CN112064084A - Preparation method of metal monoatomic titanium suboxide electrode - Google Patents
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- 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
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
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- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
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Abstract
The preparation method of the metal monoatomic titanium suboxide electrode comprises the following steps; titanium suboxide is put into a powder feeder of plasma spraying equipment and is sprayed by a spray gun; putting the titanium carrier into a plasma spraying room, setting a spraying program, and spraying to obtain a titanium suboxide electrode; dissolving a metal salt in deionized water to obtain a metal precursor salt solution; adding the obtained metal precursor salt solution into an electrochemical deposition pool; putting a titanium suboxide electrode and a titanium anode into an electrochemical deposition pool, and adjusting the distance between polar plates; and introducing pulse current into the electrochemical deposition pool, then washing with deionized water, and then drying to obtain the electrocatalytic hydrogen peroxide generation electrode loaded with metal monoatomic ions. The method prepares the metal monoatomic electro-catalytic electrode material by taking the surface oxygen defect of the titanium suboxide as an active site through an in-situ pulse electro-reduction method, realizes the monoatomic dispersion and fixation of metal atoms by utilizing the defect site, and obtains the electro-catalytic hydrogen peroxide generation electrode with high activity and high stability.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a preparation method of a metal monoatomic titanium suboxide electrode.
Background
The Fenton oxidation technology is a traditional advanced oxidation technology, and utilizes ferrous ions to catalyze hydrogen peroxide to generate hydroxyl radicals with strong oxidizing property, so that pollutants in water can be efficiently decomposed and removed. However, in the practical application process, the usage amount of the hydrogen peroxide is directly related to the COD of the wastewater, the consumption amount is too high, the treatment cost is higher, and the application of the Fenton technology in the treatment of the wastewater with higher concentration of COD is also limited. In order to solve the problem, researchers develop an electro-Fenton technology, realize the on-line preparation of hydrogen peroxide and participate in the reaction, and become a novel technology with the most advantages. Compared with the traditional Fenton technology, the method has the unique advantages that: (1) hydrogen peroxide is generated in the reaction process, so that the cost is reduced and the manufacturing cost is reduced; (2) secondary pollution cannot be generated; (3) the organic matter decomposition and removal efficiency is high, and the energy consumption is relatively low; (4) the reaction process is simple to control, and automatic control can be realized. The main working principle is as follows:
O2+H++2e→H2O2
in recent years, great researchers at home and abroad strive to obtain hydrogen peroxide production electrocatalysis catalysts with high efficiency and high selectivity through various means, and at present, porous carbon materials and supported noble metals are mostly adopted as catalysts to realize the production of hydrogen peroxide by electrocatalysis oxygen reduction.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a metal monatomic titanium suboxide electrode, which is used for preparing an electrocatalytic electrode material with dispersed metal monatomics by using an in-situ pulse electro-reduction method and taking oxygen defects on the surface of titanium suboxide as active sites, and realizing the monatomic dispersion and fixation of metal atoms by using the defect sites to obtain the electrocatalytic hydrogen peroxide generating electrode with high activity and high stability.
In order to achieve the purpose, the invention adopts the technical scheme that:
the preparation method of the metal monoatomic titanium suboxide electrode comprises the following steps;
a. 3kg of titanium suboxide is put into a powder feeder of plasma spraying equipment;
b. putting the titanium carrier into a plasma spraying room, setting a spraying program, and spraying titanium suboxide by a spray gun to obtain a titanium suboxide electrode;
c. dissolving 1-2kg of metal salt in 50-150L of deionized water to obtain a metal precursor salt solution;
d. c, adding the metal precursor salt solution obtained in the step c into an electrochemical deposition pool;
e. b, putting the titanium anode, the titanium suboxide electrode in the step b and the titanium anode into the electrochemical deposition pool, and adjusting the distance between the electrode plates of the electrodes to be 10-50 cm;
f. and e, introducing pulse current into the electrochemical deposition pool in the step e, then washing the electrochemical deposition pool for 2-5 times by using deionized water, and drying the electrochemical deposition pool at the temperature of 30-60 ℃ to obtain the metal monatomic sub-oxidation state electrode.
In the step b, the working voltage of the spray gun is set to be 20-85V, and the working current is set to be 200-800A.
In the step b, the titanium carrier is a titanium plate, a titanium mesh, porous titanium or a foamed titanium plate.
In the step b, before the titanium suboxide is sprayed on the surface of the titanium carrier, the titanium carrier is subjected to sand blasting, acid treatment and washing.
In the step d, the metal salt is copper sulfate, copper nitrate, copper chloride, copper acetate, chloroauric acid, chloroplatinic acid or gold chloride.
In the step f, the current is 5-50A, the voltage is 5-20V, the pulse time interval is 5-20 seconds, and the deposition time is 5-20 minutes.
The invention has the beneficial effects that:
the metal monoatomic subatomic electrode provided by the invention is combined with conductive titanium suboxide through metal atoms, metal atoms are anchored by using defect sites in the subatomic state, the dispersity and the stability of the metal atoms are improved, hydrogen peroxide is produced on line and simultaneously used as a catalyst to participate in reaction, and strong oxidative hydroxyl radicals can be generated without adding ferrous ions as the catalyst, so that organic pollutants in water are decomposed.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
a. 3kg of titanium suboxide is put into a powder feeder of plasma spraying equipment, the working voltage of a spray gun is set to be 20V, and the working current is set to be 200A;
b. after sand blasting, acid treatment and washing, the titanium plate is placed in a plasma spraying room, a spraying program is set, and a titanium dioxide electrode is obtained by spraying;
c. dissolving 1kg of metal salt in 50L of deionized water to obtain a metal precursor salt solution;
d. c, adding the metal precursor salt solution obtained in the step c into an electrochemical deposition pool;
e. b, putting the titanium suboxide electrode and the titanium anode in the step b into an electrochemical deposition pool, and adjusting the distance between the polar plates to be 10 cm;
f. and e, introducing pulse current into the electrochemical deposition pool in the step e, wherein the current is 5A, the voltage is 5V, the pulse time interval is 5 seconds, the deposition time is 5 minutes, then washing for 3 times by using deionized water, and drying at 40 ℃ to obtain the metal monoatomic titanium suboxide electrode.
Example 2
a. 3kg of titanium suboxide is put into a powder feeder of plasma spraying equipment, the working voltage of a spray gun is set to be 40V, and the working current is set to be 500A;
b. after sand blasting, acid treatment and washing, the titanium mesh is placed in a plasma spraying room, a spraying program is set, and a titanium dioxide electrode is obtained by spraying;
c. dissolving 1.5kg of metal salt in 100L of deionized water to obtain a metal precursor salt solution;
d. c, adding the metal precursor salt solution in the step c into an electrochemical deposition pool;
e. b, putting the titanium suboxide electrode and the titanium anode in the step b into an electrochemical deposition pool, and adjusting the distance between the polar plates to be 20 cm;
f. and e, introducing pulse current into the electrochemical deposition pool in the step e, wherein the current is 20A, the voltage is 10V, the pulse time interval is 10 seconds, the deposition time is 10 minutes, then washing for 3 times by using deionized water, and drying at 45 ℃ to obtain the metal monoatomic titanium suboxide electrode.
Example 3
a. 3kg of titanium suboxide is put into a powder feeder of plasma spraying equipment, the working voltage of a spray gun is set to be 85V, and the working current is set to be 800A;
b. b, carrying out sand blasting, acid treatment and washing on the porous titanium in the step b, putting the porous titanium into a plasma spraying room, setting a spraying program, and spraying to obtain a titanium suboxide electrode;
c. dissolving 2kg of metal salt in 150L of deionized water to obtain a metal precursor salt solution;
d. c, adding the metal precursor salt solution obtained in the step c into an electrochemical deposition pool;
e. b, putting the titanium suboxide electrode and the titanium anode in the step b into an electrochemical deposition pool, and adjusting the distance between the polar plates to be 30 cm;
f. and e, introducing pulse current into the electrochemical deposition pool in the step e, wherein the current is 50A, the voltage is 20V, the pulse time interval is 20 seconds, the deposition time is 20 minutes, then washing the electrochemical deposition pool for 5 times by using deionized water, and drying the electrochemical deposition pool at 60 ℃ to obtain the metal monoatomic titanium dioxide electrode.
And (3) experimental verification:
a. the metal monatomic titanium suboxide electrode prepared in example 3 and the titanium anode were placed in an electro-fenton reaction apparatus in a staggered manner;
b. b, introducing a water sample to be treated with COD of 500mg/L into the electro-Fenton reaction device in the step a;
c. b, introducing current into the electro-Fenton reaction device in the step a, wherein the current is 1000A, the voltage is 5V, and the retention time is 1 hour;
d. and (b) blowing oxygen into the electro-Fenton reaction device in the step a, wherein the gas flow is 20L/min.
e. B, collecting an effluent water sample after the electro-Fenton reaction device in the step a continuously operates for one hour, and determining the COD of the effluent water;
f. the COD value of the effluent is less than 50mg/L, and reaches the first level A of the sewage comprehensive discharge standard.
Claims (7)
1. The preparation method of the metal monoatomic titanium suboxide electrode is characterized by comprising the following steps;
a. titanium suboxide is put into a powder feeder of plasma spraying equipment;
b. putting the titanium carrier into a plasma spraying room, setting a spraying program, and spraying titanium suboxide by a spray gun to obtain a titanium suboxide electrode;
c. dissolving a metal salt in deionized water to obtain a metal precursor salt solution;
d. c, adding the metal precursor salt solution obtained in the step c into an electrochemical deposition pool;
e. b, putting the titanium anode and the titanium suboxide electrode in the step b into the electrochemical deposition pool, and adjusting the distance between electrode plates of the electrodes to be 10-50 cm;
f. and e, introducing current into the electrochemical deposition pool in the step e, washing the electrochemical deposition pool for 2 to 5 times by using deionized water, and drying the electrochemical deposition pool at 30 to 60 ℃ to obtain the metal monoatomic subaeration state electrode.
2. The method as claimed in claim 1, wherein the operating voltage of the lance in step a is set to 20-85V, and the operating current is set to 200-800A.
3. The method according to claim 1, wherein the titanium carrier in step b is a titanium plate, a titanium mesh, a porous titanium plate or a titanium foam plate.
4. The method for preparing a metal monatomic titanium monoxide electrode as recited in claim 1, wherein in the step b, the titanium support is subjected to sand blasting, acid treatment and washing before the titanium support is surface-sprayed with titanium monoxide.
5. The method as claimed in claim 1, wherein the metal salt is copper sulfate, copper nitrate, copper chloride, copper acetate, chloroauric acid, chloroplatinic acid, or gold chloride.
6. The method for preparing a metal monatomic titanium suboxide electrode according to claim 1, wherein in step f, the current is 5 to 50A, the voltage is 5 to 20V, the pulse time interval is 5 to 20 seconds, and the deposition time is 5 to 20 minutes.
7. The method of claim 1, wherein the amount of titanium monoxide in step a is 3kg, and 1-2kg of the metal salt in step c is dissolved in 50-150L of deionized water.
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Cited By (2)
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CN113149156A (en) * | 2021-06-07 | 2021-07-23 | 陕西科技大学 | Preparation method of titanium suboxide DSA anode |
CN114162907A (en) * | 2021-11-30 | 2022-03-11 | 上海交通大学 | Monoatomic electrode and preparation method and application thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113149156A (en) * | 2021-06-07 | 2021-07-23 | 陕西科技大学 | Preparation method of titanium suboxide DSA anode |
CN114162907A (en) * | 2021-11-30 | 2022-03-11 | 上海交通大学 | Monoatomic electrode and preparation method and application thereof |
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