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A kind of preparation method of chlorine analysis catalytic electrode supported by carbon fiber

A catalytic electrode, carbon fiber technology, applied in electrodes, electrolysis components, electrolysis process, etc., can solve the problems of expensive metal ruthenium, increased chlorine evolution potential, deactivation, etc.

Active Publication Date: 2020-10-27
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The earliest metal oxide electrode used in industry was RuO 2 -TiO 2 / Ti anode, but RuO 2 -TiO 2 The / Ti electrode has a short service life and is not suitable for strong acid and high current working conditions, and the metal ruthenium is expensive. In order to meet the needs of production development, people have done further research on the coating formula and preparation process of the anode, and developed RuO 2 -IrO 2 -TiO 2 / Ti, RuO 2 -SnO 2 -TiO 2 / Ti, RuO 2 -IrO 2 -SnO 2 -TiO 2 / Ti, RuO 2 -IrO 2 -SnO 2 -Co 3 o 4 -TiO 2 / Ti and other ternary, quaternary, and quinary coating formulations, and some add an intermediate layer between the coating and the substrate
At present, most of the electrodes used in industrial production are produced by the thermal decomposition method. After a period of use, the DSA electrode produced by this method will lose the active sites on the electrode surface due to the peeling off of the oxide coating and the dissolution of the active material. , resulting in an increase in the chlorine evolution potential on the DSA. When the chlorine evolution reaction potential is very close to the oxygen evolution reaction potential, the selectivity of the electrode reaction decreases significantly, which not only reduces the chlorine production efficiency, but also increases the oxygen evolution reaction. Formation of TiO at the coating interface 2 passivation film, leading to deactivation

Method used

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  • A kind of preparation method of chlorine analysis catalytic electrode supported by carbon fiber
  • A kind of preparation method of chlorine analysis catalytic electrode supported by carbon fiber
  • A kind of preparation method of chlorine analysis catalytic electrode supported by carbon fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A CF-loaded RuO 2 The preparation method is carried out according to the following steps:

[0045] 1) CF was pretreated, acetone, ethanol, and ultrapure water were ultrasonicated for 30 min each, and air-dried at room temperature for use.

[0046] 2) A three-electrode system was used, with CF, Pt sheet and Ag / AgCl as the working electrode, auxiliary electrode and reference electrode, respectively, with 5 mmol / L RuCl 3 The acidic aqueous solution was used as the electrolyte, heated in a water bath at 50 °C, and the cathodic deposition method was used to apply a constant working current of 20 mA cm -2 , the electrodeposition time was 1h, and the electrodeposited electrode was annealed at 500 °C for 5h in a tube furnace, and finally the CF-supported RuO was prepared. 2 nanoparticles. Through scanning electron microscope (SEM) observation, it was found that a layer of nanoparticles was uniformly loaded on CF. Figure 4 ; X-ray diffraction (XRD) analysis found that there...

Embodiment 2

[0048] A CF-loaded RuO 2 / SnO 2 The preparation method is carried out according to the following steps:

[0049] 1) CF was pretreated, acetone, ethanol, and ultrapure water were ultrasonicated for 30 minutes each, and air-dried at room temperature for use;

[0050] 2) Preparation of SnO 2 Precursor solution, SnCl 2 ·2H 2 O 2.5mmol, Na 3 C 6 H 5 O 7 ·2H 2 O 5mmol, ultrapure water 20mL, ethanol 20mL, CF and SnO 2 The precursor solution was put into the reaction kettle for hydrothermal reaction at 180°C for 8h, the reaction was completed, and the SnO 2 The CF was annealed in a tube furnace at 400 °C for 2 h.

[0051] 3) Using a three-electrode system, using SnO 2 / CF, Pt sheet and Ag / AgCl as working electrode, auxiliary electrode and reference electrode, 5mmol / L RuCl 3 The acidic aqueous solution was used as the electrolyte, heated in a water bath at 50 °C, and the cathodic deposition method was used to apply a constant operating current of 20 mA cm -2 , the electro...

Embodiment 3

[0053] A CF-loaded RuO 2 / TiO 2 / SnO 2 The preparation method is carried out according to the following steps:

[0054] 1) CF was pretreated, acetone, ethanol, and ultrapure water were ultrasonicated for 30 minutes each, and air-dried at room temperature for use;

[0055] 2) Preparation of SnO 2 Precursor solution, SnCl 2 ·2H 2 O 2.5mmol, Na 3 C 6 H 5 O 7 ·2H 2 O 5mmol, ultrapure water 20mL, ethanol 20mL, CF and SnO 2 The precursor solution was put into the reaction kettle for hydrothermal reaction at 180°C for 8h, the reaction was completed, and the SnO 2 The CF was annealed in a tube furnace at 400 °C for 2 h.

[0056] 3) Preparation of TiO 2 Precursor solution, tetrabutyl titanate 0.5mL, HCl 12mL, ultrapure water 12mL, and SnO 2 / CF and TiO 2 The precursor solution was put into the reaction kettle for hydrothermal reaction at 180°C for 2h, the reaction was completed, and the loaded TiO 2 and SnO 2 The CF was annealed in a tube furnace at 500 °C for 2 h.

...

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Abstract

The invention relates to the field of electrochemical catalytic fluorine evolution, and discloses a method for preparing carbon fiber loaded chlorine evolution catalytic electrodes. The technical scheme includes that CF is used as a working electrode, RuCl3 acidic aqueous solution is used as electrolyte solution, annealing treatment is carried out after electro-deposition is carried out, the electro-deposition includes applying constant currents of 5-20 mA cm<-2>, the electro-deposition time is 1-2 h, and the fluorine evolution catalytic electrodes RuO2 / CF can be prepared by the aid of the method; the CF represents carbon fiber cloth. The method has the advantages that the CF is used as a carrier, the catalytic electrodes are prepared by the aid of hydrothermal and electro-deposition processes, accordingly, the precious metal oxide loading capacity can be improved, and the precious metal oxide utilization rate can be increased; catalytic effects can be obviously enhanced, falling of active substances can be reduced, crack on the surfaces of the electrodes can be effectively reduced, and the electro-catalytic activity of the electrodes can be obviously improved.

Description

technical field [0001] The invention relates to the field of electrochemical catalytic chlorine analysis, in particular to a preparation method of a carbon fiber supported chlorine analysis catalytic electrode. Background technique [0002] Preparation of Cl by electrolysis of saturated salt (NaCl) water 2 and NaOH, is the largest scale aqueous electrolysis industry. With the development of chlor-alkali production technology and the increase in the demand for chlorine and alkali in the national economy, the anode materials used in the chlor-alkali industry are also constantly updated. The development history of electrolytic salt water confirms the development history of electrode materials. [0003] Titanium anodes are generally called DSA (Dimensionally Stability Anode), that is, size and shape stable anodes. Titanium anodes were first used in chlor-alkali production. After the efforts of engineers and technicians from various countries, they have been widely used in chemi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B1/34C25B11/06C25B11/12C23C18/12C25D9/06
CPCC23C18/1216C25B1/34C25D9/06C25B11/051C25B11/057C25B11/075C25B11/077C25B11/093
Inventor 王孝广张芳芳唐宾李晋平
Owner TAIYUAN UNIV OF TECH