppers respectively to wherein dripping monomer mixture and initiator solution, the two all dripped off in 1.4 hours, drip off follow-up continuation of insurance temperature reaction 3 hours, cool to room temperature promptly gets the emulsion of P (MMA-BA-HEA) multipolymer then;
Said monomer mixture is that 46 parts butyl acrylate (BA), 19 parts methyl methacrylate (MMA) and 2.3 parts Hydroxyethyl acrylate (HEA) mix by mass fraction;
Said initiator solution is the deionized water solution of azo di-isopropyl tetrahydroglyoxaline (AIP), and wherein the mass fraction of azo di-isopropyl tetrahydroglyoxaline is that 7 parts, the mass fraction of deionized water are 30 parts;
2) preparation of polyaniline composite material: the emulsion of getting P (MMA-BA-HEA) multipolymer of 26 parts aniline and 53 parts by mass fraction in reactor, mix and with the salt acid for adjusting pH value of 0.2mol/L be 1.0 mixed emulsion, get by mass fraction 12 parts ammonium persulphate mix with 26 parts deionized water ammonium persulfate aqueous solution, ammonium persulfate aqueous solution is added drop-wise in the mixed emulsion, the dropping time is 2 hours, control reaction temperature is 11 ℃, reaction times is 14 hours, with gained emulsion dehydrated alcohol breakdown of emulsion, sedimentation and filtration is also used absolute ethanol washing, up to filtrate pH value is 6, in 60 ℃ of vacuum-dryings, grind into powder is polyaniline/P (MMA-BA-HEA) matrix material.
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| CN102040695B (en) * | 2010-11-26 | 2012-02-29 | 中国人民解放军国防科学技术大学 | Preparation method of water-soluble polyvinylpyrrolidone grafted polyaniline (PVP-g-PANI) copolymer |
| CN103265783B (en) * | 2013-06-06 | 2015-08-19 | 昆明理工恒达科技股份有限公司 | The preparation method of conductive polyaniline-organic matter composite anode material |
| CN105949397B (en) * | 2016-05-17 | 2019-05-28 | 常州大学 | The method for forming nanometer abnormal shape particle as matrix using polyaniline |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1286279A (en) * | 1999-08-27 | 2001-03-07 | 罗姆和哈斯公司 | Improved polymer composition |
| CN1302829A (en) * | 2000-12-22 | 2001-07-11 | 石油大学(北京) | Process for synthesizing cationic additive for electrode of polymer electrolyte and its application |
| CN1359973A (en) * | 2000-12-19 | 2002-07-24 | 中国石化集团齐鲁石油化工公司 | Organosilicon-modified acrylic emulsion composition and its preparing process |
| CN1361200A (en) * | 2000-12-29 | 2002-07-31 | 广东工业大学 | Prepn of polyacrylate flocculant |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1286279A (en) * | 1999-08-27 | 2001-03-07 | 罗姆和哈斯公司 | Improved polymer composition |
| CN1359973A (en) * | 2000-12-19 | 2002-07-24 | 中国石化集团齐鲁石油化工公司 | Organosilicon-modified acrylic emulsion composition and its preparing process |
| CN1302829A (en) * | 2000-12-22 | 2001-07-11 | 石油大学(北京) | Process for synthesizing cationic additive for electrode of polymer electrolyte and its application |
| CN1361200A (en) * | 2000-12-29 | 2002-07-31 | 广东工业大学 | Prepn of polyacrylate flocculant |
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