CN106770576A - A kind of method that one-step method prepares polyelectrolyte compound film electrode - Google Patents
A kind of method that one-step method prepares polyelectrolyte compound film electrode Download PDFInfo
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- CN106770576A CN106770576A CN201710041694.7A CN201710041694A CN106770576A CN 106770576 A CN106770576 A CN 106770576A CN 201710041694 A CN201710041694 A CN 201710041694A CN 106770576 A CN106770576 A CN 106770576A
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Abstract
The present invention relates to a kind of preparation method of polyelectrolyte compound film electrode.With cellulose sodium sulfate (NaCS) as polyanion, PDDA (PDADMAC) is polycation to the method, and the two obtains compound polyelectrolyte by complexing（NaCS/PDADMAC）, and synchronously it is prepared for polyelectrolyte compound film electrode（NaCS/PDADMAC/GCE）.Step is as follows：PDADMAC solution is dropped in into GCE surfaces with " coated method ", then above-mentioned electrode surface is dropped in different proportion NaCS solution, while preparing compound polyelectrolyte, the membrane electrode of compound modification is also prepared for.The present invention is simple and easy to apply, and the compound of preparation can be dispersed in electrode surface film forming uniform ground, and compound film electrode has good chemical property, it is expected to for the electrochemical analysis and detection of micro substance.
Description
Technical field
Birdsed of the same feather flock together electrolyte complex film modified electrode the present invention relates to one, more particularly to by PDDA
(PDADMAC) with cellulose sodium sulfate (NaCS) in varing proportions drop coating on glass-carbon electrode (GCE) surface, the two pass through interface network
Reaction is closed compound polyelectrolyte is obtained and the preparation method of polyelectrolyte compound film electrode is obtained simultaneously.
Background technology
Chemically modified electrode is current very active research field in terms of electrochemistry, Electroanalytical Chemistry.Functional polyalkylene
Compound film is with its stronger chemistry, mechanically and electrically chemical stability assigns the more sensitive electrochemical response of electrode, has expanded electricity
The application category of pole, so receive much concern.In recent years, polymer assembling electrode development it is encouraging, its decorative material it is many
The utilizability of sample and film three-dimensional structure, is allowed to especially prominent in terms of functional film modified electrode prepares sensor,
The hypersensitivity and very high selectivity for hardly matching are shown, is had in life science, environmental science, the energy and field of medicaments
Huge application prospect.
As the PDDA (PDADMAC) of cationic polymer, because its aqueous solution is conductive,
And with charge density is high, good water solubility, it is cheap and easy to get, nontoxic the features such as, it is had in electrochemical sensor field very big
Application potential.Cellulose sodium sulfate/PDDA (NaCS/PDADMAC) is a kind of new poly- electrolysis
Matter composite membrane, with excellent mechanical strength, the transparency and the features such as small-bore, has been applied to bacterium and fungi has been fixed at present
The field such as change, microalgae immobilization, drug delivery and membranous system, but in electrochemical sensor field, there is not been reported.In view of NaCS
Each good electric conductivity, film forming with PDADMAC, we plan the two and are prepared into compound polyelectrolyte, and are allowed to film forming
Modified glassy carbon electrode, prepares new polyelectrolyte compound film electrode.
In sum, the present invention is determined polycation PDADMAC with polyanion NaCS by extremely simple coated method
Amount is deposited on glassy carbon electrode surface, and the two occurs rapidly Interfacial complexation reaction, the compound polyelectrolyte NaCS/ of generation
In the evenly laid out film forming of electrode surface, synchronous modified glassy carbon electrode is prepared into polyelectrolyte compound film electrode NaCS/ to PDADMAC
PDADMAC/GCE, and study tour its chemical property is carried out to the electrochemical behavior of the electrode.
The content of the invention
It is contemplated that developing new modified electrode, there is provided a kind of low cost, raw material are easy to get, simple to operate, excellent performance
The complex film modified electrode of polyelectrolyte and preparation method thereof.
To achieve the above object, the present invention uses following technical scheme.
1st, a kind of preparation method of polyelectrolyte membrane electrode, comprises the following steps.
（1）By glass-carbon electrode (GCE) with 0.3 μm, 0.05 μm of α-Al2O3Polishing is cleaned, respectively in ethanol, deionization
Ultrasound is cleaned in water, and room temperature is dried.
（2）A certain amount of PDDA (PDADMAC) solution is dropped in into glassy carbon electrode surface.
（3）A certain amount of cellulose sodium sulfate (NaCS) solution is dropped in into above-mentioned drop the electrode surface of PDADMAC solution, from
So dry, while generation compound polyelectrolyte, obtain polyelectrolyte compound film electrode (NaCS/PDADMAC/GCE).
2nd, above-mentioned steps（2）Described in PDADMAC solution mass concentration be 7 % (w/v).
3rd, above-mentioned steps（3）Described in NaCS solution mass concentration be 3.5 % (w/v).
Described in present method invention by " Interfacial complexation, coated film forming one-step method ", obtain compound polyelectrolyte and poly-
The preparation method of electrolyte complex film electrode, its gained composite membrane can uniform ground be scattered in electrode surface.By this simple
The complex film modified electrode of polyelectrolyte for preparing of one-step method, the investigation result to electrochemical behavior shows that it has good electrification
Learn performance.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of membrane electrode.
Fig. 2 is that PDADMAC and NaCS volume ratios are 1:The cyclic voltammogram of gained NaCS/PDADMAC/GCE when 1.
Fig. 3 is that PDADMAC and NaCS volume ratios are 2.5:The cyclic voltammogram of gained NaCS/PDADMAC/GCE when 1.
Fig. 4 is that PDADMAC and NaCS volume ratios are 4:The cyclic voltammogram of gained NaCS/PDADMAC/GCE when 1.
Fig. 5 is that PDADMAC and NaCS volume ratios are 5:The cyclic voltammogram of gained NaCS/PDADMAC/GCE when 1.
Specific embodiment
With reference to instantiation, the present invention is described further.
Example 1：By GCE with 0.3 μm, 0.05 μm of α-Al2O3Minute surface is polished to, then uses ethanol and second distillation successively
Water is cleaned by ultrasonic respectively, and room temperature is dried.Take 1 μ L PDADMAC solution and drop in glassy carbon electrode surface, then take 1 μ L NaCS solution
Drop thereon, is dried naturally, is reacted by Interfacial complexation and is obtained NaCS/PDADMAC compounds, and compound is uniform in electrode surface
Tiling film forming, while modified glassy carbon electrode obtains membrane electrode NaCS/PDADMAC/GCE.Morphology characterization is carried out to it using SEM,
It was found that the compound film electrode（Figure 1B）Compared to the membrane electrode that NaCS is individually modified（Figure 1A）Obvious flat smooth, illustrates the present invention
Made polyelectrolyte compound film electrode is more beneficial for the electron transmission of electrode surface.The composite membrane is investigated using cyclic voltammetry
The electrochemical behavior of electrode, as a result shows, present invention gained polyelectrolyte compound film electrode NaCS/PDADMAC/GCE, and it is 5
×10-3 mol·L-1 K3[Fe(CN)6] there is in solution good electrochemical response（Fig. 2）.
Example 2：By GCE with 0.3 μm, 0.05 μm of α-Al2O3Minute surface is polished to, then uses ethanol and second distillation successively
Water is cleaned by ultrasonic respectively, and room temperature is dried.Take 2.5 μ L PDADMAC solution and drop in glassy carbon electrode surface, then to take 1 μ L NaCS molten
Drop thereon, dries naturally, is reacted by Interfacial complexation and obtains NaCS/PDADMAC compounds, and compound is equal in electrode surface
Even tiling film forming, while modified glassy carbon electrode obtains membrane electrode NaCS/PDADMAC/GCE.This is investigated using cyclic voltammetry to answer
The electrochemical behavior of membrane electrode is closed, is as a result shown, present invention gained polyelectrolyte compound film electrode NaCS/PDADMAC/GCE, its
5 × 10-3 mol·L-1 K3[Fe(CN)6] there is in solution good electrochemical response（Fig. 3）.
Example 3：By GCE with 0.3 μm, 0.05 μm of α-Al2O3Minute surface is polished to, then uses ethanol and second distillation successively
Water is cleaned by ultrasonic respectively, and room temperature is dried.Take 4 μ L PDADMAC solution and drop in glassy carbon electrode surface, then take 1 μ L NaCS solution
Drop thereon, is dried naturally, is reacted by Interfacial complexation and is obtained NaCS/PDADMAC compounds, and compound is uniform in electrode surface
Tiling film forming, while modified glassy carbon electrode obtains membrane electrode NaCS/PDADMAC/GCE.This is investigated using cyclic voltammetry to be combined
The electrochemical behavior of membrane electrode, as a result shows, the present invention gained polyelectrolyte compound film electrode NaCS/PDADMAC/GCE, its
5×10-3 mol·L-1 K3[Fe(CN)6] there is in solution good electrochemical response（Fig. 4）.
Example 4：By GCE with 0.3 μm, 0.05 μm of α-Al2O3Minute surface is polished to, then uses ethanol and second distillation successively
Water is cleaned by ultrasonic respectively, and room temperature is dried.Take 5 μ L PDADMAC solution and drop in glassy carbon electrode surface, then take 1 μ L NaCS solution
Drop thereon, is dried naturally, is reacted by Interfacial complexation and is obtained NaCS/PDADMAC compounds, and compound is uniform in electrode surface
Tiling film forming, while modified glassy carbon electrode obtains membrane electrode NaCS/PDADMAC/GCE.This is investigated using cyclic voltammetry to be combined
The electrochemical behavior of membrane electrode, as a result shows, the present invention gained polyelectrolyte compound film electrode NaCS/PDADMAC/GCE, its
5×10-3 mol·L-1 K3[Fe(CN)6] there is in solution good electrochemical response（Fig. 5）.
Claims (9)
1. a kind of one-step method prepares the preparation method of polyelectrolyte compound film electrode NaCS/PDADMAC/GCE, it is characterised in that：
Glass-carbon electrode GCE polishings are cleaned, using the polycation and polyanion of different proportion, i.e. by poly dimethyl diene
Propyl ammonium chloride PDADMAC（Polycation）Solution drops in GCE surfaces, is then followed by that cellulose sodium sulfate NaCS is added dropwise（Poly- the moon
Ion）Solution, dries naturally, has obtained compound polyelectrolyte NaCS/PDADMAC, and synchronization gain polyelectrolyte composite membrane
Electrode NaCS/PDADMAC/GCE.
2. one-step method as claimed in claim 1, it is characterised in that obtain compound polyelectrolyte in electrode surface, it is in electricity
The evenly laid out film forming in pole surface, and synchronous modified electrode obtains polyelectrolyte compound film electrode.
3. polyelectrolyte composite membrane as claimed in claim 1, it is characterised in that PDADMAC and NaCS occurs in electrode surface
Interfacial complexation reacts, and gained compound polyelectrolyte is a kind of polyelectrolyte composite membrane.
4. PDADMAC solution as claimed in claim 1, its mass concentration is 7 % (w/v)；NaCS solution, its mass concentration is
3.5 %(w/v)。
5. as claimed in claim 1 using the polycation and polyanion of different proportion, it is characterised in that what is used is poly-
The volume ratio of cation and polyanion is VPDADMAC:VNaCS=1:1。
6. as claimed in claim 1 using the polycation and polyanion of different proportion, it is characterised in that what is used is poly-
The volume ratio of cation and polyanion is VPDADMAC:VNaCS=2.5:1。
7. as claimed in claim 1 using the polycation and polyanion of different proportion, it is characterised in that what is used is poly-
The volume ratio of cation and polyanion is VPDADMAC:VNaCS=4:1。
8. as claimed in claim 1 using the polycation and polyanion of different proportion, it is characterised in that what is used is poly-
The volume ratio of cation and polyanion is VPDADMAC:VNaCS=5:1。
9. the preparation method of the polyelectrolyte compound film electrode as described in any one in claim 1-8, it is characterised in that institute
The composite membrane for stating different proportion preparation can be dispersed in electrode surface with uniform ground, complex film modified using this polyelectrolyte
Electrode has good chemical property.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107983599A (en) * | 2017-11-09 | 2018-05-04 | 浙江大学 | A kind of compound polyelectrolyte coating and preparation method thereof |
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| CN103979650A (en) * | 2014-05-17 | 2014-08-13 | 北京化工大学 | Method for preparing electro-adsorption component by virtue of self-assembly technology |
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| CN107983599A (en) * | 2017-11-09 | 2018-05-04 | 浙江大学 | A kind of compound polyelectrolyte coating and preparation method thereof |
| CN107983599B (en) * | 2017-11-09 | 2020-10-13 | 浙江大学 | Polyelectrolyte composite coating and preparation method thereof |
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Application publication date: 20170531 |