CN109607690B - Preparation method of three-dimensional porous graphene hydrogel antimony-doped tin oxide electrode - Google Patents
Preparation method of three-dimensional porous graphene hydrogel antimony-doped tin oxide electrode Download PDFInfo
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- CN109607690B CN109607690B CN201811380265.3A CN201811380265A CN109607690B CN 109607690 B CN109607690 B CN 109607690B CN 201811380265 A CN201811380265 A CN 201811380265A CN 109607690 B CN109607690 B CN 109607690B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C02F1/46104—Devices therefor; Their operating or servicing
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- C02F2001/46138—Electrodes comprising a substrate and a coating
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Abstract
Three-dimensionalThe preparation method of the porous graphene hydrogel antimony-doped tin oxide electrode comprises the steps of adding graphene into deionized water, performing ultrasonic treatment, and adding ethanol and deionized water into the solution to prepare a graphene oxide precursor solution A; adding Pluronic F127 into ethanol and keeping the temperature to obtain a clear solution; adding deionized water and SnCl into the clear solution2·2H2O and SbCl3Uniformly stirring to obtain a solution B; coating 2-7 mL of the solution B on an electrode, and drying the coated electrode; then coating 2-7 mL of the solution A on the precoated electrode, and drying and calcining the coated electrode; alternately coating the solution A and the solution B; in N2Calcination under an atmosphere to obtain aged LBL crystals. The electrochemical active area is increased by preparing the three-dimensional porous graphene hydrogel framework, so that the electrode has high porosity, and meanwhile, the tin-antimony doping technology is adopted, so that the stability of the electrode is improved, the degradation rate of toxic and non-degradable organic matters of the electrode is further improved, and the electrode has a good application prospect in the water treatment direction.
Description
Technical Field
The invention relates to the technical field of electrocatalytic oxidation, and particularly relates to a preparation method of a three-dimensional porous graphene hydrogel antimony-doped tin oxide electrode.
Background
The electrolytic oxidation technology has the advantages of simple operation, mild reaction conditions, no need of a plurality of chemicals for treating wastewater, simple post-treatment and the like, shows high-efficiency degradation capability in the aspect of treating the waste water which is difficult to biodegrade, and gradually becomes a research hotspot in the field of water pollution control. Graphene is applied to an electrocatalytic electrode material due to its excellent electrochemical properties. The graphene has extremely low resistivity, extremely high electron transfer speed and stable performance, and the three-dimensional porous structure is prepared by the graphene, so that the electrochemical active area is increased. The Sb-SnO2 has the characteristics of high oxygen evolution potential and high current efficiency, and is a class of electrode materials with good catalytic activity and high stability. A Layer By Layer (LBL) method is adopted, and different kinds of materials are formed into the film with controllable structure by a simple, cheap and rapid method. The prepared electrode has high porosity, excellent conductivity, improved hydrophobicity, improved electrolysis efficiency and good application prospect.
In actual use, the electrode still has short service life, and because the electrode and the material have weak bonding force, the coating is easy to inactivate in the use process, so that the degradation rate is reduced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a three-dimensional porous graphene hydrogel antimony-doped tin oxide electrode, the method comprises the steps of preparing a three-dimensional porous hydrogel framework by using graphene, preparing aged LBL (LBL) membrane crystals in a layer-by-layer coating mode, increasing the electrochemical active area by preparing the three-dimensional porous graphene hydrogel framework, enabling the electrode to have higher porosity, and simultaneously increasing the stability of the electrode and further improving the degradation rate of toxic and non-degradable organic matters of the electrode by using a tin-antimony doping technology.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a three-dimensional porous graphene hydrogel antimony-doped tin oxide electrode comprises the following steps;
a. adding 0.005-0.03 g of graphene into 2-7 mL of deionized water, performing ultrasonic treatment for 24 hours, and then adding 10-40 mL of ethanol and 2-7 mL of deionized water into the solution to prepare a graphene oxide precursor solution A;
b. adding 0.5-2.5 g of pluronic F127 into 10-40 mL of ethanol, and keeping the mixture at 40-60 ℃ for 10-20 min to obtain a clear solution; adding 2-7 mL of deionized water and 2-4 g of SnCl into the clear solution2·2H2O and 0.005 to 0.03g of SbCl3Uniformly stirring for 6-8 hours to obtain a solution B;
c. coating 0.5-2.0 mL of the solution B on an electrode, and drying the coated electrode; then coating 0.5-2.0 mL of the solution A on the precoated electrode, and drying and calcining the coated electrode;
d. alternately coating the solution A and the solution B, and repeating the step c for 8-14 times; finally in N2Calcining for 3 hours at 300-500 ℃ in the atmosphere to obtain the three-dimensional porous graphene hydrogel antimony doped tin oxide electrode.
Preferably, in the steps a and b, the sol is coated on the surface of the electrode carrier by spin coating, dip drawing or brush coating.
Preferably, in step c, the electrode carrier is a titanium electrode.
Preferably, in step c, the electrode carrier is ground, acid-treated and washed before the surface of the electrode carrier is coated with the solution a and the solution B.
Preferably, in step c, the electrode coated with the B solution is placed in N2Drying for 10-20 min at 300-500 ℃ in the atmosphere; drying the electrode coated with the solution A at 100-120 ℃ for 30-40 min, and then placing the electrode on N2Calcining for 10-20 min at 300-500 ℃ in the atmosphere.
The invention has the beneficial effects that:
(1) the stability of the SnO2 electrode is enhanced through Sb doping; (2) the electrochemical active area is increased by preparing the three-dimensional porous graphene hydrogel framework, and meanwhile, the electrode has higher porosity; (3) the electrode has good hydrophobicity, effectively reduces water adsorption on the surface of the anode, and increases reaction efficiency.
Drawings
FIG. 1a shows a porous 3D-Ti/Sb-SnO according to the invention2SEM micrograph of Gr at 200 nm.
FIG. 1b shows a porous 3D-Ti/Sb-SnO according to the invention2SEM micrograph of Gr at 100 nm.
FIG. 1c shows a porous 3D-Ti/Sb-SnO according to the invention2SEM micrograph of Gr at 20 nm.
FIG. 2 is a porous 3D-Ti/Sb-SnO2-photograph of the contact angle of Gr.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1
a. Adding 0.005g of graphene into 2mL of deionized water, carrying out ultrasonic treatment for 24 hours, and then adding 10mL of ethanol and 2mL of deionized water into the solution to prepare a graphene oxide precursor solution A;
b. 0.5g of pluronic F127 was added to 10mL of ethanol and held at 40 ℃ for 10min to give a clear solution; to the clear solution was added 2mL of deionized water, 2g of SnCl2·2H2O and 0.005g SbCl3Uniformly stirring for 6 hours to obtain a solution B;
c. a commercially available titanium electrode is used as a carrier, and grinding, acid treatment and washing are needed before use;
d. 0.5mL of the B solution was coated on an electrode, and the coated electrode was placed on N2Drying at 300 deg.C for 10 min; then 0.5mL of solution A was coated on the pre-coated electrode and dried at 100 ℃ for 30min, after which the electrode was dried on N2Calcining at 300 deg.C for 10 min;
e. alternately coating the solution A and the solution B, and repeating the step c 8 times; finally in N2Calcination was carried out at 300 ℃ for 3 hours under an atmosphere to obtain aged LBL crystals.
Example 2
a. Adding 0.01g of graphene into 4mL of deionized water, carrying out ultrasonic treatment for 24 hours, and then adding 20mL of ethanol and 4mL of deionized water into the solution to prepare a graphene oxide precursor solution A;
b. 1.0g of pluronic F127 was added to 20mL of ethanol and held at 45 ℃ for 12min to give a clear solution; to the clear solution was added 4mL of deionized water, 2.7g of SnCl2·2H2O and 0.014g SbCl3Uniformly stirring for 6 hours to obtain a solution B;
c. a commercially available titanium electrode is used as a carrier, and grinding, acid treatment and washing are needed before use;
d. 0.8mL of the B solution was coated on the electrode, and the coated electrode was placed on N2Drying at 350 deg.C for 12 min; then 0.8mL of solution A was coated on the pre-coated electrode and dried at 105 ℃ for 33min, after which the electrode was dried on N2Calcining at 350 deg.C for 12 min;
e. alternately coating the solution A and the solution B, and repeating the step c 9 times; finally in N2Calcination was carried out at 350 ℃ for 3 hours under an atmosphere to obtain aged LBL crystals.
Example 3
a. Adding 0.02g of graphene into 5mL of deionized water, carrying out ultrasonic treatment for 24 hours, and then adding 30mL of ethanol and 4mL of deionized water into the solution to prepare a graphene oxide precursor solution A;
b. 1.4g of pluronic F127 was added to 30mL of ethanol and held at 50 ℃ for 15min to give a clear solution; to the clear solution was added 5mL of deionized water, 3.22g of SnCl2·2H2O and0.02g SbCl3uniformly stirring for 7 hours to obtain a solution B;
c. a commercially available titanium electrode is used as a carrier, and grinding, acid treatment and washing are needed before use;
d. 1.0mL of the B solution was coated on an electrode, and the coated electrode was placed on N2Drying at 400 deg.C for 15 min; then 1.0mL of solution A was coated on the pre-coated electrode and dried at 105 ℃ for 35min, after which the electrode was dried on N2Calcining at 400 deg.C for 15 min;
e. alternately coating the solution A and the solution B, and repeating the step c 10 times; finally in N2Calcination was carried out at 400 ℃ for 3 hours under an atmosphere to obtain aged LBL crystals.
Example 4
a. Adding 0.03g of graphene into 7mL of deionized water, carrying out ultrasonic treatment for 24 hours, and then adding 40mL of ethanol and 7mL of deionized water into the solution to prepare a graphene oxide precursor solution A;
b. 2.5g of pluronic F127 was added to 40mL of ethanol and held at 55 ℃ for 20min to give a clear solution; to the clear solution was added 7mL of deionized water, 3.5g of SnCl2·2H2O and 0.03g of SbCl3Uniformly stirring for 8 hours to obtain a solution B;
c. a commercially available titanium electrode is used as a carrier, and grinding, acid treatment and washing are needed before use;
d. 2.0mL of the B solution was coated on an electrode, and the coated electrode was placed on N2Drying at 500 deg.C for 20 min; then 2.0mL of solution A was coated on the pre-coated electrode and dried at 110 deg.C for 40min, after which the electrode was dried on N2Calcining at 500 deg.C for 20 min;
e. alternately coating the solution A and the solution B, and repeating the step c 14 times; finally in N2Calcination was carried out at 500 ℃ for 3 hours under an atmosphere to obtain aged LBL crystals.
Example 5
a. Loading any three-dimensional porous graphene hydrogel antimony doped tin oxide electrode prepared in the embodiment into an electrocatalytic reaction device, and carrying out electrocatalytic treatment RhB experimental study;
b. using simulated wastewater with RhB concentration of 100mg/L as target treatment liquid;
c. continuously sampling at the water outlet, and continuously monitoring the chromaticity and TOC of the discharged water;
d. the RhB concentration of the raw water is 100mg/L, the decolorization rate of the discharged water reaches 99% after 30min of treatment, and the removal rate of TOC after 4 hours of treatment is 87.5%.
The invention provides an antimony-doped tin oxide electrode of three-dimensional porous graphene hydrogel, which is prepared by mixing SnCl2·5H2O、SbCl3And graphene as raw materials, and is prepared by a sol-gel method. The electrode is mainly characterized in that: (1) the stability of the SnO2 electrode is enhanced through Sb doping; (2) the electrochemical active area is increased by preparing the three-dimensional porous graphene hydrogel framework, and meanwhile, the electrode has higher porosity; (3) the electrode has good hydrophobicity, effectively reduces water adsorption on the surface of the anode, and increases reaction efficiency.
The three-dimensional porous graphene hydrogel antimony doped tin oxide provided by the invention is used for electrochemically degrading toxic and non-degradable organic matters. Wherein, the coating-drying-calcining process must be repeated for a plurality of times to obtain the three-dimensional porous graphene hydrogel antimony doped tin oxide electrode with a certain thickness.
The electrode carrier used in the embodiment of the invention is a commercially available titanium electrode, and the three-dimensional porous graphene hydrogel antimony doped tin oxide electrode is obtained by the methods of spin coating, dipping, pulling and brushing, so that the following conclusion is deduced: the technical effects of the present invention can also be achieved when other conductive carriers are employed.
As can be seen from fig. 1a, 1b and 1c, the nano-sized pores are arranged on the whole surface of the substrate, and the high-temperature rapid evaporation of ethanol helps to maintain the pores and provide the adhesion to construct the graphene hydrogel structure, so that the surface area is increased through the pores, and the hydrophobicity is also increased. Fig. 2 shows that the hydrophilicity and hydrophobicity of the electrode are measured by measuring a video contact angle, the contact angle of the electrode is 109 degrees, the hydrophobicity of the electrode is good, and the water adsorption on the surface of the anode can be effectively reduced, so that the reaction is promoted.
Claims (5)
1. A preparation method of a three-dimensional porous graphene hydrogel antimony-doped tin oxide electrode is characterized by comprising the following steps;
a. adding 0.005-0.03 g of graphene into 2-7 mL of deionized water, performing ultrasonic treatment for 24 hours, and then adding 10-40 mL of ethanol and 2-7 mL of deionized water into the solution to prepare a graphene oxide precursor solution A;
b. adding 0.5-2.5 g of pluronic F127 into 10-40 mL of ethanol, and keeping the mixture at 40-60 ℃ for 10-20 min to obtain a clear solution; adding 2-7 mL of deionized water and 2-4 g of SnCl into the clear solution2·2H2O and 0.005 to 0.03g of SbCl3Uniformly stirring for 6-8 hours to obtain a solution B;
c. coating 0.5-2.0 mL of the solution B on an electrode, and drying the coated electrode; then coating 0.5-2.0 mL of the solution A on the precoated electrode, and drying and calcining the coated electrode;
d. alternately coating the solution A and the solution B, and repeating the step c for 8-14 times; finally in N2Calcining for 3 hours at 300-500 ℃ in the atmosphere to obtain aged LBL crystals, namely the three-dimensional porous graphene hydrogel antimony doped tin oxide electrode.
2. The preparation method of the three-dimensional porous graphene hydrogel antimony doped tin oxide electrode as claimed in claim 1, wherein in steps c and d, the sol is applied on the surface of the electrode support by spin coating, dip-coating or brush coating.
3. The method for preparing the three-dimensional porous graphene hydrogel antimony doped tin oxide electrode according to claim 1, wherein in step c, the electrode carrier is a titanium electrode.
4. The method for preparing the three-dimensional porous graphene hydrogel antimony doped tin oxide electrode as claimed in claim 1, wherein in step c, the electrode carrier is polished, acid treated and washed before the surface of the electrode carrier is coated with the solution A and the solution B.
5. According to claim1, the preparation method of the three-dimensional porous graphene hydrogel antimony doped tin oxide electrode is characterized in that in the step c, the electrode coated with the solution B is placed in N2Drying for 10-20 min at 300-500 ℃ in the atmosphere; drying the electrode coated with the solution A at 100-120 ℃ for 30-40 min, and then placing the electrode on N2Calcining for 10-20 min at 300-500 ℃ in the atmosphere.
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