CN109535395B - Interface synthesis method of poly 3-fluorothiophene nanowire - Google Patents
Interface synthesis method of poly 3-fluorothiophene nanowire Download PDFInfo
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- CN109535395B CN109535395B CN201811350731.3A CN201811350731A CN109535395B CN 109535395 B CN109535395 B CN 109535395B CN 201811350731 A CN201811350731 A CN 201811350731A CN 109535395 B CN109535395 B CN 109535395B
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G61/12—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule
- C08G61/122—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides
- C08G61/123—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds
- C08G61/126—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds with a five-membered ring containing one sulfur atom in the ring
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- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
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- C08G2261/10—Definition of the polymer structure
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- C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
- C08G2261/32—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain
- C08G2261/322—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed
- C08G2261/3223—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed containing one or more sulfur atoms as the only heteroatom, e.g. thiophene
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Abstract
The invention provides an interface synthesis method of a poly 3-fluorothiophene nanowire, which is characterized by comprising the following steps of: adding 3-fluorothiophene into n-hexane, stirring for dissolving, dissolving ferric trichloride and p-toluenesulfonic acid into an acetonitrile solution, adding into the previous n-hexane to form an immiscible solution interface, standing for reacting for 6-12 hours, precipitating in the lower acetonitrile solution, filtering, washing and drying to obtain the poly-3-fluorothiophene nanowire. The method has simple process, adopts common raw materials, and the synthesized poly-3-fluorothiophene nanowire has stable structure, higher specific surface area, greatly increased catalytic activity and electrochemical activity and better physical and chemical properties.
Description
Technical Field
The invention belongs to the technical field of material chemistry, and relates to an interface synthesis method of a poly (3-fluorothiophene) nanowire.
Background
The poly-3-fluorothiophene is a monofluoro substituted derivative of polythiophene, the fluoro-3-fluorothiophene has a skeleton structure similar to that of polythiophene, a strong electron-withdrawing substituent is introduced into a conjugated aromatic ring, and the poly-3-fluorothiophene has a certain application prospect in the fields of gas sensors, biosensors, anticorrosive coatings, supercapacitors, electrocatalysis, electrochromism and the like. A great deal of research work reports the synthesis, structure regulation and application development of polythiophene and a derivative poly-3-alkylthiophene thereof, but the polymerization of 3-fluorothiophene is only reported at present, and the invention synthesizes poly-3-fluorothiophene nanowires by oxidative polymerization on an n-hexane and acetonitrile interface.
Disclosure of Invention
The invention aims to provide an interface synthesis method of a poly 3-fluorothiophene nanowire, which is characterized by comprising the following steps: adding 3-fluorothiophene into n-hexane, stirring for dissolving, dissolving ferric trichloride and p-toluenesulfonic acid into an acetonitrile solution, adding into the previous n-hexane to form an immiscible solution interface, standing for reacting for 6-12 hours, precipitating in the lower acetonitrile solution, filtering, washing and drying to obtain the poly-3-fluorothiophene nanowire.
The concentration of the 3-fluorothiophene monomer in n-hexane is 1 mmol/L-2 mmol/L.
The concentration of the p-toluenesulfonic acid in acetonitrile is 0.01-0.02 mol/L.
The addition amount of the ferric trichloride is 3-6 times of that of the 3-fluorothiophene monomer.
The washing is alternately washing by using deionized water and ethanol, filtering is carried out by adopting a centrifuge precipitation or suction filtration device after each washing, a filtered product is dispersed in the deionized water or the ethanol again, the filtering is repeated until the pH value of the filtrate is 7, and the final washing by using the ethanol is convenient for drying; the drying is carried out in a vacuum oven at 50-80 ℃, and the vacuum degree is less than 133 Pa.
The method has simple process, adopts common raw materials, and the synthesized poly-3-fluorothiophene nanowire has stable structure, higher specific surface area, greatly increased catalytic activity and electrochemical activity and better physical and chemical properties.
While the invention has been disclosed in the foregoing description with reference to specific embodiments thereof, the foregoing description is directed to only certain specific embodiments of the invention and many more specific features of the invention may be employed than as disclosed herein. Therefore, the scope of the present invention should not be limited to the disclosure of the embodiments, but should include all combinations of the contents embodied in different parts, and various substitutions and modifications without departing from the present invention, and are covered by the claims of the present invention.
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FIG. 1 is a scanning electron micrograph of a poly-3-fluorothiophene nanowire synthesized according to the present invention (example 1).
Detailed Description
Example 1
Adding 1 mmol/L3-fluorothiophene into 50mL n-hexane, stirring for dissolving, dissolving 6mmol/L ferric trichloride and 0.02mol/L p-toluenesulfonic acid into 50mL acetonitrile solution, adding into the previous n-hexane to form an immiscible solution interface, standing for 12 hours for reaction, precipitating in the lower layer acetonitrile solution, filtering, washing and drying to obtain the poly-3-fluorothiophene nanowire shown in figure 1.
Example 2
Adding 1 mmol/L3-fluorothiophene into 50mL n-hexane, stirring for dissolving, dissolving 4mmol/L ferric trichloride and 0.01mol/L p-toluenesulfonic acid into 50mL acetonitrile solution, adding into the previous n-hexane to form a solution interface which is not mutually soluble, standing for 8 hours for reaction, precipitating in the lower layer acetonitrile solution, filtering, washing and drying to obtain the poly-3-fluorothiophene nanowire.
Example 3
Adding 2 mmol/L3-fluorothiophene into 50mL n-hexane, stirring for dissolving, dissolving 6mmol/L ferric trichloride and 0.01mol/L p-toluenesulfonic acid into 50mL acetonitrile solution, adding into the previous n-hexane to form a solution interface which is not mutually soluble, standing for 6 hours for reaction, precipitating in the lower layer acetonitrile solution, filtering, washing and drying to obtain the poly-3-fluorothiophene nanowire.
Claims (5)
1. An interface synthesis method of a poly 3-fluorothiophene nanowire is characterized by comprising the following steps: adding 3-fluorothiophene into n-hexane, stirring for dissolving, dissolving ferric trichloride and p-toluenesulfonic acid into an acetonitrile solution, adding into the previous n-hexane to form an immiscible solution interface, standing for reacting for 6-12 hours, precipitating in the lower acetonitrile solution, filtering, washing and drying to obtain the poly-3-fluorothiophene nanowire.
2. The interfacial synthesis method of poly-3-fluorothiophene nanowires of claim 1, wherein: the concentration of the 3-fluorothiophene monomer in n-hexane is 1 mmol/L-2 mmol/L.
3. The interfacial synthesis method of poly-3-fluorothiophene nanowires of claim 1, wherein: the concentration of the p-toluenesulfonic acid in acetonitrile is 0.01-0.02 mol/L.
4. The interfacial synthesis method of poly-3-fluorothiophene nanowires of claim 1, wherein: the addition amount of the ferric trichloride is 3-6 times of that of the 3-fluorothiophene monomer.
5. The interfacial synthesis method of poly-3-fluorothiophene nanowires of claim 1, wherein: the washing is alternately washing by using deionized water and ethanol, filtering is carried out by adopting a centrifuge precipitation or suction filtration device after each washing, a filtered product is dispersed in the deionized water or the ethanol again, the filtering is repeated until the pH value of the filtrate is 7, and the final washing by using the ethanol is convenient for drying; the drying is carried out in a vacuum oven at 50-80 ℃, and the vacuum degree is less than 133 Pa.
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Citations (8)
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|---|---|---|---|---|
| CN101168591A (en) * | 2007-11-27 | 2008-04-30 | 同济大学 | Process for synthesizing polythiophene |
| CN101575752A (en) * | 2009-06-02 | 2009-11-11 | 武汉工程大学 | Interfacial synthesis method of conductive polymer/silver chloride compound nanofiber |
| CN102532892A (en) * | 2012-01-20 | 2012-07-04 | 北京师范大学 | Conductive polymer film and preparation method thereof |
| CN102993646A (en) * | 2012-12-05 | 2013-03-27 | 常州大学 | Polythiophene nanometer conductive composite material and preparation method thereof |
| CN103147155A (en) * | 2013-04-08 | 2013-06-12 | 福建师范大学 | Preparation method of conjugated polymer nanofiber with crosslinking group |
| CN103265700A (en) * | 2013-05-08 | 2013-08-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Polyfluoroaniline nano-wire preparation method |
| CN104031244A (en) * | 2014-01-08 | 2014-09-10 | 上海大学 | Method for rapidly preparing polythiophene in mixed solvent system |
| KR101743907B1 (en) * | 2015-06-11 | 2017-06-08 | 한국과학기술원 | Water processable polythiophene nanowires and methods for preparing the same |
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| TWI567101B (en) * | 2013-09-23 | 2017-01-21 | 崑山科技大學 | Polythiophene nanocrystalline pillars for organic solar panels and methods for their preparation |
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168591A (en) * | 2007-11-27 | 2008-04-30 | 同济大学 | Process for synthesizing polythiophene |
| CN101575752A (en) * | 2009-06-02 | 2009-11-11 | 武汉工程大学 | Interfacial synthesis method of conductive polymer/silver chloride compound nanofiber |
| CN102532892A (en) * | 2012-01-20 | 2012-07-04 | 北京师范大学 | Conductive polymer film and preparation method thereof |
| CN102993646A (en) * | 2012-12-05 | 2013-03-27 | 常州大学 | Polythiophene nanometer conductive composite material and preparation method thereof |
| CN103147155A (en) * | 2013-04-08 | 2013-06-12 | 福建师范大学 | Preparation method of conjugated polymer nanofiber with crosslinking group |
| CN103265700A (en) * | 2013-05-08 | 2013-08-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Polyfluoroaniline nano-wire preparation method |
| CN104031244A (en) * | 2014-01-08 | 2014-09-10 | 上海大学 | Method for rapidly preparing polythiophene in mixed solvent system |
| KR101743907B1 (en) * | 2015-06-11 | 2017-06-08 | 한국과학기술원 | Water processable polythiophene nanowires and methods for preparing the same |
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