CN105885043B - The preparation method of polyaniline nano microballoon with nucleocapsid - Google Patents
The preparation method of polyaniline nano microballoon with nucleocapsid Download PDFInfo
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- CN105885043B CN105885043B CN201610288808.3A CN201610288808A CN105885043B CN 105885043 B CN105885043 B CN 105885043B CN 201610288808 A CN201610288808 A CN 201610288808A CN 105885043 B CN105885043 B CN 105885043B
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Abstract
The invention discloses a kind of preparation method of the polyaniline nano microballoon with nucleocapsid, step includes:Prepare the polystyrene microsphere of monodispersity;Polystyrene microsphere is nitrified to obtain nitrification polystyrene microsphere;Amination polystyrene microsphere will be obtained after nitrification polystyrene microsphere reduction;Aniline is dissolved in after obtaining aniline solution in non-polar organic solvent, then the acidic aqueous solution of amination polystyrene microsphere and initiator is added drop-wise in above-mentioned aniline solution, the polyaniline nano microballoon with nucleocapsid is obtained by the reaction.Not only pattern is good for the core-shell structure polyaniline nanoparticle that preparation method of the present invention obtains, size uniformity, and has good monodispersity, and good dispersion, is not easy to reunite in water.Preparation method of the present invention is simple, mild condition, and non-metallic ion interference, favorable reproducibility has very strong practicability.
Description
Technical field
The present invention relates to polymeric material field, more particularly to the system of a kind of polyaniline nano microballoon with nucleocapsid
Preparation Method.
Background technology
Polyaniline (Polyaniline, abbreviation PANI) is a kind of important conducting polymer in high molecular material, is being conjugated
Occupy in conducting polymer composite and its consequence.PANI molecules are a kind of linear conjugate macromolecules being end-to-end,
Structure is made of reduction unit (y units) and oxidation unit (1-y units), and the y values in formula are used to characterize the redox of PANI
Degree, comprising there are one quinoid structure in oxidation unit, different y values correspond to different structures, component, color and conduction
Rate.By structural formula it is found that by introducing substituent group on PANI strands or introducing different ions by protonic acid doping,
The transformation from insulator to conductor may be implemented;In addition, PANI is easy to get with monomer raw material, synthesis technology is simple while also having
There are excellent physical property, good environmental stability, to the hot spot as the research of current conducting polymer composite.
Mono- important application field of PANI is electrode material, this is that its unique conjugated system is passed with preferable electronics
Ability is led, and the energy gaps and ionization potential of strand can be changed by chemical modification, to be applied to electric chemical super
Capacitor area.But the polymer prepared using conventional method has that easily reunite, effective ratio area is small, stability is poor etc. no
Foot place, to influence the chemical property of PANI.To overcome these disadvantages, by control pattern and the structure of PANI materials come
It is a most direct approach to increase its effective ratio area and stability.In recent years, the research of Polyaniline is mainly collected
In nanosphere (RSC Adv.2015,5,12034-12042), nano wire (J.Mater.Chem.A, 2015,3,23307-
23315), nanofiber (J.Power Sources 2015,294,16-21), nanometer rods (J.Mater.Chem.2012,22,
2774-2780) and nanotube (J.Mater.Chem.A, 2013,1,3315-3324) etc..Although the polyaniline of these patterns has
There is preferable chemical property, but there is also some problems, if preparation process is more complicated, process route is not easy to control;Institute
The PANI materials of preparation with other materials is compound can just preferable chemical property etc.;And the problems such as poorly water-soluble.
In order to solve the above-mentioned technical problem, the synthesis of polyaniline microsphere is also as this year come the hot spot studied, such as application number
Chinese patent polystyrene (Polystyrene, the abbreviation PS) microballoon for being 200710304102.2 is used as synthesis template, uses nitre
Sour iron (Fe (NO3)3), iron chloride (FeCl3) etc. be used as oxidant, the polystyrene/polyaniline for having invented nucleocapsid is conductive high
Molecule complex microsphere, although this technology can obtain the polyaniline microsphere of preferable pattern, the introducing of metallic element can influence
The chemical property of material.Application No. is 201110403637.1 Chinese patents to be prepared for one using water and alcohol mixed solution
Kind polyaniline nano microballoon, diameter is in 50-200nm, although preferable pattern can be obtained, Size Distribution is inhomogenous,
And it is water-soluble poor.Huang Bin etc. (functional material, 2011,42 (1), 144-147) is with PS colloidal particles with template
PANI hollow microspheres are prepared in microballoon core, and are applied to ESC electrode materials, study its electricity in energy storage field
Chemical property, although there is this tiny balloon preferable chemical property still to be deposited from the point of view of the picture of scanning electron microscope
The problems such as size is inhomogenous.Application No. is 201510852325.7 Chinese patents to have synthesized with sulfonated polystyrene (referred to as
SPS it is) kernel, polyaniline is the complex microsphere of sulfonated polystyrene/polyaniline of shell, water-soluble is asked although solving its
Topic, but electric conductivity is bad.
Invention content
The purpose of the present invention is to solve problem of the prior art, provide a kind of polyaniline nano with nucleocapsid
The preparation method of microballoon, with the polyaniline nano microballoon for the nucleocapsid that this method is prepared, not only size uniformity, Er Qieshui
Good dispersion, stable structure, good conductivity.The technical solution is as follows:
A kind of preparation method of the polyaniline nano microballoon with nucleocapsid, step include:
(1) polystyrene microsphere of monodispersity is prepared;
(2) will in the polystyrene microsphere ultrasonic disperse to nitrating agent in step (1), at 40~50 DEG C react 1~
2h is washed, is dried to obtain nitrification polystyrene microsphere;
(3) amination polystyrene microsphere will be obtained after the nitrification polystyrene microsphere reduction in step (2);
(4) aniline is dissolved in after obtaining aniline solution in non-polar organic solvent, then ammonia described in step (3) will be contained
The acidic aqueous solution of base polystyrene microsphere and initiator is added drop-wise in above-mentioned aniline solution, after stable system, -5~5
Reaction 10 at DEG C~purify afterwards for 24 hours, it is dry after obtain the polyaniline nano microballoon with nucleocapsid.
The non-polar organic solvent is preferably chloroform.
Preferably, the polystyrene microsphere in the step (1) is prepared by the method for emulsifier-free emulsion polymerization.Tool
Preparation can be adjusted according to the prior art, such as application No. is 201510852325.7 China in background technology
Described in patent.
Preferably, the nitrating agent in the step (2) is the concentrated sulfuric acid and concentrated nitric acid volume ratio is 3:2 mixed acid.
Preferably, the reduction in the step (3) is to pass through Na2S2O4Or sodium borohydride reductase 12~5h at 70~80 DEG C
It obtains.
Preferably, the initiator is ammonium persulfate.
Preferably, the acidic aqueous solution in the step (4) is the sulfuric acid or aqueous hydrochloric acid solution that concentration is 0.5mol/L.
Preferably, the purifying in the step (4) is filtered after acetone is added, and is obtained after then being washed with ethyl alcohol.
Preferably, the mass ratio of amination polystyrene microsphere and aniline is 1 in the step (4):(1~4).
Preferably, the molar ratio of aniline and initiator is 1 in the step (4):(0.5~5), more preferably 1:1.
Preferably, the dodecyl sodium sulfonate in the acidic aqueous solution of the step (4) also containing Solute mass 10~20%
Sodium.
Present invention utilizes the methods of interfacial polymerization, and in the polymerization of step (4), upper layer is aqueous phase solution, and lower layer is to have
Machine phase solution, polymerisation occur in interface, since the polyaniline nano microballoon of synthesis has hydrophily, to water phase after generation
Diffusion causes the reduction of interface concentration, reaction to be continued for carrying out.It therefore can be by simply adjusting aniline monomer and initiation
The dosage of agent effectively controls the shape characteristic of polyaniline microsphere, obtains the more uniform microspheres product of size.Meanwhile it adding
Dodecyl sodium sulfate, may stretch to water phase due to hydrophilic chain part, and hydrophobic chain puts in the micella that organic phase forms bending, makes to gather
Aniline nano microballoon is not easy to reunite due to Van der Waals force, to play the role of stable reaction system.
The advantageous effect that technical solution provided in an embodiment of the present invention is brought is:
The core-shell structure polyaniline nanoparticle that preparation method of the present invention obtains is using amination polystyrene as kernel, polyphenyl
Amine is shell, and not only pattern is good, size uniformity, and has good monodispersity, and good dispersion, is not easy to reunite in water.
Meanwhile containing several amination polyphenyl second in the microballoon of each polyaniline package of the polyaniline nano microballoon that is prepared of the present invention
Alkene increases its surface area.And the discovery of applicant's creativeness can be increased hydrophilic with the polystyrene after amination modified
Property and conductive effect, amino can also carry out other surface modifications, so that the polyaniline nano microballoon that is prepared of the present invention is existed
Electric chemical super capacitor field has more good application prospect.Preparation method of the present invention is simple, mild condition, no metal
Ion interference, favorable reproducibility have very strong practicability.
Description of the drawings
Fig. 1 is the field emission scanning electron microscope micrograph of the monodisperse polystyrene microsphere of the present invention;
Fig. 2 is the field emission scanning electron microscope micrograph of the amination polystyrene microsphere of the present invention;
Fig. 3 is the field emission scanning electron microscope micrograph of the polyaniline nano microballoon 1 of embodiment 1;
Fig. 4 is the field emission scanning electron microscope micrograph of the polyaniline nano microballoon 2 of embodiment 2;
Fig. 5 is the field emission scanning electron microscope micrograph of the polyaniline nano microballoon 3 of embodiment 3;
Fig. 6 is the field emission scanning electron microscope micrograph of the polyaniline nano microballoon 4 of embodiment 4;
Fig. 7 is the field emission scanning electron microscope micrograph of the polyaniline nano microballoon 5 of embodiment 5;
Fig. 8 is the field emission scanning electron microscope micrograph of the polyaniline nano microballoon 6 of embodiment 6.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment to the present invention
Embodiment is described in further detail.
Embodiment 1
(1) by 95mL ethyl alcohol, 5mL deionized waters, 1.818g polyvinylpyrrolidones are added in four-neck flask, in nitrogen
Under protection, at 70 DEG C after magnetic agitation 20min, 20g styrene, the azodiisobutyronitrile of 0.182g, magnetic agitation reaction is added
Natural cooling after 12h, obtains white emulsion, with absolute ethyl alcohol washed product, centrifuges and is dried in vacuo 10h under room temperature, obtain
Polystyrene microsphere powder.
(2) it is 3 above-mentioned polystyrene microsphere powder ultrasonic to be distributed to the concentrated sulfuric acid and concentrated nitric acid volume ratio:2 mixed acid
In, 2h is reacted at 40 DEG C, washs, be dried to obtain nitrification polystyrene microsphere;
(3) by above-mentioned nitrification polystyrene microsphere Na2S2O4It is micro- to obtain amination polystyrene by reduction 5h at 70 DEG C
Ball;
(4) 0.2g aniline is dissolved in after obtaining aniline solution in chloroform, then the above-mentioned amination polystyrene of 0.2g is micro-
The acidic aqueous solution of ball, 0.14g dodecyl sodium sulfates and 0.49g initiator ammonium persulfates is added drop-wise in above-mentioned aniline solution,
The molar ratio of aniline and ammonium persulfate is 1:1, acidic aqueous solution is the aqueous hydrochloric acid solution that concentration is 0.5mol/L.Wait for stable system
Afterwards, it reacts at -5 DEG C and is filtered after acetone is added afterwards for 24 hours, it is dry after then being washed with ethyl alcohol, it obtains described with nucleocapsid
Polyaniline nano microballoon 1.
Embodiment 2
(1) by 95mL ethyl alcohol, 5mL deionized waters, 1.818g polyvinylpyrrolidones are added in four-neck flask, in nitrogen
Under protection, at 70 DEG C after magnetic agitation 20min, 20g styrene, the azodiisobutyronitrile of 0.182g, magnetic agitation reaction is added
Natural cooling after 12h, obtains white emulsion, with absolute ethyl alcohol washed product, centrifuges and is dried in vacuo 10h under room temperature, obtain
Polystyrene microsphere powder.
(2) it is 3 above-mentioned polystyrene microsphere powder ultrasonic to be distributed to the concentrated sulfuric acid and concentrated nitric acid volume ratio:2 mixed acid
In, 1h is reacted at 50 DEG C, washs, be dried to obtain nitrification polystyrene microsphere;
(3) by above-mentioned nitrification polystyrene microsphere, with sodium borohydride, to obtain amination polystyrene micro- by the reductase 12 h at 80 DEG C
Ball;
(4) 0.4g aniline is dissolved in after obtaining aniline solution in chloroform, then the above-mentioned amination polystyrene of 0.2g is micro-
The acidic aqueous solution of ball, 0.118g dodecyl sodium sulfates and 0.98g initiator ammonium persulfates is added drop-wise in above-mentioned aniline solution,
The molar ratio of aniline and ammonium persulfate is 1:1, acidic aqueous solution is the aqueous sulfuric acid that concentration is 0.5mol/L.Wait for stable system
Afterwards, it reacts and is filtered after acetone is added after 10h at 5 DEG C, it is dry after then being washed with ethyl alcohol, it obtains described with nucleocapsid
Polyaniline nano microballoon 2.
Embodiment 3
(1) by 95mL ethyl alcohol, 5mL deionized waters, 1.818g polyvinylpyrrolidones are added in four-neck flask, in nitrogen
Under protection, at 70 DEG C after magnetic agitation 20min, 20g styrene, the azodiisobutyronitrile of 0.182g, magnetic agitation reaction is added
Natural cooling after 12h, obtains white emulsion, with absolute ethyl alcohol washed product, centrifuges and is dried in vacuo 10h under room temperature, obtain
Polystyrene microsphere powder.
(2) it is 3 above-mentioned polystyrene microsphere powder ultrasonic to be distributed to the concentrated sulfuric acid and concentrated nitric acid volume ratio:2 mixed acid
In, 1.5h is reacted at 45 DEG C, washs, be dried to obtain nitrification polystyrene microsphere;
(3) above-mentioned nitrification polystyrene microsphere is restored with sodium borohydride at 75 DEG C to 3h, and to obtain amination polystyrene micro-
Ball;
(4) 0.8g aniline is dissolved in after obtaining aniline solution in chloroform, then the above-mentioned amination polystyrene of 0.2g is micro-
The acidic aqueous solution of ball, 0.25g dodecyl sodium sulfates and 1.96g initiator ammonium persulfates is added drop-wise in above-mentioned aniline solution,
The molar ratio of aniline and ammonium persulfate is 1:1, acidic aqueous solution is the aqueous hydrochloric acid solution that concentration is 0.5mol/L.Wait for stable system
Afterwards, it reacts at 0 DEG C and is filtered after acetone is added after 20h, it is dry after then being washed with ethyl alcohol, it obtains described with nucleocapsid
Polyaniline nano microballoon 3.
Embodiment 4
(1) by 95mL ethyl alcohol, 5mL deionized waters, 1.818g polyvinylpyrrolidones are added in four-neck flask, in nitrogen
Under protection, at 70 DEG C after magnetic agitation 20min, 20g styrene, the azodiisobutyronitrile of 0.182g, magnetic agitation reaction is added
Natural cooling after 12h, obtains white emulsion, with absolute ethyl alcohol washed product, centrifuges and is dried in vacuo 10h under room temperature, obtain
Polystyrene microsphere powder.
(2) it is 3 above-mentioned polystyrene microsphere powder ultrasonic to be distributed to the concentrated sulfuric acid and concentrated nitric acid volume ratio:2 mixed acid
In, 1h is reacted at 50 DEG C, washs, be dried to obtain nitrification polystyrene microsphere;
(3) by above-mentioned nitrification polystyrene microsphere, with sodium borohydride, to obtain amination polystyrene micro- by the reductase 12 h at 80 DEG C
Ball;
(4) 0.4g aniline is dissolved in after obtaining aniline solution in chloroform, then the above-mentioned amination polystyrene of 0.2g is micro-
The acidic aqueous solution of ball and 0.98g initiator ammonium persulfates is added drop-wise in above-mentioned aniline solution, mole of aniline and ammonium persulfate
Than being 1:1, acidic aqueous solution is the aqueous sulfuric acid that concentration is 0.5mol/L.After stable system, after reacting 10h at 5 DEG C
It is filtered after acetone is added, it is dry after then being washed with ethyl alcohol, obtain the polyaniline nano microballoon 4 with nucleocapsid.
Embodiment 5
(1) by 95mL ethyl alcohol, 5mL deionized waters, 1.818g polyvinylpyrrolidones are added in four-neck flask, in nitrogen
Under protection, at 70 DEG C after magnetic agitation 20min, 20g styrene, the azodiisobutyronitrile of 0.182g, magnetic agitation reaction is added
Natural cooling after 12h, obtains white emulsion, with absolute ethyl alcohol washed product, centrifuges and is dried in vacuo 10h under room temperature, obtain
Polystyrene microsphere powder.
(2) it is 3 above-mentioned polystyrene microsphere powder ultrasonic to be distributed to the concentrated sulfuric acid and concentrated nitric acid volume ratio:2 mixed acid
In, 1h is reacted at 50 DEG C, washs, be dried to obtain nitrification polystyrene microsphere;
(3) by above-mentioned nitrification polystyrene microsphere, with sodium borohydride, to obtain amination polystyrene micro- by the reductase 12 h at 80 DEG C
Ball;
(4) 0.2g aniline is dissolved in after obtaining aniline solution in chloroform, then the above-mentioned amination polystyrene of 0.2g is micro-
The acidic aqueous solution of ball, 0.08g dodecyl sodium sulfates and 0.245g initiator ammonium persulfates is added drop-wise in above-mentioned aniline solution,
The molar ratio of aniline and ammonium persulfate is 1:0.5, acidic aqueous solution is the aqueous sulfuric acid that concentration is 0.5mol/L.Wait for that system is steady
After determining, filtered after acetone is added after reaction 10h at 5 DEG C, it is dry after then being washed with ethyl alcohol, it obtains described with nucleocapsid
Polyaniline nano microballoon 5.
Embodiment 6
(1) by 95mL ethyl alcohol, 5mL deionized waters, 1.818g polyvinylpyrrolidones are added in four-neck flask, in nitrogen
Under protection, at 70 DEG C after magnetic agitation 20min, 20g styrene, the azodiisobutyronitrile of 0.182g, magnetic agitation reaction is added
Natural cooling after 12h, obtains white emulsion, with absolute ethyl alcohol washed product, centrifuges and is dried in vacuo 10h under room temperature, obtain
Polystyrene microsphere powder.
(2) it is 3 above-mentioned polystyrene microsphere powder ultrasonic to be distributed to the concentrated sulfuric acid and concentrated nitric acid volume ratio:2 mixed acid
In, 1h is reacted at 50 DEG C, washs, be dried to obtain nitrification polystyrene microsphere;
(3) by above-mentioned nitrification polystyrene microsphere, with sodium borohydride, to obtain amination polystyrene micro- by the reductase 12 h at 80 DEG C
Ball;
(4) 0.2g aniline is dissolved in after obtaining aniline solution in chloroform, then the above-mentioned amination polystyrene of 0.2g is micro-
The acidic aqueous solution of ball, 0.2g dodecyl sodium sulfates and 1.225g initiator ammonium persulfates is added drop-wise in above-mentioned aniline solution,
The molar ratio of aniline and ammonium persulfate is 1:5, acidic aqueous solution is the aqueous hydrochloric acid solution that concentration is 0.5mol/L.Wait for stable system
Afterwards, it reacts and is filtered after acetone is added after 10h at 5 DEG C, it is dry after then being washed with ethyl alcohol, it obtains described with nucleocapsid
Polyaniline nano microballoon 6.
The amination polystyrene that polystyrene microsphere that the above various embodiments step (1) obtains, step (3) are obtained is micro-
The polyaniline nano microballoon 1-6 of ball and nucleocapsid carries out electron microscope scanning, and it is micro- to have obtained field emission scanning electron microscope
Figure, as shown in attached drawing 1-8.It can be seen in the drawings that the obtained core-shell structure polyaniline nanoparticle of the present invention not only pattern
It is good, size uniformity, and there is good monodispersity, it is not easy to reunite.Meanwhile the polyaniline nano that the present invention is prepared is micro-
Contain several amination polystyrene in the microballoon of each polyaniline package of ball, increases its surface area.
After above-mentioned polyaniline nano microballoon 1-6 is carried out hydrochloric acid secondary doping, conductivity and cyclic voltammetry detection are carried out,
As a result show that its conductivity is good, and energy storage is good.
Above-mentioned polyaniline nano microballoon 1-6 is added to the water, its good dispersion is shown, is not easy to reunite.
It should be noted that:Above-described embodiment only enumerates a small number of structures, and other structures those of ordinary skill in the art can be with
Corresponding construction can be obtained using method in embodiment, only change, be not listed one by one in data.
The embodiments of the present invention are for illustration only, can not represent the quality of embodiment.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the polyaniline nano microballoon with nucleocapsid, step include:
(1) polystyrene microsphere of monodispersity is prepared;
(2) by the polystyrene microsphere ultrasonic disperse to nitrating agent in step (1), 1~2h is reacted at 40~50 DEG C, is washed
It washs, be dried to obtain nitrification polystyrene microsphere;
(3) amination polystyrene microsphere will be obtained after the nitrification polystyrene microsphere reduction in step (2);
(4) aniline is dissolved in after obtaining aniline solution in non-polar organic solvent, then amination described in step (3) will be contained
The acidic aqueous solution of polystyrene microsphere and initiator is added drop-wise in above-mentioned aniline solution, after stable system, at -5~5 DEG C
Reaction 10~purify afterwards for 24 hours obtains the polyaniline nano microballoon with nucleocapsid after drying;In the acidic aqueous solution
Dodecyl sodium sulfate also containing Solute mass 10~20%.
2. the preparation method of the polyaniline nano microballoon with nucleocapsid according to claim 1, it is characterised in that:It is described
Polystyrene microsphere in step (1) is prepared by the method for emulsifier-free emulsion polymerization.
3. the preparation method of the polyaniline nano microballoon with nucleocapsid according to claim 1, it is characterised in that:It is described
Nitrating agent in step (2) is the concentrated sulfuric acid and concentrated nitric acid volume ratio is 3:2 mixed acid.
4. the preparation method of the polyaniline nano microballoon with nucleocapsid according to claim 1, it is characterised in that:It is described
Reduction in step (3) is to pass through Na2S2O4Or sodium borohydride reductase 12~5h at 70~80 DEG C is obtained.
5. the preparation method of the polyaniline nano microballoon with nucleocapsid according to claim 1, it is characterised in that:It is described
Initiator is ammonium persulfate.
6. the preparation method of the polyaniline nano microballoon with nucleocapsid according to claim 1, it is characterised in that:It is described
Acidic aqueous solution in step (4) is the sulfuric acid or aqueous hydrochloric acid solution that concentration is 0.5mol/L.
7. the preparation method of the polyaniline nano microballoon with nucleocapsid according to claim 1, it is characterised in that:It is described
Purifying in step (4) is filtered after acetone is added, and is obtained after then being washed with ethyl alcohol.
8. the preparation method of the polyaniline nano microballoon with nucleocapsid according to claim 1, it is characterised in that:It is described
The mass ratio of amination polystyrene microsphere and aniline is 1 in step (4):(1~4).
9. the preparation method of the polyaniline nano microballoon with nucleocapsid according to claim 1, it is characterised in that:It is described
The molar ratio of aniline and initiator is 1 in step (4):(0.5~5).
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导电聚苯胺/聚苯乙烯核/壳结构复合微球的制备;周辰等;《天津科技大学学报》;20061231;第21卷(第4期);14-16,20 * |
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