[0029] Example 1
[0030] Doped nano TiO 2 The preparation method of the photode plate, including the following steps:
[0031] (1) Washing and cleaning treatment of stainless steel sheets: First use 600 mesh, 1000 mesh, 2000 mesh paper on the surface of the stainless steel plate, and put the stainless steel plate (25 * 20 * 0.5cm) into the addition of nitric acid after polishing. The solution (the volume fraction of 20%) is soaked in 24 h, and the nitric acid solution is used to remove the surface oxide of the stainless steel sheet. Finally, the purified water was washed to obtain a stainless steel plate after being cleaned;
[0032] (2) Sulfuric acid treatment of stainless steel sheet: Place the stainless steel sheet after the polishing in step (1) is placed in the reaction tank, soaked in 98% concentrated sulfuric acid overnight, then washed with deionized water to obtain a stainless steel after acid treatment. Board, concentrated sulfuric acid for passivation of stainless steel plate surface;
[0033] (3) Stainless steel electrode electrolysis treatment: After placing the acid treatment in step (2), the stainless steel plate is placed in the electrolytic cell, and the current density of electrodeposition is 8 mA / cm. 2 First, the electrolysis is electrolymented in the first electrolytic solution for 5 min, and then electrolyzed in the electrolytic solution for 7 minutes, the hot air is dried 3 min, and then placed in an electrolyte in the electrolyte, in order to continuously apply layer-by-layer Covered to achieve thicker, more stable and rugged catalytic films, alternately deposited 5 times in the two electrolytes, and 40 times in total; one of the electrolytes containing SN 2+ Solution of hydrochloric acid, anion is CL - , SN 2+ The concentration of 0.15 mol / L, the concentration of hydrochloric acid was 0.1 mol / L; the second electrolyte was containing SB 3+ Citric acid solution, anion is CL - , SB 3+ The concentration was 0.01 mol / L, the concentration of citric acid was 0.1 mol / L;
[0034] (4) Stainless steel electrode calcination treatment: The electrodes of electrodeposition of electrodeposition of metal ions in step (3) is placed in the muffle furnace, the temperature is 550 ° C, the calcination time is 4 h, the temperature rise rate is 5 ° C / min, obtained SS / SNO 2 -SB;
[0035] (5) 2 ml of bis (acetylacetone) diisopropyl titanate is added dropwise to 24 mL of acetic acid-ethylene glycol mixed solvent (V / V = 1: 1), at room temperature, 500R / min agitate 1h;
[0036] (6) Transferring the solution formed by step (5) to 50 ml of a stainless steel high pressure reactor in which polytetrafluoroethylene, heated to 200 ° C (temperature rate of 1 ° C / min), and collected after cooling to room temperature. Precipitation, washed 5 times after washing with distilled water and ethanol, dried overnight at 60 ° C;
[0037] (7) The white precipitate obtained by step (6) is soaked in a volume fraction (ie, the volume percentage content, the same below) is 10% ammonia solution, collects white precipitate, and in the muffle furnace, 500 ° C (temperature rate rate) Calcination under 1 ° C / min, resulting in nitrogen doped nano-titanium titanium dioxide;
[0038] (8) Take the nitrogen doped nano-titanium titanium dioxide 4G obtained by step (7) and 2 mL of 5 wt% Nafion solution is dispersed in 100 ml of isopropyl alcohol solution, ultrasonic 30min, resulting in a slurry;
[0039] (9) The slurry obtained by step (8) is applied to the surface of the electrode plate obtained in step (4), and the mass of the slurry and the electrode plate area ratio Mg: cm 2 The ratio was 5: 1 drip, after the discharging was dripped, the oven was dried at 60 ° C for 0.5 h, then at 80 ° C, 2 h was hot for 2 h, and the doping nano TiO was obtained. 2 Photoeolar plate SS / SNO 2 -SB @ TiO 2.
[0040] The doping nano TiO of the present embodiment 2 The photode plate is performed to perform oxidation properties and characterization verification:
[0041] Oxidation properties: Doped nano TiO in this example by linear voltammetry in electrochemical workstations 2 The photode plate is scanned verification, and its LSV curve is like figure 1 , From the figure, the doping nano TiO of the present embodiment 2 Photoeolar plate (1.8VVS.SCE (saturated glycide electrode)) than FTO @ TiO 2 (1.7VVS.SCE) The oxygen potential is high, and the doping nano TiO of the present embodiment will be described. 2 The oxidative properties of the photode plate is better, in which the FTO @ TiO of the present embodiment 2 The preparation method of the photode is: the obtained titanium dioxide slurry is applied to the surface of the FTO conductive glass, according to the mass of the slurry and the electrode plate area ratio Mg: cm 2 The ratio was 5: 1 drip, after dripping, the oven was dried at 60 ° C for 0.5 h, then obtained after hot pressing at 80 ° C for 2 h.
[0042] Doped nano TiO in this example 2 The XRD map of the photolatum is like figure 2 Doped nano TiO prepared from the figure 2 Atriky TiO is generated on the photode plate 2 Sno 2 -SB, can improve the oxidation resistance of the electrode; its electron microscope image 3 , By electron microscopy, SS / SNO of the present embodiment can be seen. 2 The surface of the -SB has a gap and is coated with nitrogen-doped nano titanium dioxide in SS / SNO. 2 After the -SB surface, the doping nano Tio is obtained. 2 Photoelectric plate, SS / SNO 2 -SB @ TiO 2 The surface smooth structure is tight, it is not easy to fall off, and it greatly improves the service life.
[0043] The present embodiment is doped nano TiO 2 The application of the photode plate in the treatment of waste salts, the specific steps are as follows:
[0044] Figure 4 For the device structure of the H-acid wastewater treatment device, the H-acid wastewater treatment device includes a degradation pool, a power source, a light source, a photode, a cathode, a single degradation pool is a cylinder having a diameter of 0.5 m, a high 0.6m, to implement Example 1 Prepared Doped Nano TiO 2 The photode plate is used as an anode, the same area of stainless steel sheets as the cathode, parallel to the degradation tank, the cathode and the anode and the power supply, NA obtained by the H acid production process. 2 SO 4 Salter mud dissolved to give a saturated waste salt solution as an example, the saturated waste salt solution is transferred into the degradation tank, and each degradation pool feed 50L, the bottom air, the cooling solution is 500 mg / L, degradation current density is 6mA / cm 2 , After 36W of UV lamps as a light source, the COD of the sewage obtained by the redox reduction treatment was 100 mg / L after the photovoltage degradation of 60 minutes.
