CN105037719A - Soluble polyaniline synthetic method - Google Patents
Soluble polyaniline synthetic method Download PDFInfo
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- CN105037719A CN105037719A CN201510558045.5A CN201510558045A CN105037719A CN 105037719 A CN105037719 A CN 105037719A CN 201510558045 A CN201510558045 A CN 201510558045A CN 105037719 A CN105037719 A CN 105037719A
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Abstract
The invention provides a soluble polyaniline synthetic method. Aniline serves as a monomer, SDS (lauryl sodium sulfate) serves as a soft template, Fe(II) serves as a catalyst, H2O2 serves as an oxidizing agent, and soluble polyaniline is synthesized rapidly in an HCl medium. The method is characterized in that the SDS can serve as the soft template of the soluble polyaniline catalyzed and synthesized by the Fe(II); when the concentration of the SDS is 0.02 mol/L, the concentration of the HCl is 0.30 mol/L, the concentration of the Fe(II) is 1.6*10<-4> mol/L, the concentration of the aniline is 0.011 mol/L, and the concentration of the H2O2 is 3.0*10<-4> mol/L, reaction is conducted at the temperature of 60 DEG C for 45 minutes, and a dark green, stable and transparent polyaniline solution can be obtained.
Description
Technical field
A synthetic method for soluble polyaniline, belongs to conducting polymer technical field.
Background technology
Polyaniline (PANI) has raw material and is easy to get, and the features such as cheap and unique oxidation-reduction quality, catalytic, proton exchange properties and photoelectric conversion, therefore all show application prospect widely in a lot of fields.But because polyaniline is water insoluble, make its application receive certain restriction.Therefore people take various way to improve its solubility and workability.At present, the research of the solubility problem of p-poly-phenyl amine makes great progress.The method solved probably has following several: prepare Polyaniline, utilize function protonic acid doping polyaniline, prepare polyaniline derivative or copolymer polyaniline, prepare polyaniline colloidal particle, be that template obtains water-soluble polyaniline with tensio-active agent.According to the literature, Liu Jiaming etc. first with polystyrolsulfon acid (PSSA) for template, FeCl
3for oxygenant has synthesized the PANI of water-soluble PSSA doping; After this people such as Angelopoulos take ammonium persulphate as the preparation that oxygenant in depth have studied acid doping PANI water-soluble polymers; And with oxyphorase biological enzyme for catalyzer, take SDS as template, be that monomer also can synthesizing soluble polyaniline with aniline, that play katalysis in the method is the Fe (II) in oxyphorase (Hb).If replace Hb as catalyzer using Fe (II) ion, catalytic efficiency is higher, and reduces experimental cost, Reaction time shorten.
Summary of the invention
The object of this invention is to provide a kind of synthetic method of soluble polyaniline.
Technical scheme of the present invention:
A synthetic method for soluble polyaniline, is characterized in that comprising the steps:
(1) take aniline as monomer, SDS is soft template, and HCl is medium, at Fe
2+and H
2o
2fast back-projection algorithm soluble polyaniline in the Fenton system formed.
(2) take SDS as template, SDS optimum concn is 0.020mol/L.
(3) optimizing HCl optimum concn is 0.30mol/L.
(4) optimizing Fe (II) optimum concn is 1.6 × 10
-4mol/L.
(5) optimizing aniline optimum concn is 0.011mol/L.
(6) H is optimized
2o
2optimum concn is 3.0 × 10
-4mol/L.
The present invention replaces biological enzyme as catalyzer using Fe (II), and catalytic efficiency is higher, and reduces costs, Reaction time shorten.Be soft template with SDS, take hydrogen peroxide as oxygenant, under the condition of HCl as protonic acid, catalyze and synthesize water-soluble polyaniline, and polymerizing condition is optimized, deep green, stable, transparent polyaniline solutions can be obtained.
Embodiment
The synthesis of embodiment 1 soluble polyaniline
A certain amount of HCl solution, SDS solution, aniline solution, FeSO is pipetted successively with valinche
4solution, H
2o
2solution, in 25mL volumetric flask, is used deionized water constant volume, is shaken up.Be placed on modulated in the digital display thermostat water bath of certain temperature, start reaction, timing.After reaction terminates, take deionized water as reference solution, with the absorption spectrum of measurement of ultraviolet-visible spectrophotometer product.
Embodiment 2SDS concentration optimization
The soluble polyaniline obtained in SDS micellar system has 3 obvious charateristic avsorption bands in the SPECTRAL REGION of 300 ~ 900nm; 320 ~ 360nm is the π-π on phenyl ring
*move two proton shifting peaks near peak and 450nm, between 700 ~ 800nm, show the conduction PANI defining high molecular in SDS micellar system.Examination different SDS concentration (0.02M, 0.03M, 0.04M, 0.05M) is on the impact of polymerization, and along with the reduction of SDS concentration, absorbancy increases gradually, and therefore the SDS of lower concentration is conducive to the generation of product.But SDS micella threshold concentration is in aqueous about 8 × 10
-3mol/L, when SDS concentration is lower than its micelle-forming concentration, has green precipitate to separate out, therefore selects 0.02mol/L to be the optimum concn of SDS.
Embodiment 3HCl concentration optimization
In reaction system, the effect of hydrochloric acid is as follows: form aniline hydrochloride with monomer; For polymerization provides a sour environment; For polyaniline provides doping agent; Participate in H
2o
2redox reaction, its potential value is raised.When acidity is too high (during higher than 2mol/L), electroconductibility, the productive rate of polyaniline decline; Under crossing highly acidity, product viscosity reduces, and polyaniline is hydrolyzed.That is, under highly acidity, the polymerization of aniline and polyaniline be hydrolyzed to competitive relation, polyaniline be hydrolyzed to principal reaction, cause the molecular weight of polyaniline to reduce, viscosity degradation.Examine or check the impact of different HCl concentration (1.0M, 0.30M, 0.10M, 0.030M, 0.010M, 0.0030M, 0.0010M) on polymerization.When HCl concentration is 0.30mol/L, product absorbancy has maximum value, so select 0.30mol/LHCl to be best medium.
Embodiment 4Fe (II) concentration optimization
Will by Fe
2+/ H
2o
2the reagent of composition is called Fenton reagent, uses the reaction of Fenton reagent to be called that Fenton reacts.In Fenton reaction, H
2o
2at Fe
2+katalysis under generate there is the hydroxyl radical free radical (OH) of high reaction activity
[12], hydroxyl radical free radical oxidation aniline generates polyaniline.Examine different Fe (II) concentration (0.04mM, 0.08mM, 0.12mM, 0.16mM, 0.2mM) to the impact of product absorbancy.Result shows, reacts and also can carry out when not adding Fe (II) catalyzer, but sluggish, product is yellow solution, and after 12h, products therefrom has the last one absorption peak in about 550nm place, and does not substantially absorb at 720nm.There is the PANI of strong absorption peak normally nonconducting in this region, illustrate in aqueous phase system, to define lower molecular weight insulation PANI.When catalyst levels is few, reaction product is less, and absorbancy is little; When catalyst levels is from 4.0 × 10
-5mol/L is increased to 8.0 × 10
-5during mol/L, absorbancy sharply increases, and reaction conversion ratio increases; Consumption continues to increase to 1.6 × 10
-4during mol/L, reaction conversion ratio is tending towards maximum value; When catalyst levels continues to increase, absorbancy declines on the contrary, and this may be that excessive Fe (II) forms too much hydroxyl radical free radical with hydrogen peroxide and causes polyaniline Partial digestion.Therefore select 1.6 × 10
-4mol/L is optimum catalyst consumption.
The optimization of embodiment 5 concentration of aniline
Investigate different concentration of aniline (2.2mM, 4.5mM, 6.7mM, 9.0mM, 11mM, 13Mm, 16mM) to the impact of polymerisate absorbancy.Result shows, along with the increase of concentration of aniline, absorbs and strengthens thereupon, absorb tend towards stability when concentration of aniline is at 0.011mol/L, therefore select concentration of aniline to be 0.011mol/L.
Embodiment 6H
2o
2concentration optimization
When other condition is fixed, investigate different H
2o
2concentration (0.1mM, 0.3mM, 0.5mM) is on the impact of product absorbancy.Result shows, along with H
2o
2concentration increases, and product absorbancy increases; But work as H
2o
2concentration is greater than 3.0 × 10
-4during mol/L, product absorbancy slightly declines on the contrary, and this may be because H
2o
2when consumption is too many, part H
2o
2disintegrate, causes utilization ratio to reduce.Therefore select H
2o
2concentration is 3.0 × 10
-4mol/L.The product obtained under this condition is the deep green clear solution of stable performance, has maximum absorption in 720nm place.
Claims (6)
1. a synthetic method for soluble polyaniline, is characterized in that: take aniline as monomer, and SDS is soft template, and HCl is medium, at Fe
2+and H
2o
2fast back-projection algorithm soluble polyaniline in the Fenton system formed.
2. synthetic method according to claim 1, it is characterized in that SDS is template, SDS optimum concn is 0.020mol/L.
3. synthetic method according to claim 1, is characterized in that HCl optimum concn is 0.30mol/L.
4. synthetic method according to claim 1, is characterized in that Fe (II) optimum concn is 1.6 × 10
-4mol/L.
5. synthetic method according to claim 1, is characterized in that aniline optimum concn is 0.011mol/L.
6. synthetic method according to claim 1, is characterized in that H
2o
2optimum concn 3.0 × 10
-4mol/L.
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108774320A (en) * | 2018-07-02 | 2018-11-09 | 合肥萃励新材料科技有限公司 | A kind of synthetic method of nickel oxide loaded polyaniline |
| CN109824891A (en) * | 2019-02-27 | 2019-05-31 | 扬州大学广陵学院 | A kind of synthetic method of polyaniline |
| CN111548486A (en) * | 2020-06-05 | 2020-08-18 | 扬州大学 | Synthetic method of polyaniline |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1667020A (en) * | 2005-01-10 | 2005-09-14 | 厦门大学 | Process for synthesizing electron donor substituted polyaniline derivatives |
-
2015
- 2015-09-02 CN CN201510558045.5A patent/CN105037719A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1667020A (en) * | 2005-01-10 | 2005-09-14 | 厦门大学 | Process for synthesizing electron donor substituted polyaniline derivatives |
Non-Patent Citations (1)
| Title |
|---|
| 张磊等: "乳液聚合法制备聚苯胺及其电容性能研究", 《化工新型材料》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108774320A (en) * | 2018-07-02 | 2018-11-09 | 合肥萃励新材料科技有限公司 | A kind of synthetic method of nickel oxide loaded polyaniline |
| CN109824891A (en) * | 2019-02-27 | 2019-05-31 | 扬州大学广陵学院 | A kind of synthetic method of polyaniline |
| CN111548486A (en) * | 2020-06-05 | 2020-08-18 | 扬州大学 | Synthetic method of polyaniline |
| CN111548486B (en) * | 2020-06-05 | 2022-11-08 | 扬州大学 | Synthetic method of polyaniline |
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