CN101302294B - Preparation of polyaniline nano-wire/nano-particle compound system - Google Patents
Preparation of polyaniline nano-wire/nano-particle compound system Download PDFInfo
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Abstract
The invention relates to a method for preparing a polyaniline nano wire/nano particle complex system. The method is characterized in that the method takes fat-soluble sucrose octaacetate containing eight branch chains as a template and a homogeneous system formed by water and water-soluble organic solvents as the reaction medium and prepares a polyaniline nano wire/nano particle complex system by utilizing a template polymerization method and taking hydrochloric acids as doping acids, which facilitates the utilization of branch chains of sucrose octaacetate molecules to initiate the stereotactic polymerization of aniline to prepare the polyaniline nano wire/nano particle complex system; moreover, the use of water and water-soluble organic solvents as a reaction system avoids the environmental pollution of fat phase organic solvents in interfacial polymerization and emulsion polymerization; moreover, the water-soluble organic solvents are also good solvents for a plurality of polymers, thereby providing a new research method for preparing polyaniline conductive composite materials and having better use value.
Description
Technical field
The present invention relates to the preparation method of a kind of polyaniline nano-line/nano particle compound system, with the fat-soluble Sucrose octaacetate that contains eight branched structures is that template, hydrochloric acid are that the homogeneous system that doping agent, water and water-miscible organic solvent are formed is a reaction medium, utilizes the template polymerization method to prepare by series of steps.
Background technology
Polyaniline nano structure such as nano wire, nanotube, nano particle etc. have and are different from the random particulate performance of common polyaniline, noticeable change will take place with respect to bulk material in its performance when the characteristic dimension of material reaches nano-scale, play the part of important role at aspects such as making the nano functional device.In recent years, the researchist is obtaining bigger progress aspect the preparation of nano polyaniline, but the preparation of the polyaniline nano-line that morphological parameters is adjustable, electromagnetic performance is good/nano particle compound system remains and realizes their key in application technically.
The method that is used to prepare polyaniline nano-line/nano particle compound system at present mainly is methods such as template, self-assembly method, interfacial polymerization, seeding polymerization method, the following problem of these method ubiquities: the template that (1) aniline polymerization finishes to be adopted the back is difficult for removing; (2) problem of environmental pollution of oil phase organic solvent in the reaction medium; (3) production cost height; Problem such as (4) polyaniline nano-line/pattern parameter of nano particle compound system, electromagnetic performance be restive.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes the preparation method of a kind of polyaniline nano-line/nano particle compound system, on the basis of preparation nano polyaniline, with the fat-soluble Sucrose octaacetate that contains eight branched structures is template, the homogeneous system that water and water-miscible organic solvent are formed is a reaction medium, has obtained good polyaniline nano-line/nano particle compound system of a kind of pattern controllable parameters, electromagnetic performance and preparation method thereof.Preparation method's environmentally safe, the technology that the present invention sets forth is simple, productive rate is high, is easy to suitability for industrialized production, and gained polyaniline nano fiber/nano particle compound system has good electromagnetic performance.Can be applicable to fields such as stealth material, electromagnetic shielding material, antistatic material with institute of the present invention synthetic polyaniline nano-line/nano particle compound system.
Technical scheme
The preparation method of a kind of polyaniline nano-line/nano particle compound system is characterized in that step is as follows:
Step 1,0.1～10 part of Sucrose octaacetate is dissolved in the homogeneous system that 30～200 parts of water and water-miscible organic solvent form;
Step 2, under agitation condition, hydrochloric acid is dissolved in the above-mentioned homogeneous system for 5～20 parts and forms hydrochloric acid soln;
Step 3, under agitation condition, add 2～10 parts of aniline and form component A;
Step 4, under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 1.0ml/min～5.0ml/min, after dropwising, continues reaction 3～12 hours, and temperature of reaction is controlled between 0 ℃～5 ℃; Described component B is: 4～50 parts of oxygenant ammonium persulphates are dissolved in the homogeneous system that 20～50 parts of water and water-miscible organic solvent form form component B;
Step 5, use methyl alcohol, acetone and deionized water wash colourless respectively after will reaction product filtering to filtrate;
Step 6, carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5M～4.0M, and the adulterated time is 3～12 hours;
Step 7, washing final vacuum are drying to obtain polyaniline nano-line/nano particle compound system, and the vacuum tightness during vacuum-drying is 0.6MPa～0.9MPa, and the exsiccant temperature is 60 ℃～100 ℃;
Each component unit is a mass parts in the above-mentioned steps.
Described Sucrose octaacetate is a kind of fat-soluble organic micromolecule compound that contains eight branched structures.
Described water-miscible organic solvent is the organic solvent that alcohols or ketone can form homogeneous system with water, and wherein the volume content of water-miscible organic solvent is 0～100%.
Beneficial effect
The preparation method of the polyaniline nano-line that the present invention relates to/nano particle compound system, its characteristics are: it is template that (1) the present invention adopts the fat-soluble Sucrose octaacetate that contains eight branched structures, to make aniline be template with the Sucrose octaacetate molecule in polymerization process by dropwise dripping ammonium persulfate solution, assembles and exist in the nano wire/mode of nano particle compound system.With the Sucrose octaacetate is that template helps synthetic polyaniline nano-line/nano particle compound system that the microscopic appearance parameter is adjustable, electromagnetic performance is good; (2) homogeneous system that forms with water and water-miscible organic solvent is reaction medium, has avoided the problem of environmental pollution of oil phase organic solvent in interfacial polymerization and the letex polymerization; (3) water-miscible organic solvent also is the good solvent of many polymkeric substance, and this just provides new research thinking for the preparation polyaniline nanometer conductive composite material, has bigger practical value.The homogeneous system that is template with the Sucrose octaacetate, forms with water and water-miscible organic solvent be the stereoscan photograph (SEM) of polyaniline nano-line/nano particle compound system of reaction medium preparation and x-ray diffraction pattern (XRD) as shown in Figure 1 and Figure 2; The homogeneous system that is template with the Sucrose octaacetate, forms with water and water-miscible organic solvent be the polyaniline nano-line/nano particle compound system of reaction medium preparation in 8.2GHz～12.4GHz scope the electrical loss performance and the magnetic loss performance as shown in Figure 3, Figure 4.
Description of drawings
Fig. 1: scanning electron microscope (SEM) photo that with the Sucrose octaacetate is the polyaniline nano-line/nano particle compound system of the homogeneous system preparation that forms of template, water and water-miscible organic solvent: (a) in the water, in the homogeneous system of (b) water and water-miscible organic solvent formation, in (c) water-miscible organic solvent.
Fig. 2: X-ray diffraction (XRD) figure that with the Sucrose octaacetate is the polyaniline nano-line/nano particle compound system of the homogeneous system preparation that forms of template, water and water-miscible organic solvent: (a) in the water, in the homogeneous system of (b) water and water-miscible organic solvent formation, in (c) water-miscible organic solvent.
Fig. 3: be the dielectric properties figure of the polyaniline nano-line/nano particle compound system of the homogeneous system preparation that forms of template, water and water-miscible organic solvent, wherein (a) real part of permittivity with the Sucrose octaacetate; (b) specific inductivity imaginary part; (c) dielectric loss.
Fig. 4: be the magnetic property figure of the polyaniline nano-line/nano particle compound system of the homogeneous system preparation that forms of template, water and water-miscible organic solvent, wherein (a) magnetic permeability real part with the Sucrose octaacetate; (b) magnetic permeability imaginary part; (c) magnetic loss.
Embodiment
Now in conjunction with the embodiments, accompanying drawing is further described the present invention:
Embodiment 1:
(1) 0.1 part of Sucrose octaacetate dissolving is dispersed in 30 parts of water reaction mediums;
(2) under agitation condition with 5 parts of dissolving with hydrochloric acid in above-mentioned solution;
(3) under agitation condition, add 2 parts of aniline and form component A;
(4) 5 parts of ammonium persulphates are dissolved in formation component B in 20 parts of water;
(5) under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 1.0ml/min～5.0ml/min, after dropwising, continues reaction 3～12 hours, and temperature of reaction is controlled between 0 ℃～5 ℃;
(6) will use methyl alcohol, acetone and deionized water wash colourless respectively after the reaction product filtration to filtrate;
(7) carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5M～4.0M, and the adulterated time is 3～12 hours;
(8) the washing final vacuum is drying to obtain polyaniline nano-line/nano particle compound system, and the vacuum tightness during vacuum-drying is 0.6MPa～0.9MPa, and the exsiccant temperature is 60 ℃～100 ℃.
Embodiment 2:
(1) water and 1: 1 by volume mixed of water-miscible organic solvent are formed 70 parts homogeneous system;
(2) 2 parts of Sucrose octaacetates are dissolved in the above-mentioned system;
(3) under stirring condition with 5 parts of dissolving with hydrochloric acid in above-mentioned solution;
(4) under agitation condition, add 4 parts of aniline and form component A;
(5) 10 parts of ammonium persulphates are dissolved in 20 parts of homogeneous systems that water and 1: 1 by volume mixed of water-miscible organic solvent generate and form component B;
(6) under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 1.0ml/min～5.0ml/min; Dropwise the back and continue reaction 3～12 hours, temperature of reaction is controlled between 0 ℃～5 ℃;
(7) will use methyl alcohol, acetone and deionized water wash colourless respectively after the reaction product filtration to filtrate;
(8) carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5M～4.0M, and the adulterated time is 3～12 hours;
(9) the washing final vacuum is drying to obtain polyaniline nano fiber/nano particle compound system, and the vacuum tightness during vacuum-drying is 0.6MPa～0.9MPa, and the exsiccant temperature is 60 ℃～100 ℃.
Embodiment 3:
(1) 3 parts of Sucrose octaacetate dissolvings is dispersed in 100 parts of water reaction mediums;
(2) under agitation condition with 5 parts of dissolving with hydrochloric acid in above-mentioned solution;
(3) under agitation condition, add 2 parts of aniline and form component A;
(4) 5 parts of ammonium persulphates are dissolved in formation component B in 20 parts of water;
(5) under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 1.0ml/min～5.0ml/min, after dropwising, continues reaction 3～12 hours, and temperature of reaction is controlled between 0 ℃～5 ℃;
(6) will use methyl alcohol, acetone and deionized water wash colourless respectively after the reaction product filtration to filtrate;
(7) carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5M～4.0M, and the adulterated time is 3～12 hours;
(8) the washing final vacuum is drying to obtain polyaniline nano-line/nano particle compound system, and the vacuum tightness during vacuum-drying is 0.6MPa～0.9MPa, and the exsiccant temperature is 60 ℃～100 ℃.
Embodiment 4:
(1) water and 3: 2 by volume mixed of water-miscible organic solvent are formed 150 parts homogeneous system;
(2) 5 parts of Sucrose octaacetates are dissolved in the above-mentioned system;
(3) under stirring condition with 10 parts of dissolving with hydrochloric acid in above-mentioned solution;
(4) under agitation condition, add 10 parts of aniline and form component A;
(5) 50 parts of ammonium persulphates are dissolved in 50 parts of homogeneous systems that water and 3: 2 by volume mixed of water-miscible organic solvent generate and form component B;
(6) under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 1.0ml/min～5.0ml/min; Dropwise the back and continue reaction 3～12 hours, temperature of reaction is controlled between 0 ℃～5 ℃;
(7) will use methyl alcohol, acetone and deionized water wash colourless respectively after the reaction product filtration to filtrate;
(8) carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5M～4.0M, and the adulterated time is 3～12 hours;
(9) the washing final vacuum is drying to obtain polyaniline nano fiber/nano particle compound system, and the vacuum tightness during vacuum-drying is 0.6MPa～0.9MPa, and the exsiccant temperature is 60 ℃～100 ℃.
Embodiment 5:
(1) 10 parts of Sucrose octaacetates is dissolved in 200 parts of water-miscible organic solvent media;
(2) under stirring condition with 20 parts of dissolving with hydrochloric acid in above-mentioned solution;
(3) under agitation condition, add 10 parts of aniline and form component A;
(4) 50. parts of ammonium persulphates are dissolved in 50 parts of water-miscible organic solvents and form component B;
(5) under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 1.0ml/min～5.0ml/min; Dropwise the back and continue reaction 3～12 hours, temperature of reaction is controlled between 0 ℃～5 ℃;
(6) will use methyl alcohol, acetone and deionized water wash colourless respectively after the reaction product filtration to filtrate;
(7) carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5M～4.0M, and the adulterated time is 3～12 hours;
(8) the washing final vacuum is drying to obtain polyaniline nano fiber/nano particle compound system, and the vacuum tightness during vacuum-drying is 0.6MPa～0.9MPa, and the exsiccant temperature is 60 ℃～100 ℃.
The present invention is a template with the fat-soluble Sucrose octaacetate that contains eight side chains, the homogeneous system that water and water-miscible organic solvent are formed is a reaction medium, by the template polymerization method is that dopant acid prepares polyaniline nano-line/nano particle compound system with hydrochloric acid, help utilizing the tactic polymerization of the chain initiation aniline in the Sucrose octaacetate molecule to prepare polyaniline nano-line/nano particle compound system, and to adopt water and water-miscible organic solvent be reaction system, avoided the problem of environmental pollution of oil phase organic solvent in interfacial polymerization and the letex polymerization, water-miscible organic solvent also is the good solvent of many polymkeric substance in addition, this just provides new research thinking for the preparation polyaniline composite material, has bigger practical value.By provided by the invention with fat-soluble Sucrose octaacetate be template, the homogeneous system that forms with water and water-miscible organic solvent is reaction medium synthetic polyaniline nano-line/nano particle compound system, its pattern parameter can be controlled by the consumption that changes Sucrose octaacetate, the volume content of water-miscible organic solvent, the reaction parameters such as concentration, reaction times and temperature of reaction of dopant acid.
Claims (2)
1. the preparation method of polyaniline nano-line/nano particle compound system is characterized in that step is as follows:
Step 1,0.1～10 part of Sucrose octaacetate is dissolved in the homogeneous system that 30～200 parts of water and water-miscible organic solvent form;
Step 2, under agitation condition, hydrochloric acid is dissolved in the above-mentioned homogeneous system for 5～20 parts and forms hydrochloric acid soln;
Step 3, under agitation condition, add 2～10 parts of aniline and form component A;
Step 4, under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 1.0ml/min～5.0ml/min, after dropwising, continues reaction 3～12 hours, and temperature of reaction is controlled between 0 ℃～5 ℃; Described component B is: 4～50 parts of oxygenant ammonium persulphates are dissolved in the homogeneous system that 20～50 parts of water and water-miscible organic solvent form form component B;
Step 5, use methyl alcohol, acetone and deionized water wash colourless respectively after will reaction product filtering to filtrate;
Step 6, carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5M～4.0M, and the adulterated time is 3～12 hours;
Step 7, washing final vacuum are drying to obtain polyaniline nano-line/nano particle compound system, and the vacuum tightness during vacuum-drying is 0.6MPa～0.9MPa, and the exsiccant temperature is 60 ℃～100 ℃;
Each component unit is a mass parts in the above-mentioned steps.
2. the preparation method of polyaniline nano-line according to claim 1/nano particle compound system is characterized in that: described Sucrose octaacetate is a kind of fat-soluble organic micromolecule compound that contains eight branched structures.
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| CN103613758B (en) * | 2013-12-03 | 2016-05-11 | 江南大学 | Self-assembly method is prepared molecular engram polyaniline nano compound |
| CN105131282A (en) * | 2015-10-09 | 2015-12-09 | 桂林理工大学 | Method for preparing conductive polyaniline nanotube by taking sucrose as template |
| CN110452379B (en) * | 2019-09-03 | 2021-09-24 | 南昌航空大学 | Ferroferric oxide/polyaniline composite material and preparation method thereof |
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| CN1621432A (en) * | 2004-10-26 | 2005-06-01 | 中国科学院长春应用化学研究所 | Process for preparing poly-o-phenylamine nano-belt |
| WO2005068551A1 (en) * | 2004-01-13 | 2005-07-28 | Seoul National University Industry Foundation | A exfoliated nano-composite from polyaniline graft copolymer/clay |
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| WO2005068551A1 (en) * | 2004-01-13 | 2005-07-28 | Seoul National University Industry Foundation | A exfoliated nano-composite from polyaniline graft copolymer/clay |
| CN1621432A (en) * | 2004-10-26 | 2005-06-01 | 中国科学院长春应用化学研究所 | Process for preparing poly-o-phenylamine nano-belt |
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