CN1626564A - Technique for synthesizing polyaniline from atmospheric oxidation - Google Patents
Technique for synthesizing polyaniline from atmospheric oxidation Download PDFInfo
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- CN1626564A CN1626564A CN 200310111159 CN200310111159A CN1626564A CN 1626564 A CN1626564 A CN 1626564A CN 200310111159 CN200310111159 CN 200310111159 CN 200310111159 A CN200310111159 A CN 200310111159A CN 1626564 A CN1626564 A CN 1626564A
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Abstract
A process for preparing polyphenylamine by air oxidizing includes using air to oxidize the phenylamine in the aqueous solution of hydrochloric acid to obtain the deposit of polyphenylamine, filter, washing, baking, grinding to obtain electrically conductive polyphenylamine doped by hydrochloc acid, immersing in ammonia solution, filtering, washing, baking, and grinding to obtain target product.
Description
Technical field:
The present invention relates to a kind of application of air as oxygenant, to make aniline oxypolymerization be the novel method of polyaniline, belongs to the macromolecule chemical industry field in the chemical industry class.
Background technology:
Polyaniline is a kind of conducting polymer composite, is applied to electronic product, luminescent material, protection against corrosion, aspect such as antistatic.The polyaniline product can be divided into two big classes: polyaniline in eigenstate and conductive polyaniline.Polyaniline in eigenstate can be converted into conductive polyaniline behind protonic acid doping.Conductive polyaniline can be converted into polyaniline in eigenstate again behind the basic solution dedoping.Polyaniline in eigenstate does not have electroconductibility.
Oxidative polymerization by aniline can synthesize and obtains polyaniline.Normally add oxygenant in the acidic aqueous solution of aniline, reaction obtains the polyaniline throw out, through filtering, washing, oven dry, obtaining the polyaniline product after grinding supervisor.The oxygenant of studying comprises ammonium persulphate, potassium bichromate, hydrogen peroxide etc., and wherein modal is ammonium persulphate.
Changchun Inst. of Applied Chemistry, Chinese Academy of Sciences once just in organic solvent/water mixed solvent, used ammonium persulphate oxygenant synthesized polyaniline the method application national patent (China Patent No.: CN1141310A).Its claim mainly is at organic solvent/water mixed solvent of being invented.It is said, use this mixed solvent and replace the pure water solvent can improve the quality of polyaniline.Directly use and have side chain and bad situation such as crosslinked in the polyaniline macromole that the ammonium persulphate oxygenant obtains from the aniline acidic aqueous solution.
The price of ammonium persulphate oxygenant is higher, and its reduzate ammonium sulfate will remain in the waste liquid.Replace the pure water solvent can improve the quality of polyaniline though use organic solvent/water mixed solvent, increased the cost of liquid waste disposal because of there being organic solvent in the waste liquid.Too high production cost has limited the widespread use of polyaniline.
Summary of the invention:
The objective of the invention is at the deficiencies in the prior art, propose a kind of novel method for preparing polyaniline.
We once paper (
Chuanping LiaoMingyuan Gu. " Electroless deposition of polyanilinefilm via autocatalytic polymerization of aniline " .Thin Solid Films, 2002,408 (1-2): propose the method by aniline autocatalysis polymerization synthesized polyaniline 37～42.): under the catalysis of platinum or palladium caused, airborne oxygen can be oxidized to the aniline in the acidic solution and be adsorbed on platinum or the suprabasil polyaniline film of palladium; Then under the self-catalysis of polyaniline film, reaction is proceeded.Use for reference aniline autocatalysis polymeric reaction principle, the present invention proposes the method for atmospheric oxidation synthesized polyaniline.
Technical scheme of the present invention is: in the hydrochloric acid acidic solution of aniline, add a spot of doped hydrochloride polyaniline powder in advance, constantly blast air then in solution; Under the katalysis of polyaniline powder, airborne oxygen is polyaniline with aniline oxypolymerization; Then under the self-catalysis of polyaniline product, reaction is proceeded; After treating the aniline complete reaction, after throw out filtration, washing, oven dry, grinding, obtain the polyaniline product.
Concrete technology of the present invention is: 1) contain 10%～30% aniline, pH value scope at 0～3 acidic solution with hydrochloric acid preparation; 2) in aforementioned solution, add the doped hydrochloride polyaniline powder of 0.1%～10% (with respect to the aniline amount in the solution); 3) in solution, blasted air 20～30 hours with air compressor; 4) resulting throw out filtered, wash with water, heating, drying, grinding, obtain the electrically conductive polyaniline of doped hydrochloride; 5) electrically conductive polyaniline of doped hydrochloride is soaked in 1%～10% the ammoniacal liquor, stirred 0.1～2 hour, and then filter, wash with water, heating, drying, grinding, obtain polyaniline in eigenstate.
Can be dissolved in N-Methyl pyrrolidone fully at the resultant polyaniline in eigenstate of the present invention, solubleness＞10%, in conjunction with infrared spectra and results of elemental analyses, the description architecture height is regular, does not have side chain and crosslinked situation in the macromolecular structure, and quality product is good; Number-average molecular weight is about 2500, and molecular weight distribution is about 1.5; The specific conductivity of doped hydrochloride electrically conductive polyaniline is greater than 1Scm
-1The present invention has reduced the production cost of polyaniline from three aspects: the cost of 1) having saved the ammonium persulphate oxygenant; 2) use pure water as solvent, saved the cost of organic solvent; 3) because the atmospheric oxidation agent is excessive far away, the transformation efficiency of aniline is very high, is higher than 98%; 4) very a spot of oligomer of phenylamine is only arranged in the waste liquid, liquid waste disposal is simple.
Embodiment:
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1
1) to contain 10% aniline, pH value be 0 hydrochloric acid soln to preparation 300mL; 2) in aforementioned solution, add 3g doped hydrochloride polyaniline powder; 3) in solution, blasted air 30 hours with air compressor; 4) resulting throw out filtered, wash with water, heating, drying, grinding, obtain the electrically conductive polyaniline of doped hydrochloride; 5) electrically conductive polyaniline with doped hydrochloride is soaked in the ammoniacal liquor of 300mL 1%, stirred 2 hours, and then filter, wash with water, heating, drying, grinding, obtain polyaniline in eigenstate.
Embodiment 2
1) to contain 20% aniline, pH value be 1.5 hydrochloric acid soln to preparation 150mL; 2) in aforementioned solution, add 0.3g doped hydrochloride polyaniline powder; 3) in solution, blasted air 25 hours with air compressor; 4) resulting throw out filtered, wash with water, heating, drying, grinding, obtain the electrically conductive polyaniline of doped hydrochloride; 5) electrically conductive polyaniline with doped hydrochloride is soaked in the ammoniacal liquor of 200mL 5%, stirred 1 hour, and then filter, wash with water, heating, drying, grinding, obtain polyaniline in eigenstate.
Embodiment 3
1) to contain 30% aniline, pH value be 3 hydrochloric acid soln to preparation 100mL; 2) in aforementioned solution, add 0.03g doped hydrochloride polyaniline powder; 3) in solution, blasted air 25 hours with air compressor; 4) resulting throw out filtered, wash with water, heating, drying, grinding, obtain the electrically conductive polyaniline of doped hydrochloride; 5) electrically conductive polyaniline with doped hydrochloride is soaked in the ammoniacal liquor of 100mL 10%, stirred 0.1 hour, and then filter, wash with water, heating, drying, grinding, obtain polyaniline in eigenstate.
Claims (1)
1, a kind of method of synthesized polyaniline is characterized in that comprising following concrete steps:
1) in the hydrochloric acid soln of aniline, adds the doped hydrochloride polyaniline powder of 0.1%～10% (with respect to the aniline amount in the solution) in advance;
2) blasted air 20～30 hours to aforementioned solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111159 CN1626564A (en) | 2003-12-10 | 2003-12-10 | Technique for synthesizing polyaniline from atmospheric oxidation |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200310111159 CN1626564A (en) | 2003-12-10 | 2003-12-10 | Technique for synthesizing polyaniline from atmospheric oxidation |
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| CN1626564A true CN1626564A (en) | 2005-06-15 |
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| CN 200310111159 Pending CN1626564A (en) | 2003-12-10 | 2003-12-10 | Technique for synthesizing polyaniline from atmospheric oxidation |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332997C (en) * | 2006-03-02 | 2007-08-22 | 扬州大学 | Chemical synthesization of poly-o-toluidine |
| CN104530425A (en) * | 2014-12-10 | 2015-04-22 | 中南大学 | Copper doped poly(m-phenylenediamine) nanoparticle and synthesis and application method thereof |
| CN109824891A (en) * | 2019-02-27 | 2019-05-31 | 扬州大学广陵学院 | A kind of synthetic method of polyaniline |
-
2003
- 2003-12-10 CN CN 200310111159 patent/CN1626564A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332997C (en) * | 2006-03-02 | 2007-08-22 | 扬州大学 | Chemical synthesization of poly-o-toluidine |
| CN104530425A (en) * | 2014-12-10 | 2015-04-22 | 中南大学 | Copper doped poly(m-phenylenediamine) nanoparticle and synthesis and application method thereof |
| CN109824891A (en) * | 2019-02-27 | 2019-05-31 | 扬州大学广陵学院 | A kind of synthetic method of polyaniline |
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