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A nickel-boron-fluorine co-doped lead dioxide anode and its preparation method and application

A technology of lead dioxide and co-doping, which is applied in chemical instruments and methods, oxidized water/sewage treatment, water/sludge/sewage treatment, etc., can solve the problem of unsatisfactory electrode current efficiency and electrode service life, and chemical stability It needs to be further improved, the preparation process conditions are harsh, etc., to achieve the effect of improving electrode stability, stable mechanical properties, and simple preparation methods

Active Publication Date: 2020-08-04
河南省宗祥环保工程有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The electrocatalytic oxidation reaction occurs on the surface of the electrode. Therefore, the key to the electrocatalytic oxidation treatment of phenol wastewater lies in the performance of the electrode. The lead dioxide anode has the advantages of low cost, strong corrosion resistance, and high electrocatalytic oxidation activity. In the electrocatalytic oxidation technology However, because the current efficiency and service life of the electrode in the electrocatalytic oxidation process are not ideal, scholars have used various methods to modify the lead dioxide electrode.
Although the doping of rare earth metals such as Ce and La improves the catalytic performance of lead dioxide, the price is relatively expensive; the doping of Bi, Fe and Go, although the oxidation performance is improved, is greatly affected by pH, and the doping concentration It is also not easy to control, which will reduce the bonding force of the coating and greatly reduce the stability of the electrode
[0006] Lead dioxide has two different crystal structures, the outer layer β-PbO 2 The electrical conductivity is good, but the chemical stability needs to be further improved
According to literature reports, nickel-doped metal oxide anodes can generate ozone in the electrocatalytic anodization process, so they have high catalytic activity; current domestic and foreign studies have shown that boron-doped diamond (BDD) electrodes have high stability and high Catalytic activity, limited by the harsh conditions of its preparation process, it is difficult to promote industrialization

Method used

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  • A nickel-boron-fluorine co-doped lead dioxide anode and its preparation method and application
  • A nickel-boron-fluorine co-doped lead dioxide anode and its preparation method and application
  • A nickel-boron-fluorine co-doped lead dioxide anode and its preparation method and application

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Embodiment 1

[0053] A method for preparing a nickel-boron-fluorine co-doped lead dioxide anode, comprising the following steps:

[0054] (1) The porous titanium plate is placed in a hydrochloric acid solution (the volume ratio of concentrated hydrochloric acid and water is 1:2) and boiled for 15min, then, ultrasonically (ultrasonic power 35KHz) in distilled water is cleaned for 8min to obtain a pretreated porous titanium plate; Citric acid, ethylene glycol, tin tetrachloride and antimony trichloride are mixed, heated and stirred to obtain a molten sol; wherein, the molar ratio of citric acid, ethylene glycol, tin tetrachloride and antimony trichloride is 650 :200:9:1;

[0055] (2) Coating the molten sol obtained in step (1) on the pretreated porous titanium plate, drying at 140°C for 10 minutes, then calcining at 550°C for 10 minutes, and cooling to 30°C; repeat coating-drying-calcination- Cooled for 5 times, calcined again at 550 °C for 1 h to obtain a tin-antimony bottom layer;

[0056...

Embodiment 2

[0061] A method for preparing a nickel-boron-fluorine co-doped lead dioxide anode, comprising the following steps:

[0062] (1) The porous titanium plate is placed in a hydrochloric acid solution (the volume ratio of concentrated hydrochloric acid and water is 1:2), boiled for 20 minutes, and ultrasonically cleaned with distilled water (ultrasonic power 40KHz) for 10 minutes to obtain a pretreated porous titanium plate; , ethylene glycol, tin tetrachloride and antimony trichloride are mixed, heated and stirred to obtain a molten sol; wherein, the molar ratio of citric acid, ethylene glycol, tin tetrachloride and antimony trichloride is 700:100 : 10:2;

[0063] (2) Coating the molten sol obtained in step (1) on the pretreated porous titanium plate, drying at 130°C for 20min, calcining at 600°C for 20min, cooling to 20°C, repeating coating-drying-calcination -Cool 6 times, calcined again at 600°C for 1.5h to obtain the tin-antimony bottom layer;

[0064] (3) the tin-antimony b...

Embodiment 3

[0068] A method for preparing a nickel-boron-fluorine co-doped lead dioxide anode, comprising the following steps:

[0069] (1) The porous titanium plate is placed in a hydrochloric acid solution (the volume ratio of concentrated hydrochloric acid and water is 1:2) and boiled for 18min, then, ultrasonically (ultrasonic power 30KHz) in distilled water is cleaned for 5min to obtain a pretreated porous titanium plate; Citric acid, ethylene glycol, tin tetrachloride and antimony trichloride are mixed, heated and stirred to obtain a molten sol; wherein, the molar ratio of citric acid, ethylene glycol, tin tetrachloride and antimony trichloride is 600 :150:8:1.5;

[0070] (2) Coating the molten sol obtained in step (1) on the pretreated porous titanium plate, drying at 135°C for 15min, then calcining at 500°C for 15min, and cooling to 40°C; repeat coating-drying-calcination- Cooling for 7 times, calcining at 500 °C for 2 h, to obtain the tin-antimony bottom layer;

[0071] (3) the...

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Abstract

The invention belongs to the technical field of electrochemical water treatment and specifically relates to a nickel-boron-fluorine codoped lead dioxide positive pole and a preparation method and application thereof. The preparation method disclosed by the invention comprises the following steps: mixing citric acid, ethylene glycol, stannic chloride and antimony trichloride and heating and stirring to obtain fused sol; then coating a pretreated matrix, drying, calcining and cooling; repeatedly coating-drying-calcining-cooling for many times; finally calcining to obtain a tin-antimony bottom layer; putting the tin-antimony bottom layer in a lead oxide alkaline solution to perform electrolytic deposition to obtain an alpha-lead dioxide intermediate layer; putting the alpha-lead dioxide intermediate layer into a beta-lead dioxide deposition solution to perform electrolytic deposition to obtain the nickel-boron-fluorine codoped lead dioxide positive pole. As the nickel is added, catalysisof the pole is improved; as the boron and the fluorine are added, stability of the pole is improved; the fluorine is favorable for improving an oxidation rate of Pb<2+>. By means of nickel-boron-fluorine codoping, stability of the lead dioxide pole is effectively improved, catalytic activity of the pole is improved, and the pole can be applied to treating of waste water.

Description

technical field [0001] The invention belongs to the technical field of electrochemical water treatment, and in particular relates to a nickel-boron-fluorine co-doped lead dioxide anode and a preparation method and application thereof. Background technique [0002] Phenol is an important organic chemical raw material, which can be used to prepare chemical products such as phenolic resin, pentachlorophenol, phenolphthalein, n-acetoethoxyaniline, etc. It has important uses in synthetic fibers, plastics, pesticides, dyes, coatings and oil refining industries. . [0003] However, with the rapid development of the industry and the increase in production capacity, serious phenol wastewater pollution has been brought about. It not only pollutes water sources and poisons fish in water bodies, but also inhibits the growth of microorganisms, destroys the ecological balance of water, and pollutes the environment; phenol wastewater flows into farmland, endangering the survival of crops,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F1/461C02F1/72C02F101/34
CPCC02F1/46109C02F1/4672C02F2001/46138C02F2101/345
Inventor 魏学锋苗娟张军杰张瑞昌万晓阳沈荣杰牛青山
Owner 河南省宗祥环保工程有限公司
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