CN101575751B - Method for preparing conductive polymer/silver chloride compound nanofiber on ion liquid/water interface - Google Patents
Method for preparing conductive polymer/silver chloride compound nanofiber on ion liquid/water interface Download PDFInfo
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- CN101575751B CN101575751B CN2009100623745A CN200910062374A CN101575751B CN 101575751 B CN101575751 B CN 101575751B CN 2009100623745 A CN2009100623745 A CN 2009100623745A CN 200910062374 A CN200910062374 A CN 200910062374A CN 101575751 B CN101575751 B CN 101575751B
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Abstract
The invention relates to a method for preparing conductive polymer/silver chloride compound nanofiber on an ion liquid/water interface. The method includes the following steps of: 1) preparation of solution A: first adding conductive polymer monomer and hydrochloric acid to ion liquid to obtain solution A; 2) preparation of solution B: then adding silver nitrate, iron nitrate and helianthine to water to obtain solution B; and 3) slowly pouring the solution B to the solution A to form an interface in between, standing, centrifugalizing water phase and washing the precipitate with dilute acid, distilled water and ethanol respectively for three times, and drying the obtained solid powder under vacuum to subsequently obtain the conductive polymer/silver chloride compound nanofiber. The method achieves the following technical effects: 1) by adopting an interfacial synthesis method, the conductive polymer/silver chloride compound nanofiber can be obtained through one-step reaction, the preparation process is simple, the operation is easy and the technological flow process is short; and 2) by adopting the ion liquid and water as the solvents which are both green solvents, no pollution is caused to the environment.
Description
Technical field
The present invention relates to a kind of method for preparing conducting polymer/silver chloride compound nanofiber in ionic liquid/water termination.
Background technology
Conducting polymer is because its electrical conductivity height, synthetic simple, stable in properties, narrower, the easy processing of bandwidth, can be employed in many aspects, such as luminescent device, electronic device, chemical sensor, diffusion barrier, antistatic coating and electric chemical super capacitor.In recent years, people carry out inorganic material and conducting polymer compound, give full play to inorganic material and conducting polymer advantage separately, preparation conducting polymer/inorganic composite nano material.Because physical property that they are interesting and potential application, conducting polymer/inorganic composite nano material has attracted the interest of academia and industrial quarters.Shape, size and the pattern of control composite nano materials also have conducting polymer and the compound uniformity of inorganic material, for its performance of control, are very important such as electron energy band spacing, electrical conductivity and luminous efficiency.
The synthetic method of conducting polymer can be divided into chemical method and electrochemical method substantially.Wherein, electrochemical method for synthesizing can obtain conducting polymer film, but is not easy the disposable conducting polymer/inorganic composite nano material that obtains.Chemical synthesis process often obtains neutral conducting polymer, and electrical conductivity is positioned at semi-conductive scope, and through overdoping, its electrical conductivity can increase substantially.Interfacial polymerization is one of new method of a kind of chemical synthesis conducting polymer, has synthesized nanometer fibrous, granular conducting polymer composite by interfacial polymerization.
Ionic liquid is a kind of new organic salt of broad development in recent years, is in a liquid state near room temperature.Compare with traditional volatile organic solvent, ionic liquid has electrochemical window, Gao Re and the advantages such as some chemistry stability and selective dissolution ability of good electrical conductivity, non-volatile, broad, so it has been synthetic at organic catalysis, unique effect has been brought into play in fields such as organic electrochemistry is synthetic, electrochemistry, biochemistry.Ionic liquid is a kind of good green solvent owing to non-volatile and incombustibility, and helps mixing synchronously in the process of conducting high polymers owing to containing inorganic anion in its composition.In view of above advantage, existing bibliographical information passes through chemistry or electrochemical method compositing conducting macromolecule in ionic liquid.
Summary of the invention
Problem to be solved by this invention is that propose at above-mentioned existing deficiency a kind of prepares the method for conducting polymer/silver chloride compound nanofiber in ionic liquid/water termination, and this method technology is simple, operation easily, technological process are short.
The present invention for the solution that problem adopts of the above-mentioned proposition of solution is: a kind ofly prepare the method for conducting polymer/silver chloride compound nanofiber in ionic liquid/water termination, it is characterized in that including following steps:
1) preparation of A solution: at first conductive high polymer monomer, the 1-2mmol hydrochloric acid with 1mmol-5mmol joins in the ionic liquid of 10-20mL, obtains A solution;
2) preparation of B solution: in the water of 10-20mL, add silver nitrate, the ferric nitrate of 0.25mmol-2mmol and the methyl orange of 0.1mmol-0.2mmol of 0.25mmol-2mmol again, obtain B solution;
3) slowly pour B solution into A solution, between forms the interface, after leaving standstill 24-48 hour, the centrifugation water, sediment is respectively washed 3 times with diluted acid, distilled water, ethanol, and the gained pressed powder can obtain conducting polymer/silver chloride compound nanofiber in 24 hours 40 ℃ of following vacuumizes.
Press such scheme, described conductive high polymer monomer is pyrroles, aniline or methylpyrrole.
Press such scheme, described ionic liquid is 1-butyl-3-methylimidazole hexafluorophosphate or 1-butyl-3-methyl imidazolium tetrafluoroborate.
Press such scheme, described diluted acid is watery hydrochloric acid, spirit of vinegar or dilute sulfuric acid.
Compared with the prior art, the technique effect that reached of the present invention:
1) interfacial synthesis method of Cai Yonging, single step reaction has obtained conducting polymer/silver chloride compound nanofiber; Simple, the easy operation of preparation technology, technological process weak point.
2) solvent of the present invention's employing is ionic liquid and water, all is green solvents, can not cause the pollution to environment.
Description of drawings
Fig. 1 is the X-ray diffractogram of the polypyrrole/silver chloride compound nanofiber of the inventive method preparation.
The specific embodiment
For a better understanding of the present invention, further illustrate content of the present invention, but content of the present invention not only is confined to the following examples below in conjunction with embodiment.
Embodiment 1:
1) preparation of A solution: pyrrole monomer, the 1mL hydrochloric acid (1mol/L) with 1mmol adds in ionic liquid 1-butyl-3-methylimidazole hexafluorophosphate of 10mL earlier, obtains A solution;
2) preparation of B solution: the methyl orange of the ferric nitrate of the silver nitrate of 0.25mmol, 0.25mmol and 0.1mmol in the water of 10mL obtains B solution;
3) slowly pour B solution into A solution, between forms the interface.After leaving standstill 24 hours, the centrifugation water respectively washs sediment 3 times with watery hydrochloric acid, distilled water, ethanol, and the gained pressed powder can obtain polypyrrole/silver chloride compound nanofiber in 24 hours 40 ℃ of following vacuumizes, and diameter is between 100-250nm.Observe with X-ray diffraction, the result shows that polypyrrole/silver chloride compound nanofiber contains polypyrrole and silver chlorate, as shown in Figure 1.
Embodiment 2:
1) preparation of A solution: earlier 2mmol aniline monomer, 2mL hydrochloric acid (1mol/L) are added in ionic liquid 1-butyl-3-methylimidazole hexafluorophosphate of 10mL, obtain A solution;
2) preparation of B solution: the methyl orange of the ferric nitrate of the silver nitrate of 0.5mmol, 0.25mmol and 0.1mmol in the water of 10mL obtains B solution;
3) slowly pour B solution into A solution, between forms the interface.After leaving standstill 24 hours, the centrifugation water respectively washs sediment 3 times with spirit of vinegar, distilled water, ethanol, and the gained pressed powder can obtain polyaniline/silver chloride compound nanofiber in 24 hours 40 ℃ of following vacuumizes, and diameter is between 80-250nm.
Embodiment 3:
1) preparation of A solution: methylpyrrole monomer, the 1mL hydrochloric acid (1mol/L) with 1mmol adds in ionic liquid 1-butyl-3-methylimidazole hexafluorophosphate of 20mL earlier, obtains A solution;
2) preparation of B solution: the methyl orange of the ferric nitrate of the silver nitrate of 1mmol, 1mmol and 0.1mmol in the water of 20mL obtains B solution;
3) slowly pour B solution into A solution, between forms the interface.After leaving standstill 36 hours, the centrifugation water respectively washs sediment 3 times with watery hydrochloric acid, distilled water, ethanol, and the gained pressed powder can obtain poly-methyl pyrrole/silver chloride compound nanofiber in 24 hours 40 ℃ of following vacuumizes, and diameter is between 100-280nm.
Embodiment 4:
1) preparation of A solution: methylpyrrole monomer, the 2mL hydrochloric acid (1mol/L) with 5mmol adds in ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate of 20mL earlier, obtains A solution;
2) preparation of B solution: the methyl orange of the ferric nitrate of the silver nitrate of 2mmol, 2mmol and 0.15mmol in the water of 20mL obtains B solution;
3) slowly pour B solution into A solution, between forms the interface.After leaving standstill 48 hours, the centrifugation water respectively washs sediment 3 times with spirit of vinegar, distilled water, ethanol, and the gained pressed powder can obtain poly-methyl pyrrole/silver chloride compound nanofiber in 24 hours 40 ℃ of following vacuumizes, and diameter is between 80-200nm.
Embodiment 5:
1) preparation of A solution: pyrrole monomer, the 2mL hydrochloric acid (1mol/L) with 3mmol adds in ionic liquid 1-butyl-3-methylimidazole hexafluorophosphate of 15mL earlier, obtains A solution;
2) preparation of B solution: the ferric nitrate of the silver nitrate of 0.3mmol, 0.3mmol and 0.1 methyl orange in the water of 15mL obtain B solution;
3) slowly pour B solution into A solution, between forms the interface.After leaving standstill 36 hours, the centrifugation water respectively washs sediment 3 times with dilute sulfuric acid, distilled water, ethanol, and the gained pressed powder can obtain polypyrrole/silver chloride compound nanofiber in 24 hours 40 ℃ of following vacuumizes, and diameter is between 90-300nm.。
Embodiment 6:
1) preparation of A solution: aniline monomer, the 2mL hydrochloric acid (1mol/L) with 4mmol adds in ionic liquid 1-butyl-3-methylimidazole hexafluorophosphate of 20mL earlier, obtains A solution;
2) preparation of B solution: the methyl orange of the ferric nitrate of the silver nitrate of 1mmol, 1.5mmol and 0.1mmol in the water of 120mL obtains B solution;
3) slowly pour B solution into A solution, between forms the interface.After leaving standstill 36 hours, the centrifugation water respectively washs sediment 3 times with dilute sulfuric acid, distilled water, ethanol, and the gained pressed powder can obtain polyaniline/silver chloride compound nanofiber in 24 hours 40 ℃ of following vacuumizes, and diameter is between 120-330nm.。
Embodiment 7:
1) preparation of A solution: methylpyrrole monomer, the 2mL hydrochloric acid (1mol/L) with 3mmol adds in ionic liquid 1-butyl-3-methylimidazole hexafluorophosphate of 10mL earlier, obtains A solution;
2) preparation of B solution: the methyl orange of the ferric nitrate of the silver nitrate of 0.5mmol, 1mmol and 0.15mmol in the water of 10mL obtains B solution;
3) slowly pour B solution into A solution, between forms the interface.After leaving standstill 24 hours, the centrifugation water respectively washs sediment 3 times with watery hydrochloric acid, distilled water, ethanol, and the gained pressed powder can obtain poly-methyl pyrrole/silver chloride compound nanofiber in 24 hours 40 ℃ of following vacuumizes, and diameter is between 80-270nm.。
Embodiment 8:
1) preparation of A solution: earlier 1mmol aniline monomer, 1mL hydrochloric acid (1mol/L) are added in ionic liquid 1-butyl-3-methylimidazole hexafluorophosphate of 10mL, obtain A solution;
2) preparation of B solution: the ferric nitrate of the silver nitrate of 0.25mmol, 1mmol and 0.1mmol methyl orange in the water of 10mL obtain B solution;
3) slowly pour B solution into A solution, between forms the interface.After leaving standstill 48 hours, the centrifugation water respectively washs sediment 3 times with dilute sulfuric acid, distilled water, ethanol, and the gained pressed powder can obtain polyaniline/silver chloride compound nanofiber in 24 hours 40 ℃ of following vacuumizes, and diameter is between 120-280nm.。
Each cited raw material of the present invention can both be realized the present invention, and the bound value of each raw material, interval value can both realize the present invention; Do not enumerate embodiment one by one at this.Bound value, the interval value of technological parameter of the present invention (as temperature, time etc.) can both be realized the present invention, do not enumerate embodiment one by one at this.
Claims (4)
1. one kind prepares the method for conducting polymer/silver chloride compound nanofiber in ionic liquid/water termination, it is characterized in that including following steps:
1) preparation of A solution: at first conductive high polymer monomer, the 1-2mmol hydrochloric acid with 1mmol-5mmol joins in the ionic liquid of 10-20mL, obtains A solution;
2) preparation of B solution: in the water of 10-20mL, add silver nitrate, the ferric nitrate of 0.25mmol-2mmol and the methyl orange of 0.1mmol-0.2mmol of 0.25mmol-2mmol again, obtain B solution;
3) slowly pour B solution into A solution, between forms the interface, after leaving standstill 24-48 hour, the centrifugation water, sediment is respectively washed 3 times with diluted acid, distilled water, ethanol, and the gained pressed powder can obtain conducting polymer/silver chloride compound nanofiber in 24 hours 40 ℃ of following vacuumizes.
2. a kind ofly prepare the method for conducting polymer/silver chloride compound nanofiber by claim 1 is described, it is characterized in that described conductive high polymer monomer is pyrroles, aniline or methylpyrrole in ionic liquid/water termination.
3. describedly a kind ofly prepare the method for conducting polymer/silver chloride compound nanofiber by claim 1 or 2, it is characterized in that described ionic liquid is 1-butyl-3-methylimidazole hexafluorophosphate or 1-butyl-3-methyl imidazolium tetrafluoroborate in ionic liquid/water termination.
4. describedly a kind ofly prepare the method for conducting polymer/silver chloride compound nanofiber by claim 1 or 2, it is characterized in that described diluted acid is watery hydrochloric acid, spirit of vinegar or dilute sulfuric acid in ionic liquid/water termination.
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