CN109205738B - Tin antimony-carbon aerogel composite adsorptive electrode and preparation method thereof - Google Patents
Tin antimony-carbon aerogel composite adsorptive electrode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a tin antimony-carbon aerogel composite adsorptive electrode and a preparation method thereof. The composite electrode comprises a nano-porous titanium matrix, a tin-antimony intermediate layer and a tin-antimony-carbon aerogel composite active surface layer. The method adopts a brush coating method, wherein tin-antimony solution containing carbon aerogel is brushed on a nano porous titanium substrate electrode plate of an electrodeposited tin-antimony middle layer, and the tin-antimony-carbon aerogel composite adsorption electrode is prepared by drying and sintering. Due to the huge specific surface area of the carbon aerogel and the introduction of the antimony/tin dioxide composite material, the catalytic activity of the electrode is greatly improved, the electrode has an electrocatalysis-adsorption synergistic effect, the service life of the electrode is obviously prolonged, and the electrode has great application value in the field of electrochemical catalysis.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis electrode preparation, and particularly relates to a tin-antimony-carbon aerogel composite adsorptive electrode and a preparation method thereof.
Background
Electrochemical oxidation has been widely used in the treatment of high concentration wastewater as a treatment technique with promising application prospects. Among them, electrodes in which oxides such as Sb, Sn, and the like are supported on titanium as a base are widely used. Particularly, after self-extraction, the tin oxide/antimony composite electrode has been greatly improved, has low manufacturing cost compared with noble metals, is an anode material with great potential, can effectively improve the specific surface area of the electrode, improves the electrochemical performance of the electrode, and is a hotspot of future electrode preparation research.
The existing preparation method of the tin-antimony composite electrode mainly comprises a brush coating method and an electrodeposition method, but the methods have the defects of small specific surface and SnO2Low load, etc. (Wang Q, Jin T, Hu Z X, Zhou L, Zhou M H. TiO)2-NTs/SnO2-Sb anode for efficient electrocatalytic degradation of organic pollutants:Effect of TiO2-NTs architecture[J].Separation and Purification Technology,2013,102:180-186)。
Disclosure of Invention
The invention aims to provide a tin antimony-carbon aerogel composite adsorption electrode with electrochemical oxidation and good adsorption performance and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows:
the tin-antimony-carbon aerogel composite adsorptive electrode comprises a nano porous titanium matrix, a tin-antimony intermediate layer and a tin-antimony-carbon aerogel composite active surface layer.
The pore diameter of the nano-porous titanium substrate is 20-100 nm.
The specific surface area of the tin antimony-carbon aerogel composite active surface layer is 100-200 m2·g-1。
The preparation method of the tin antimony-carbon aerogel composite adsorptive electrode comprises the following specific steps:
and brushing tin-antimony solution containing carbon aerogel on the nano porous titanium matrix electrode plate of the electrodeposited tin-antimony middle layer by adopting a brush-coating method, drying, sintering at the high temperature of 450 +/-10 ℃, repeatedly brushing, drying and sintering at the high temperature for more than three times to obtain the tin-antimony-carbon aerogel composite adsorption electrode.
The nano-porous titanium matrix is prepared by the conventional method and can be prepared by the following steps: and (2) carrying out anodic oxidation in aqueous hydrogen fluoride by taking the titanium substrate as an anode and the stainless steel plate as a cathode, washing the oxidized titanium substrate with water, drying, and sintering at 500 +/-10 ℃ to obtain the nano porous titanium substrate.
The nano-porous titanium matrix electrode plate for electrodepositing the tin-antimony interlayer is prepared by the conventional method and can be prepared by the following steps: and (3) taking the nano porous titanium substrate as a cathode and a stainless steel plate as an anode, sequentially carrying out constant-current electrodeposition in the electrodeposition solution of antimony trichloride and the electrodeposition solution of tin tetrachloride, and sintering the anode at the temperature of 450 +/-10 ℃ after reaction to obtain the nano porous titanium substrate electrode plate with the electrodeposited tin-antimony intermediate layer.
Preferably, the tin-antimony solution of the carbon-containing aerogel is an ethanol solution containing tin tetrachloride, antimony trichloride, hydrochloric acid and carbon aerogel, wherein the molar ratio of the tin tetrachloride to the antimony trichloride to the HCl is 10:1:1, and the mass concentration of the carbon aerogel is 0.1-0.5%.
Preferably, the temperature rise speed of the high-temperature sintering is 3-5 ℃/min, and the sintering time is 3-4 h.
Compared with the prior art, the invention has the following advantages:
(1) the tin-antimony-carbon aerogel composite adsorptive electrode greatly increases the specific surface area of the electrode due to the addition of the carbon aerogel, and SnO2The loading capacity is increased, and the carbon aerogel has the function of adsorbing pollutants, so that the electrode has the electrocatalysis-adsorption synergistic effect, and the capacity of electrolyzing and degrading the pollutants is improved;
(2) because the tin antimony doped in the carbon aerogel and the tin antimony intermediate layer form a eutectic body, the service life of the electrode is obviously prolonged, and the electrode can be applied to electrocatalytic oxidation of refractory organic pollutants.
Drawings
Fig. 1(a, b) is a femsem image of the nanoporous titanium matrix, fig. 1(c) is a femsem image of the nanoporous titanium matrix containing the tin-antimony intermediate layer, and fig. 1(d, e, f) is a FESEM image of the tin-antimony-carbon aerogel composite adsorptive electrode in which the carbon aerogel content is 0.1% and 0.5%, respectively.
FIG. 2 is an XRD pattern of a tin-antimony composite electrode and a carbon aerogel composite adsorptive electrode having a content of 0.1%, 0.5% and 1% tin-antimony-carbon aerogel.
FIG. 3 is a plot of cyclic voltammograms for the tin antimony composite electrode and carbon aerogel content of 0.1%, 0.5% and 1% tin antimony-carbon aerogel composite adsorbent electrode of example 1.
FIG. 4 is a graph showing the removal rates of degraded catechol with reaction time for the tin-antimony composite electrode and the carbon aerogel content of 0.1%, for the 0.5% and for the 1% tin-antimony-carbon aerogel composite adsorbent electrode in example 1.
Fig. 5 is an SEM image of the composite electrode prepared in comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
Reference is made to the preparation of nanoporous titanium matrices [ Chen Y, Hong L, Xue H, et al preparation and characterization of TiO 2-NTs/SnO 2Sb electrolytes by electrodeposition [ J]Journal of electroanalytical Chemistry 2010,648(2):119-127. The method comprises the following specific steps: sequentially polishing the surface of the titanium plate by using sand paper with the roughness of 500 meshes, 1000 meshes and 1500 meshes until the surface is flat and smooth; ultrasonic cleaning with deionized water and acetone for 20min respectively to remove oil stain on the surface; then properly heating in 18% hydrochloric acid solution for 20min to remove a surface oxide layer; finally, placing the mixture in deionized water for standby. The treated titanium substrate is used as an anode, a stainless steel plate is used as a cathode, and the concentration is 0.075 mol.L-1Hydrofluoric acid, 0.1 mol. L-1Potassium fluoride and 1 mol. L-1Anodizing with sulfuric acid solution at constant voltage of 20V in 2cm interval in the electrolyte in a plate immersed in the electrolyte, magnetic stirring, washing with distilled water, stoving at 80 +/-5 deg.c and 1 deg.c/min in a muffle furnace-1The temperature is raised to 500 ℃, the temperature is kept for 3 hours, and the nano porous titanium matrix is obtained after natural cooling to the room temperature.
Preparation of tin antimony interlayers reference [ Yu L, Chen Y, Han W, et al]RscAdvances,2016,6(24): 19848-. The method comprises the following specific steps: takes a nano-porous titanium matrix as a cathodeThe stainless steel plate is used as an anode, and the concentration is 0.01 mol.L-1Antimony trichloride, 0.01 mol. L-1Performing constant current electrodeposition in citric acid aqueous solution for 1min at 0.2 mol. L-1Tin tetrachloride, 0.01 mol. L-1Performing constant current electrodeposition in sulfuric acid water solution for 60min at current of 5mA cm-2After the reaction, the anode is sintered at high temperature in a muffle furnace, and the heating rate of the muffle furnace is 1 ℃ min-1And heating to 450 ℃ to obtain a tin-antimony intermediate layer, thus obtaining the nano porous titanium matrix electrode plate with the electrodeposited tin-antimony intermediate layer.
Example 1
Will contain 1 mol. L-1Tin tetrachloride, 0.1 mol. L-1Antimony trichloride, 0.1 mol. L-1And (3) brushing an ethanol solution of hydrochloric acid and 1% carbon aerogel on a nano porous titanium matrix electrode plate for electrodepositing the tin-antimony middle layer, brushing for many times, drying, sintering at high temperature, repeatedly brushing, drying and sintering at high temperature for more than three times, wherein the high-temperature sintering temperature is 450 +/-10 ℃, and the temperature rise speed is 5 ℃/min, so that the tin-antimony-carbon aerogel composite adsorptive electrode is obtained. The composite electrodes with the carbon aerogel content of 0, 0.1%, 0.5% and 1% are prepared by the same method, and when the carbon aerogel content is 0, the electrode is a tin-antimony composite electrode.
FIG. 1(a, b) is a FESEM image of a nanoporous titanium matrix in which nanopores are aligned and have uniform pore diameters; FIG. 1(c) is a FESEM of a nanoporous titanium matrix containing a tin-antimony interlayer, in which the tin-antimony interlayer is structurally dense; fig. 1(d, e, f) are FESEM images of the sn-sb-c aerogel composite adsorptive electrode having a c aerogel content of 0.1%, 0.5%, and 1%, respectively, in which the sn-sb-c aerogel active layer is tightly bonded to the sn-sb intermediate layer, and the sn-sb-c aerogel active layer structure is looser as the c aerogel content increases.
FIG. 2 is an XRD pattern of a tin-antimony composite electrode and a carbon aerogel composite adsorptive electrode having a content of 0.1%, 0.5% and 1% tin-antimony-carbon aerogel. SnO can be analyzed in the figure2The crystal structure of (A) is a tetragonal crystal form, only a small amount of titanium peaks are detected, which shows that SnO2The coating preferably covers the titanium substrate. The carbon aerogel 002 peak positions were coincident with tin 110, so no detection was made in the composite electrodeTo the peak of carbon aerogel.
FIG. 3 is a plot of cyclic voltammograms for the tin antimony composite electrode and carbon aerogel content of 0.1%, 0.5% and 1% tin antimony-carbon aerogel composite adsorbent electrode of example 1. The voltammetric charge of the electrode increases with increasing carbon aerogel content in the electrode.
Example 2
The performance of the tin-antimony composite electrode and the tin-antimony-carbon aerogel composite adsorptive electrode is measured, and the specific measurement method comprises the following steps:
500mL of catechol simulated wastewater with the concentration of 100mg/L are prepared, 7g/L of anhydrous Na2SO4 is added to serve as electrolyte, a tin-antimony composite electrode and a carbon aerogel content of 0.1 percent, a tin-antimony-carbon aerogel composite adsorptive electrode of 0.5 percent and 1 percent are respectively used as anodes, stainless steel is used as a cathode, and the current density is controlled to be 5mA/cm under the action of a magnetic stirrer2The four electrodes were compared for catechol degradation performance.
In the standing mode, the trend of the tin-antimony composite electrode and the carbon aerogel content of 0.1%, 0.5% and 1% of the tin-antimony-carbon aerogel composite adsorption electrode prepared in example 1 with respect to the catechol removal efficiency with time is shown in fig. 4. It can be seen from the figure that, under the action of a magnetic stirrer, after 90min of electrolysis, the contents of the tin-antimony composite electrode and the carbon aerogel are 0.1%, and the removal efficiencies of the 0.5% tin-antimony-carbon aerogel composite adsorptive electrode to catechol are 66.63%, 82.3%, 88.9% and 98.99%, respectively, which indicates that the tin-antimony-carbon aerogel composite adsorptive electrode has higher electrochemical oxidation performance and the effect is in a proportional trend along with the increase of the content of the carbon aerogel.
Comparative example 1
This comparative example is essentially the same as example 1, except that the sintering environment is under nitrogen and the sintering temperature is 900 ℃. The SEM image of the prepared composite electrode is shown in fig. 5, and it can be seen from the image that the surface of the electrode is observed to be obviously "cracked" with many "ravines", the whole coating is divided into many small whole bodies, the coating is not firmly bonded to the substrate and is easily peeled off, the coating liquid and the substrate cannot be tightly bonded due to the brush coating method, and voids are left, which indicates that the bonding force under the protection of nitrogen is inferior to that under the condition of oxygen.
Claims (10)
1. The tin-antimony-carbon aerogel composite adsorptive electrode is characterized by comprising a nano porous titanium matrix, a tin-antimony intermediate layer and a tin-antimony-carbon aerogel composite active surface layer.
2. The composite adsorbent electrode of claim 1, wherein the nanoporous titanium matrix has a pore size of 20-100 nm.
3. The composite adsorptive electrode of claim 1, wherein said tin antimony-carbon aerogel composite active surface layer has a specific surface area of 100 to 200m2·g-1。
4. The method for preparing the composite adsorptive electrode according to any one of claims 1 to 3, comprising the following steps:
and brushing tin-antimony solution containing carbon aerogel on the nano porous titanium matrix electrode plate of the electrodeposited tin-antimony middle layer by adopting a brush-coating method, drying, sintering at the high temperature of 450 +/-10 ℃, repeatedly brushing, drying and sintering at the high temperature for more than three times to obtain the tin-antimony-carbon aerogel composite adsorption electrode.
5. The method according to claim 4, wherein the nanoporous titanium matrix is prepared by the following steps: and (2) carrying out anodic oxidation in aqueous hydrogen fluoride by taking the titanium substrate as an anode and the stainless steel plate as a cathode, washing the oxidized titanium substrate with water, drying, and sintering at 500 +/-10 ℃ to obtain the nano porous titanium substrate.
6. The preparation method of claim 4, wherein the preparation method of the nano-porous titanium substrate electrode plate for electrodepositing the tin-antimony intermediate layer comprises the following steps: and (3) taking the nano porous titanium substrate as a cathode and a stainless steel plate as an anode, sequentially carrying out constant-current electrodeposition in the electrodeposition solution of antimony trichloride and the electrodeposition solution of tin tetrachloride, and sintering the anode at the temperature of 450 +/-10 ℃ after reaction to obtain the nano porous titanium substrate electrode plate with the electrodeposited tin-antimony intermediate layer.
7. The method according to claim 4, wherein the tin-antimony solution of the carbon-containing aerogel is an ethanol solution containing tin tetrachloride, antimony trichloride, hydrochloric acid and carbon aerogel.
8. The preparation method according to claim 7, wherein the molar ratio of stannic chloride, antimony trichloride and HCl in the tin-antimony solution of the carbon-containing aerogel is 10:1: 1.
9. The preparation method of claim 7, wherein the mass concentration of the carbon aerogel in the tin-antimony solution of the carbon aerogel is 0.1-0.5%.
10. The preparation method according to claim 4, wherein in the tin-antimony solution of the carbon-containing aerogel, the temperature rise speed of the high-temperature sintering is 3-5 ℃/min, and the sintering time is 3-4 h.
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| CN105110425A (en) * | 2015-09-01 | 2015-12-02 | 上海应用技术学院 | Preparation method of carbon-nanotube-modified three-dimensional porous-titanium-base lead dioxide electrode |
| CN105712428A (en) * | 2016-02-01 | 2016-06-29 | 南京理工大学 | Antimony-doped tin oxide-carbon nanotube compounded adsorptive electrode and preparation method thereof |
| CN206244480U (en) * | 2016-10-27 | 2017-06-13 | 天津市大陆制氢设备有限公司 | A kind of tin dioxide coating on titanium antimony adsorbing nanowires electrode |
| CN107302102A (en) * | 2017-05-19 | 2017-10-27 | 南京理工大学 | A kind of 3-D ordered multiporous lead dioxide membrane electrode and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105110425A (en) * | 2015-09-01 | 2015-12-02 | 上海应用技术学院 | Preparation method of carbon-nanotube-modified three-dimensional porous-titanium-base lead dioxide electrode |
| CN105712428A (en) * | 2016-02-01 | 2016-06-29 | 南京理工大学 | Antimony-doped tin oxide-carbon nanotube compounded adsorptive electrode and preparation method thereof |
| CN206244480U (en) * | 2016-10-27 | 2017-06-13 | 天津市大陆制氢设备有限公司 | A kind of tin dioxide coating on titanium antimony adsorbing nanowires electrode |
| CN107302102A (en) * | 2017-05-19 | 2017-10-27 | 南京理工大学 | A kind of 3-D ordered multiporous lead dioxide membrane electrode and preparation method thereof |
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