CN102675877B - Polypyrrole nanowire, and preparation method and usage thereof - Google Patents
Polypyrrole nanowire, and preparation method and usage thereof Download PDFInfo
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- CN102675877B CN102675877B CN 201110066952 CN201110066952A CN102675877B CN 102675877 B CN102675877 B CN 102675877B CN 201110066952 CN201110066952 CN 201110066952 CN 201110066952 A CN201110066952 A CN 201110066952A CN 102675877 B CN102675877 B CN 102675877B
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- polypyrrole
- alumina formwork
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- benzoglyoxaline
- nano line
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Abstract
The invention discloses a polypyrrole nanowire, and a preparation method and usage thereof. The nanowire is linear polypyrrole decorated with 2-guanethidine benzimidazole, the linear diameter of the nanowire is 25-35nm, and the linear length of the nanowire is 10-80mum. According to the method, after a through-hole alumina template is obtained by a secondary anodic oxidation method, one side of the template is plated with a gold film in a steaming mode firstly, then the template is soaked in an ethanol solution of the 2-guanethidine benzimidazole for at least 2h, the 2-guanethidine benzimidazole on the surface of the template is washed away with ethanol, a template of which a pored inner wall is covered with the 2-guanethidine benzimidazole is obtained, then the template of which one sideis covered with the gold film and the pored inner wall is covered with the 2-guanethidine benzimidazole is put in a pyrrole ethanol water solution, the template is used as an anode and graphite is used as a cathode for electrolytic deposition for 2-8h at a direct current voltage to obtain a template with one side covered with the gold film and with the polypyrrole and the 2-guanethidine benzimidazole in holes, and the gold film and the template are sequentially removed by a physical method and a chemical method to prepare a target product. The polypyrrole nanowire can be widely used for Fe<3+> trace detection in an organism environment.
Description
Technical field
The present invention relates to a kind of nano wire and preparation method and purposes, especially a kind of polypyrrole nano line and its production and use.
Background technology
Iron is one of most important metallic element, accounts for 95% of world's Metal Production industry.It is indispensable starting material in industry and the machinery production.In addition, iron also is that the human body metabolic processes is necessary, at human body oxygen absorption metabolism, drug metabolism, adenosine triphosphate production and DNA is played an important role in the process such as synthetic.The minimizing of human body iron level can cause anaemia; Yet the too much storage of iron will cause multiple disease in the body, as liver and heart disease, diabetes, some tumour etc.Liver is the main position that iron stores, and the excessive liver that also often involves of iron becomes the main target organ that iron is too much induced damage; Liver iron is excessive will to cause hepatic fibrosis even liver cirrhosis, and hepatoma.In addition, the excessive discussion with the heart disease relation of iron, also existing a lot of report; Generally believe, Tie Tong cross the generation of catalysis free radical, the lipid that promotes lipoprotein and protein portion peroxidation, form effect such as Ox LDL, participate in atherosclerotic formation.The enhancing of the peroxidatic reaction of lipid that iron is too much induced causes the unbalance of body oxidation and antioxidant system, and coup injury DNA brings out sudden change, and is relevant with the tumour of multiple organs such as liver, colon, rectum, lung, oesophagus, bladder.Therefore, particularly important to rapid detection and the improvement of iron level in food, the environment.
Macromolecular material because of generally have many metals and inorganic materials the advantage that can't replace obtained development rapidly, yet, at present widespread use also be the polymer substance that uses under the ordinary condition, be so-called commodity polymer, they have defectives such as physical strength and poor rigidity, thermotolerance be low.Therefore, people are in order to obtain the more novel high polymer material of high-performance and Geng Jia function, some trials and effort have been done, as a kind of " preparation method of electric polypyrrole nano line " who mentions among the disclosed Chinese invention patent specification sheets CN1262575C on July 5th, 2006.It is earlier in neutrality or acidic aqueous solution, adds quaternary ammonium cation tensio-active agent, pyrrole monomer successively, makes pyrrole monomer be dissolved in the water phase surfactant mixture fully; Again with the temperature regulation of reaction system after-20～30 ℃, add neutrality or the acidic aqueous solution of oxygenant, under-20～30 ℃ of conditions, reacted 2～48 hours, obtain the black insolubles and be the electric polypyrrole nano line.But, no matter be the electric polypyrrole nano line, or its preparation method, all exist weak point, at first, the electric polypyrrole nano line is a kind of macromolecular material with conductivity, and it only can be used for conduction, and can not especially can not be used for the ferric ion (Fe to the organism environment as his usefulness
3+) quick trace detection; Secondly, the preparation method can not make the polypyrrole nano line that ferric ion is carried out quick trace detection.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of polypyrrole nano line that can carry out quick trace detection to ferric ion for overcoming weak point of the prior art.
Another technical problem that the present invention will solve is for providing a kind of preparation method of above-mentioned polypyrrole nano line.
What the present invention will solve also has a technical problem for a kind of purposes of above-mentioned polypyrrole nano line is provided.
For solving technical problem of the present invention, the technical scheme that adopts is: polypyrrole nano line comprises polypyrrole, particularly,
Described polypyrrole is wire, and described wire polypyrrole is modified with 2-guanidine pyridine benzoglyoxaline (GBI) outward;
Described its outer linear diameter that is modified with the polypyrrole of 2-guanidine pyridine benzoglyoxaline is that 25～35nm, line length are 10～80 μ m.
For solving another technical problem of the present invention, another technical scheme that adopts is: the preparation method of above-mentioned polypyrrole nano line comprises that using the two-step anodization method to obtain bore dia is that 25～35nm, thickness of slab are that 10～80 μ m, hole density are 10
9～10
11/ cm
2The through hole alumina formwork, particularly completing steps is as follows:
Further improvement as the preparation method of polypyrrole nano line, the process that described use two-step anodization method obtains the through hole alumina formwork is, earlier aluminium flake being placed concentration is the sulphuric acid soln of 0.2～0.4mo1/L, be anodic oxidation 3～5h under 25～29V in volts DS, be placed on again in the mixed solution of chromic acid of the phosphoric acid of 4～8wt% and 1.6～2wt% and soak 5～7h, then, after it is placed the anodic oxidation of carrying out 9～10h under the same processing condition again, with the unoxidized aluminium of Cupric Chloride Solution or the tin tetrachloride solution removal back side, the phosphoric acid solution with 3～7wt% erodes the aluminum oxide barrier layer that is positioned at the bottom, hole more earlier; The concentration of the aqueous ethanolic solution in the described epolamine aqueous solution is 50vol% (volume percent); Described physical method is sand papering or mechanical curettage; The described concentration that erodes the phosphoric acid solution of through hole alumina formwork is 5wt%.
For solving the technical problem that also has of the present invention, the technical scheme that also has that adopts is: the purposes of above-mentioned polypyrrole nano line is,
It is the aqueous ethanolic solution of 50vol% that polypyrrole nano line is placed the water that is subjected to the ferric ion pollution or the concentration that polluted by ferric ion, use UV-light that it is shone earlier, re-use fluorescence spectrophotometer and measure the fluorescence emission spectral intensity of the 2-guanidine pyridine benzoglyoxaline in the polypyrrole nano line, obtain the content of ferric ion.
As the further improvement of the purposes of polypyrrole nano line, described ultraviolet light wavelength is 230～270nm.
Beneficial effect with respect to prior art is, one uses scanning electron microscope, transmission electron microscope and infrared spectrometer to characterize respectively to the target product that makes, by characterization result as can be known, target product is wire, and the linear target product is modified with 2-guanidine pyridine benzoglyoxaline outward by polypyrrole and constitutes; Wherein, its outer linear diameter that is modified with the polypyrrole of 2-guanidine pyridine benzoglyoxaline is that 25～35nm, line length are 10～80 μ m.Its two, to containing trace Fe
3+Target product use the steady-state life fluorescence spectrophotometer to come it is carried out the sign of fluorescent effect, by its result as can be known: the one, target product has excellent optical property, with wavelength be the excitation light source excites of 230～270nm, in water or aqueous ethanolic solution (volume ratio is 1: 1) time, it all has very strong photoluminescence band at 350～480nm or 300～480nm wave band respectively, thereby it is a kind of good embedded photoluminescent material.The 2nd, target product is along with including Fe
3+The increase of concentration, its fluorescence intensity at 350～480nm or 300～480nm wavelength place are respectively linear and strengthen or weaken, until Fe
3+Concentration is 1.4 * 10
-5Mol/L, the fluorescence intensity of this linear change has possessed as Fe in the water or in the aqueous ethanolic solution target product
3+The primary condition of fluorescent optical sensor.Particularly importantly, target product is that concentration in 1: 1 the aqueous ethanolic solution is low to moderate 2 * 10 to volume ratio
-6The Fe of mol/L
3+Still can detect effectively.The 3rd, the fluorescence intensity of target product is not subjected to the interference of other common metal ion impurity, namely can only identify Fe specifically
3+The 4th, target product is to Fe
3+Selectivity and sensitivity, far above selectivity and the sensitivity of GBI molecule among same solution of free state; This is because GBI molecule fixing on the polypyrrole nano line surface, both reduce the intermolecular electronics of GBI and energy and shifted the loss that energy is caused, avoided non-radiative processes such as molecular motion, collision to its dissipation of energy again, thereby increased its fluorescence quantum efficiency, strengthen its luminous power, thereby improved it effectively as Fe
3+The sensitivity of fluorescent sensing material.The 5th, target product is with respect to existing detection Fe
3+Method, have make simple and easy, highly sensitive, detect characteristics quick and with low cost; It has been realized Fe
3+Highly sensitive, the detection of highly selective.Target product detects trace Fe
3+Mechanism be, based on Fe
3+And form co-ordination complex between the GBI molecule, target product owing to exist proton to cause fluorescent quenching, makes that the fluorescence quantum efficiency of GBI is on the low side, Fe in water the time
3+Existence make GBI molecule and its formation co-ordination complex, weakened the fluorescent quenching that proton in the water causes GBI effectively, thereby target product fluorescence strengthens; Target product is in aqueous ethanolic solution the time, and it is not obvious that proton causes fluorescent quenching, GBI and Fe
3+After forming co-ordination complex, use the UV-irradiation target product, the GBI molecule of excited state will take place to Fe
3+The photic transfer transport of part, thereby fluorescent weakening.The target product that makes can be widely used among the sample detection in fields such as environment, food and medical science.Its three, preparation method's science, had effectively both been prepared the polypyrrole nano line that finishing has the GBI molecule, made the target product of preparing satisfy the counterweight metal cations Fe again
3+Carry out the requirement of quick trace detection, the advantage that preparation device simple, technology are simple, with low cost, be easy to suitability for industrialized production is also arranged.
Further embodiment as beneficial effect, one process that is to use the two-step anodization method to obtain the through hole alumina formwork is preferably, earlier aluminium flake being placed concentration is the sulphuric acid soln of 0.2～0.4mo l/L, be anodic oxidation 3～5h under 25～29V in volts DS, be placed on again in the mixed solution of chromic acid of the phosphoric acid of 4～8wt% and 1.6～2wt% and soak 5～7h, then, after it is placed the anodic oxidation of carrying out 9～10h under the same processing condition again, earlier with the unoxidized aluminium of Cupric Chloride Solution or the tin tetrachloride solution removal back side, phosphoric acid solution with 3～7wt% erodes the aluminum oxide barrier layer that is positioned at the bottom, hole again, for the nano wire for preparing suitable pattern and size is had laid a good foundation; The 2nd, the concentration of the aqueous ethanolic solution in the epolamine aqueous solution is preferably 50vol%, is beneficial to that galvanic deposit goes out polypyrrole nano line of fine quality in the hole of alumina formwork; The 3rd, physical method is preferably sand papering or mechanical curettage, not only simply but also convenient; The 4th, the concentration that erodes the phosphoric acid solution of through hole alumina formwork is preferably 5wt%, is easy to obtain quickly target product; The 5th, the ultraviolet light wavelength is preferably 230～270nm, has guaranteed that target product all has very strong photoluminescence band at 350～480nm or 300～480nm wave band.
Description of drawings
Below in conjunction with accompanying drawing optimal way of the present invention is described in further detail.
Fig. 1 uses one of result that scanning electron microscope (SEM) and transmission electron microscope (TEM) characterize respectively to the target product that makes.Wherein, Figure 1A is the SEM photo of target product, and Figure 1B is the TEM photo of target product; Can be seen pattern and the size of target product by these two photos.
Fig. 2 uses one of result that infrared spectra (FTIR) instrument characterizes respectively to middle product and target product.Curve 1 in the FTIR spectrogram is for intermediate product (PPyNWs)---unmodified has the spectral line of the polypyrrole nano line of GBI, and curve 2 is the spectral line of target product (GBI-PPyNWs).By FTI R spectrogram as can be known, 1545 in the curve 1
-1, 1311
-1, 1177cm
-1Absorption peak be the charateristic avsorption band of polypyrrole; And a new 3444cm has appearred in the curve 2
-1Absorption peak, it has confirmed thus that corresponding to GBI guanidine radicals absorption of vibrations the GBI molecule successfully has been modified at the surface of intermediate product.
Fig. 3 is that subtend contains the Fe that drips different concns in the different solutions of 34 μ g/ml target products respectively
3+Behind the solution, the result who uses the steady-state life fluorescence spectrophotometer to characterize.Wherein, the excitation wavelength of excitation light source is 250nm.Fig. 3 A is the Fe that drips different concns in the deionized water solution of target product
3+The fluorescence spectrum figure that obtains behind the solution, Fig. 3 B are the corresponding titration curve of Fig. 3 A; Fig. 3 C is for dripping the Fe of different concns in the ethanol deionized water mixing solutions (volume ratio is 1: 1) of target product
3+The fluorescence spectrum figure that obtains behind the solution, Fig. 3 D are the corresponding titration curve of Fig. 3 C.By Fig. 3 A, Fig. 3 B, Fig. 3 C and Fig. 3 D as can be known, for the deionized water solution of target product, its fluorescence intensity is along with the Fe that adds
3+The concentration of solution increases and strengthens, and for the ethanol deionized water mixing solutions of target product, its fluorescence intensity is along with the Fe that adds
3+The concentration of solution increases and weakens.
Fig. 4 be subtend contain drip the different metal ion salt solution of same concentrations respectively in the different solutions of 34 μ g/ml target products after, the result who uses the steady-state life fluorescence spectrophotometer to characterize.Wherein, the excitation wavelength of excitation light source is 250nm.Fig. 4 A is for dripping the fluorescence spectrum figure that obtains behind the different metal ion salt solution of same concentrations in the deionized water solution of target product, Fig. 4 B is for dripping the fluorescence spectrum figure that obtains behind the different metal ion salt solution of same concentrations in the ethanol deionized water mixing solutions (volume ratio is 1: 1) of target product.By Fig. 4 A and Fig. 4 B as can be known, no matter be deionized water or 1: 1 ethanol deionized water mixing solutions, drip the different metal ion salt solution of same concentrations, except Fe
3+Outward, its fluorescence intensity does not change substantially, and the existence of these ionizable metal salts can be to Fe
3+Detection impact, illustrated that target product is to Fe
3+Has extraordinary selectivity.
Embodiment
At first buy from market or make with ordinary method:
Bore dia is that 25～35nm, thickness of slab are that 10～80 μ m, hole density are 10
9～10
11/ cm
2The through hole alumina formwork, it obtains for using the two-step anodization method, the process of making is, earlier aluminium flake being placed concentration is the sulphuric acid soln of 0.2～0.4mol/L, be anodic oxidation 3～5h under 25～29V in volts DS, be placed on again in the mixed solution of chromic acid of the phosphoric acid of 4～8wt% and 1.6～2wt% and soak 5～7h, then, after it is placed the anodic oxidation of carrying out 9～10h under the same processing condition again, with the unoxidized aluminium of Cupric Chloride Solution or the tin tetrachloride solution removal back side, the phosphoric acid solution with 3～7wt% erodes the aluminum oxide barrier layer that is positioned at the bottom, hole more earlier;
2-guanidine pyridine benzoglyoxaline; Ethanol; The epolamine aqueous solution, the concentration of aqueous ethanolic solution wherein are 50vol%.
Then,
The concrete steps of preparation are:
The concrete steps of preparation are:
The concrete steps of preparation are:
The concrete steps of preparation are:
The concrete steps of preparation are:
The purposes of polypyrrole nano line is, it is the aqueous ethanolic solution of 50vol% that polypyrrole nano line is placed the water that is subjected to the ferric ion pollution or the concentration that polluted by ferric ion, use UV-light that it is shone earlier, wherein, the ultraviolet light wavelength is 230～270nm; Re-use fluorescence spectrophotometer and measure the fluorescence emission spectral intensity of the 2-guanidine pyridine benzoglyoxaline in the polypyrrole nano line, obtain as or be similar to the content of the ferric ion shown in the curve among Fig. 3 or Fig. 4.
Obviously, those skilled in the art can carry out various changes and modification to polypyrrole nano line of the present invention and its production and use and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (7)
1. a polypyrrole nano line comprises polypyrrole, it is characterized in that:
Described polypyrrole is wire, and described wire polypyrrole is modified with 2-guanidine pyridine benzoglyoxaline outward;
Described its outer linear diameter that is modified with the polypyrrole of 2-guanidine pyridine benzoglyoxaline is that 25～35nm, line length are 10～80 μ m.
2. the preparation method of the described polypyrrole nano line of claim 1 comprises that using the two-step anodization method to obtain bore dia is that 25～35nm, thickness of slab are that 10～80 μ m, hole density are 10
9～10
11/ cm
2The through hole alumina formwork, it is characterized in that completing steps is as follows:
Step 1, prior to a gold evaporation film of through hole alumina formwork, again the alumina formwork that simultaneously is covered with golden film being placed concentration is 10
-3～10
-5After soaking at least 2h in the ethanolic soln of the 2-guanidine pyridine benzoglyoxaline of mol/L, use ethanol to wash the 2-guanidine pyridine benzoglyoxaline on alumina formwork surface, obtain being covered with on its hole inwall the alumina formwork of 2-guanidine pyridine benzoglyoxaline;
Step 2, earlier one side being covered with the alumina formwork that is covered with 2-guanidine pyridine benzoglyoxaline on golden film, the hole inwall, to place concentration be the epolamine aqueous solution of 0.15～0.25mol/L, be that anode, graphite are negative electrode with it, be galvanic deposit 2～8h under 0.8～1.2V in volts DS, obtain one side and be covered with the alumina formwork that is equipped with polypyrrole and 2-guanidine pyridine benzoglyoxaline in golden film, the hole, after re-using physical method and removing the golden film that alumina formwork simultaneously is covered with, be placed on and erode alumina formwork in the phosphoric acid solution, make polypyrrole nano line.
3. the preparation method of polypyrrole nano line according to claim 2, it is characterized in that the process of using the two-step anodization method to obtain the through hole alumina formwork is, earlier aluminium flake being placed concentration is the sulphuric acid soln of 0.2～0.4mol/L, be anodic oxidation 3～5h under 25～29V in volts DS, be placed on again in the mixing solutions of chromic acid of the phosphoric acid of 4～8wt% and 1.6～2wt% and soak 5～7h, then, after it is placed the anodic oxidation of carrying out 9～10h under the same processing condition again, with the unoxidized aluminium of Cupric Chloride Solution or the tin tetrachloride solution removal back side, the phosphoric acid solution with 3～7wt% erodes the aluminum oxide barrier layer that is positioned at the bottom, hole more earlier.
4. the preparation method of polypyrrole nano line according to claim 2, the concentration that it is characterized in that the aqueous ethanolic solution in the epolamine aqueous solution is 50vol%.
5. the preparation method of polypyrrole nano line according to claim 2 is characterized in that physical method is sand papering or mechanical curettage.
6. the preparation method of polypyrrole nano line according to claim 2, the concentration that it is characterized in that eroding the phosphoric acid solution of through hole alumina formwork is 5wt%.
7. the purposes of the described polypyrrole nano line of claim 1 is characterized in that:
It is the aqueous ethanolic solution of 50vol% that polypyrrole nano line is placed the water that is subjected to the ferric ion pollution or the concentration that polluted by ferric ion, use UV-light that it is shone earlier, re-use fluorescence spectrophotometer and measure the fluorescence emission spectral intensity of the 2-guanidine pyridine benzoglyoxaline in the polypyrrole nano line, obtain the content of ferric ion; Wherein, the ultraviolet light wavelength is 230～270nm.
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| CN106340402B (en) * | 2016-10-28 | 2018-09-07 | 齐鲁工业大学 | A kind of polypyrrole film based flexible super capacitor and its preparation method and application |
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| CN1597732A (en) * | 2003-09-15 | 2005-03-23 | 北京大学 | Preparation method of electric conductive polypyrrole nanometer wire |
| CN101928972A (en) * | 2010-07-23 | 2010-12-29 | 北京航空航天大学 | Method for preparing nickel-polypyrrole double-layer nanowire array material |
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| CN1597732A (en) * | 2003-09-15 | 2005-03-23 | 北京大学 | Preparation method of electric conductive polypyrrole nanometer wire |
| CN101928972A (en) * | 2010-07-23 | 2010-12-29 | 北京航空航天大学 | Method for preparing nickel-polypyrrole double-layer nanowire array material |
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