CN114044560B - Manufacturing method of electrode for electrocatalytic degradation of nitrobenzene, product and application thereof - Google Patents
Manufacturing method of electrode for electrocatalytic degradation of nitrobenzene, product and application thereof Download PDFInfo
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- CN114044560B CN114044560B CN202111364298.0A CN202111364298A CN114044560B CN 114044560 B CN114044560 B CN 114044560B CN 202111364298 A CN202111364298 A CN 202111364298A CN 114044560 B CN114044560 B CN 114044560B
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- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 230000015556 catabolic process Effects 0.000 title claims description 20
- 238000006731 degradation reaction Methods 0.000 title claims description 20
- 239000010936 titanium Substances 0.000 claims abstract description 57
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 53
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 41
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000002243 precursor Substances 0.000 claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 30
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 27
- 239000010439 graphite Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 230000000593 degrading effect Effects 0.000 claims abstract description 10
- 239000007772 electrode material Substances 0.000 claims abstract description 10
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 10
- 238000003892 spreading Methods 0.000 claims abstract description 9
- 150000001462 antimony Chemical class 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 73
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 22
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- GVFOJDIFWSDNOY-UHFFFAOYSA-N antimony tin Chemical compound [Sn].[Sb] GVFOJDIFWSDNOY-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 229910006404 SnO 2 Inorganic materials 0.000 description 6
- 229910021607 Silver chloride Inorganic materials 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000006056 electrooxidation reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 231100000570 acute poisoning Toxicity 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Abstract
The invention discloses a manufacturing method of an electrode for electrocatalytically degrading nitrobenzene, a product and application thereof, comprising the steps of preparing a precursor solution containing antimony Sb and tin Sn; immersing graphite felt in precursor solution containing antimony and tin; spreading graphite felt adsorbed with precursor solution containing antimony and tin on a titanium sheet substrate, and preparing carbon-modified antimony doped tin dioxide Sb-SnO on the surface of the titanium sheet by using a thermal decomposition method 2 An electrode material. The electrode obtained by the method of the invention has higher activity of electrochemically degrading nitrobenzene, on one hand, the carbon-based material has stronger electron transmission capability, and the Sb-SnO is effectively improved 2 The charge transfer capability of the surface, on the other hand, the carbon material is used as a reaction substrate, so that the Sb-SnO is optimized 2 The surface structure of (2) increases the reactive sites.
Description
Technical Field
The invention belongs to the technical field of catalysis and environmental protection, and particularly relates to a manufacturing method of an electrode for electrocatalytic degradation of nitrobenzene, a product and application thereof.
Background
Nitrobenzene compounds are important raw materials or intermediates in industrial production and are widely applied to various fields of chemical industry, dyes, medicines, pesticides, organic synthesis and the like. Nitrobenzene has strong toxicity, and can absorb a large amount of steam or pollute the skin, thereby causing acute poisoning. Nitrobenzene has extremely high stability in water, and as the density of nitrobenzene is larger than that of water, nitrobenzene entering the water body can sink into the water bottom and remain unchanged for a long time. And because of certain solubility in water, the water pollution can last for a quite long time, nitrobenzene is difficult to be degraded by microorganisms, and the nitrobenzene is put into a blacklist of environmental-friendly pollutants in China. Therefore, it is necessary to establish an effective means for removing p-nitrobenzene organic pollutants. The traditional chemical, physical and biological methods can be faced with a plurality of problems when treating nitrobenzene-containing organic wastewater, such as the need of introducing chemical substances, difficult removal of trace and trace pollutants, high biotoxicity, high treatment difficulty and the like. The electrochemical oxidation has the advantages of mild reaction conditions, environmental friendliness, strong oxidizing capacity and the like, and is a hot spot of current research. Electrochemical oxidation is therefore considered a promising wastewater treatment technology and has attracted considerable attention in water treatment research.
Ti/Sb-SnO 2 The electrode has high oxygen evolution potential and electrocatalytic activity, and is widely studied in the field of electrochemical catalysis. But based on the semiconductor property of tin dioxide, the electron transmission rate is low, which limits the practical application of the tin dioxide. In order to further improve the catalytic performance and optimize the crystal structure, many researchers have tried different Ti/Sb-SnO 2 Modification methods such as Pt, ru, gd, cu and other metal ion doping, and the like. Although there is some improvement in the removal/degradation efficiency, on the one hand, heavy metal ion-modified Ti/Sb-SnO 2 The resulting dissolution of metals is prone to secondary pollution, and on the other hand, the high cost of using noble metal modification hinders large-scale industrial applications.
Based on the research background, the invention selects the carbon material as the base material, and the method is suitable for Sb-SnO 2 The structure and the surface are modified, and the Ti/Sb-SnO is effectively improved due to the advantages of high conductivity, good thermal/chemical stability, low raw material price, multiple surface active sites and the like of the carbon material 2 Is used as an electrocatalytic activity of the catalyst.
Disclosure of Invention
In order to realize efficient removal of nitrobenzene in water, the invention aims to provide a manufacturing method of an electrode for electrocatalytic degradation of nitrobenzene.
Still another object of the present invention is: an electrode product for electrocatalytic degradation of nitrobenzene prepared by the method is provided.
Yet another object of the present invention is: there is provided the use of the above product.
The invention aims at realizing the following scheme: the manufacturing method of the electrode for electrocatalytically degrading nitrobenzene comprises the following steps:
(1) Preparing a precursor solution containing antimony Sb and tin Sn: respectively configuring the concentration of SnCl to be 1mol/L 4 ˙5H 2 O-butanol solution, 1mol/L SbCl 3 N-butanol solution; taking two solutions according to the doping proportion of 2% -10% of antimony, and uniformly mixing the two solutions by ultrasonic treatment for 5 min to obtain a mixed solution;
(2) Immersing a graphite felt with the thickness of 1-3 mm and the size of 2 multiplied by 3 cm in an antimony-and tin-containing precursor solution to obtain a graphite felt adsorbed with the antimony-and tin-containing precursor solution;
(3) Spreading graphite felt adsorbed with antimony-tin-containing precursor solution on a titanium sheet substrate, roasting at 450 ℃ for 2h by using a thermal decomposition method, and finally naturally cooling to room temperature to obtain the carbon-modified antimony-doped tin dioxide Sb-SnO on the surface of the titanium sheet 2 An electrode material.
In the step (2), the graphite felt is soaked in the precursor solution containing antimony and tin for 10-30 min.
In the step (3), the titanium sheet is a titanium sheet with the thickness of 0.1-0.2 mm and the size of 2 multiplied by 3 cm, the titanium sheet is respectively washed for 1-2 hours by 40% sodium hydroxide solution and 6M HCl at 90 ℃, then washed for several times by deionized water, and naturally dried to obtain a pretreated titanium sheet for standby.
In the step (3), the temperature rising rate is 3 ℃/min.
The invention provides an electrode for electrocatalytic degradation of nitrobenzene, which is prepared by any one of the methods, and specifically comprises the following steps: a titanium sheet substrate; and the titanium sheet substrate is covered with a carbon-modified antimony-doped tin dioxide catalyst.
The invention provides an application of an electrode for electrocatalytically degrading nitrobenzene as an electrode in electrocatalytically degrading nitrobenzene at normal temperature.
The invention provides a manufacturing method of an electrode for electrocatalytic degradation of nitrobenzene. The electrode takes a titanium sheet as a substrate and carbon-modified Sb-SnO 2 The material is an electrode material and has higher activity of electrochemically degrading nitrobenzene. On the one hand, the carbon-based material has stronger electron transmission capability, so that the Sb-SnO is effectively improved 2 Charge transfer capability of the surface. On the other hand, the carbon material is used as a reaction substrate to optimize the Sb-SnO 2 The surface structure of (2) increases the reactive sites.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
Example 1
An electrode for electrocatalytic degradation of nitrobenzene is prepared by the following steps:
(1) Pretreatment of titanium sheets: respectively cleaning titanium sheets with the thickness of 0.1mm and the size of 2 multiplied by 3 cm with 40% sodium hydroxide solution and 6M HCl at 90 ℃ for 1h, then washing with deionized water for 3 times, and naturally airing to obtain pretreated titanium sheets for later use;
(2) Preparing a mixed solution of precursor solutions containing antimony Sb and tin Sn: respectively configuring the concentration of SnCl to be 1mol/L 4 ˙5H 2 O-butanol solution, 1mol/L SbCl 3 N-butanol solution; according to the doping proportion of antimony, snCl is taken 4 ˙5H 2 O-butanol 10ml, sbCl 3 N-butanol solution 0.2 ml, and ultrasound for 5 min to obtain mixed solution;
(3) Immersing the graphite felt with the thickness of 2mm and the size of 2 multiplied by 3 cm in a mixed solution of precursor solutions containing antimony and tin for 10 min to obtain the graphite felt adsorbed with the precursor solutions containing antimony and tin;
(4) Spreading graphite felt adsorbed with precursor solution containing antimony and tin on the pretreated titanium sheet substrateRoasting for 2 hours at a temperature rising rate of 3 ℃/min to 450 ℃ by using a thermal decomposition method, and finally naturally cooling to room temperature to obtain the carbon-modified antimony-doped tin dioxide Sb-SnO prepared on the surface of the titanium sheet 2 An electrode material.
The electrode is used as a working electrode, the Pt sheet is used as a counter electrode, ag/AgCl is used as a reference electrode, 50ml of 100mg/L nitrobenzene is used as a solution to be degraded, 0.71g of anhydrous sodium sulfate containing electrolyte, and the degradation rate of 3h nitrobenzene reaches 95% under 5V voltage.
Example 2
An electrode for electrocatalytic degradation of nitrobenzene was prepared in analogy to the procedure of example 1, following steps:
(1) Pretreatment of titanium sheets: respectively cleaning titanium sheets with the thickness of 0.1mm and the size of 2 multiplied by 3 cm with 40% sodium hydroxide solution and 6M HCl at 90 ℃ for 1h, then washing with deionized water for 3 times, and naturally airing to obtain pretreated titanium sheets for later use;
(2) Preparing a mixed solution of precursor solutions containing antimony Sb and tin Sn: respectively configuring the concentration of SnCl to be 1mol/L 4 ˙5H 2 O-butanol solution, 1mol/L SbCl 3 N-butanol solution; according to the doping proportion of antimony, snCl is taken 4 ˙5H 2 O-butanol 10ml, sbCl 3 N-butanol solution 0.5 ml, and ultrasound for 5 min to obtain mixed solution;
(3) Immersing graphite felt with the thickness of 3 mm and the size of 2 multiplied by 3 cm in the mixed solution for 20 min;
(4) Spreading graphite felt adsorbed with precursor solution containing antimony and tin on a titanium sheet substrate, roasting for 2h at 450 ℃ at a heating rate of 3 ℃/min by using a thermal decomposition method, and naturally cooling to room temperature to obtain carbon-modified antimony doped tin dioxide (Sb-SnO) on the surface of the titanium sheet 2 ) An electrode material.
The electrode is used as a working electrode, the Pt sheet is used as a counter electrode, ag/AgCl is used as a reference electrode, 50ml of nitrobenzene with concentration of 100mg/L is used as a solution to be degraded, 0.71g of anhydrous sodium sulfate containing electrolyte, and the degradation rate of nitrobenzene is 100% in 3h under the voltage of 5V.
Example 3
An electrode for electrocatalytic degradation of nitrobenzene was prepared in analogy to the procedure of example 1, following steps:
(1) Pretreatment of titanium sheets: respectively cleaning titanium sheets with the thickness of 0.2mm and the size of 2 multiplied by 3 cm with 40% sodium hydroxide solution and 6M HCl at 90 ℃ for 1h, then washing with deionized water for 3 times, and naturally airing to obtain pretreated titanium sheets for later use;
(2) Preparing a mixed solution of precursor solutions containing antimony Sb and tin Sn: respectively configuring the concentration of SnCl to be 1mol/L 4 ˙5H 2 O-butanol solution, 1mol/L SbCl 3 N-butanol solution; taking SnCl 4 ˙5H 2 O-butanol 10ml, sbCl 3 N-butanol solution 1ml, and ultrasound for 5 min to obtain mixed solution;
(3) Immersing a graphite felt with the thickness of 2mm, the size of 2 multiplied by 3 cm in the mixed solution for 30 min to obtain the graphite felt adsorbed with the precursor solution containing antimony and tin;
(4) Spreading graphite felt adsorbed with precursor solution containing antimony and tin on a pretreated titanium sheet substrate, roasting for 2h at 450 ℃ at a heating rate of 3 ℃/min by using a thermal decomposition method, and naturally cooling to room temperature to obtain carbon-modified antimony doped tin dioxide (Sb-SnO) on the surface of the titanium sheet 2 ) An electrode material.
The electrode is used as a working electrode, the Pt sheet is used as a counter electrode, ag/AgCl is used as a reference electrode, 50ml of 100mg/L nitrobenzene is used as a solution to be degraded, 0.71g of anhydrous sodium sulfate containing electrolyte, and the degradation rate of 3h nitrobenzene is 90% under the voltage of 5V.
Comparative example:
an electrode for electrocatalytically degrading nitrobenzene, the same as steps (1) and (2) of example 3, but without carbon modification of antimony doped tin dioxide, was made by the steps of:
(1) Pretreatment of titanium sheets: respectively cleaning titanium sheets with the thickness of 0.2mm and the size of 2 multiplied by 3 cm with 40% sodium hydroxide solution and 6M HCl at 90 ℃ for 1h, then washing with deionized water for 3 times, and naturally airing to obtain pretreated titanium sheets for later use;
(2) Preparing a mixed solution of precursor solutions containing antimony Sb and tin Sn: dividing intoThe concentration is 1mol/L SnCl 4 ˙5H 2 O-butanol solution, 1mol/L SbCl 3 N-butanol solution; taking SnCl 4 ˙5H 2 O-butanol 10ml, sbCl 3 N-butanol solution 1ml, and ultrasound for 5 min to obtain mixed solution;
(3) Directly soaking the pretreated titanium sheet obtained in the step (1) in the mixed solution for 30 min;
(4) Placing the titanium sheet in a muffle furnace, roasting for 2 hours at a temperature rising rate of 3 ℃/min to 450 ℃ by using a thermal decomposition method, and naturally cooling to room temperature to obtain the antimony doped tin dioxide (Sb-SnO) on the surface of the titanium sheet 2 ) An electrode material.
The electrode is used as a working electrode, the Pt sheet is used as a counter electrode, ag/AgCl is used as a reference electrode, 50ml of 100mg/L nitrobenzene is used as a solution to be degraded, 0.71g of anhydrous sodium sulfate containing electrolyte, and the degradation rate of 3h nitrobenzene is 80% under the voltage of 5V.
Inventive examples 1 to 3 are compared with comparative examples: the degradation rate of nitrobenzene is obviously improved.
Claims (6)
1. The manufacturing method of the electrode for electrocatalytically degrading nitrobenzene is characterized by comprising the following steps of:
(1) Preparing a precursor solution containing antimony Sb and tin Sn: respectively configuring the concentration of SnCl to be 1mol/L 4 ˙5H 2 O-butanol solution, 1mol/L SbCl 3 N-butanol solution; taking the two solutions according to the doping proportion of 2% -10% of antimony, and uniformly mixing the two solutions for 5 min by ultrasound to obtain precursor solution containing antimony and tin;
(2) Immersing a graphite felt with the thickness of 1-3 mm and the size of 2 multiplied by 3 cm in an antimony-and tin-containing precursor solution to obtain a graphite felt adsorbed with the antimony-and tin-containing precursor solution;
(3) Spreading graphite felt adsorbed with a precursor solution containing antimony and tin on a pretreated titanium sheet substrate, roasting for 2 hours at a temperature rising rate of 3 ℃/min to 450 ℃ by using a thermal decomposition method, and finally naturally cooling to room temperature to obtain the antimony doped tin dioxide Sb-SnO with carbon modification covered on the surface of the titanium sheet 2 Is of (a)A polar material;
in the step (2), the graphite felt is soaked in the precursor solution containing antimony and tin for 10-30 min;
in the step (3), titanium sheets with the thickness of 0.1-0.2 mm and the size of 2 multiplied by 3 cm are selected, the titanium sheets are respectively washed for 1-2 hours by 40% sodium hydroxide solution and 6M HCl at the temperature of 90 ℃, then are washed by deionized water for several times, and are naturally dried to obtain pretreated titanium sheets for standby.
2. The method for manufacturing an electrode for electrocatalytic degradation of nitrobenzene according to claim 1, wherein the method comprises the following steps:
(1) Pretreatment of titanium sheets: respectively cleaning titanium sheets with the thickness of 0.1mm and the size of 2 multiplied by 3 cm with 40% sodium hydroxide solution and 6M HCl at 90 ℃ for 1h, then washing with deionized water for 3 times, and naturally airing to obtain pretreated titanium sheets for later use;
(2) Preparing a mixed solution of precursor solutions containing antimony Sb and tin Sn: respectively configuring the concentration of SnCl to be 1mol/L 4 ˙5H 2 O-butanol solution, 1mol/L SbCl 3 N-butanol solution; according to the doping proportion of antimony, snCl is taken 4 ˙5H 2 O-butanol 10ml, sbCl 3 N-butanol solution 0.2 ml, and ultrasound for 5 min to obtain mixed solution;
(3) Immersing the graphite felt with the thickness of 2mm and the size of 2 multiplied by 3 cm in a mixed solution of precursor solutions containing antimony and tin for 10 min to obtain the graphite felt adsorbed with the precursor solutions containing antimony and tin;
(4) Spreading graphite felt adsorbed with a precursor solution containing antimony and tin on a pretreated titanium sheet substrate, roasting for 2 hours at a temperature rising rate of 3 ℃/min to 450 ℃ by using a thermal decomposition method, and finally naturally cooling to room temperature to obtain the antimony doped tin dioxide Sb-SnO with carbon modification covered on the surface of the titanium sheet 2 Is a metal electrode material.
3. The method for manufacturing an electrode for electrocatalytic degradation of nitrobenzene according to claim 1, wherein the method comprises the following steps:
(1) Pretreatment of titanium sheets: respectively cleaning titanium sheets with the thickness of 0.1mm and the size of 2 multiplied by 3 cm with 40% sodium hydroxide solution and 6M HCl at 90 ℃ for 1h, then washing with deionized water for 3 times, and naturally airing to obtain pretreated titanium sheets for later use;
(2) Preparing a mixed solution of precursor solutions containing antimony Sb and tin Sn: respectively configuring the concentration of SnCl to be 1mol/L 4 ˙5H 2 O-butanol solution, 1mol/L SbCl 3 N-butanol solution; according to the doping proportion of antimony, snCl is taken 4 ˙5H 2 O-butanol 10ml, sbCl 3 N-butanol solution 0.5 ml, and ultrasound for 5 min to obtain mixed solution;
(3) Immersing a graphite felt with the thickness of 3 mm and the size of 2 multiplied by 3 cm in the mixed solution for 20 min to obtain the graphite felt adsorbed with the precursor solution containing antimony and tin;
(4) Spreading graphite felt adsorbed with a precursor solution containing antimony and tin on a pretreated titanium sheet substrate, roasting for 2 hours at a temperature rising rate of 3 ℃/min to 450 ℃ by using a thermal decomposition method, and finally naturally cooling to room temperature to obtain the antimony doped tin dioxide Sb-SnO with carbon modification covered on the surface of the titanium sheet 2 Is a metal electrode material.
4. The method for manufacturing an electrode for electrocatalytic degradation of nitrobenzene according to claim 1, wherein the method comprises the following steps:
(1) Pretreatment of titanium sheets: respectively cleaning titanium sheets with the thickness of 0.2mm and the size of 2 multiplied by 3 cm with 40% sodium hydroxide solution and 6M HCl at 90 ℃ for 1h, then washing with deionized water for 3 times, and naturally airing to obtain pretreated titanium sheets for later use;
(2) Preparing a mixed solution of precursor solutions containing antimony Sb and tin Sn: respectively configuring the concentration of SnCl to be 1mol/L 4 ˙5H 2 O-butanol solution, 1mol/L SbCl 3 N-butanol solution; taking SnCl 4 ˙5H 2 O-butanol 10ml, sbCl 3 1ml of n-butanol solution, and uniformly mixing for 5 min by ultrasonic treatment to obtain a mixed solution;
(3) Immersing a graphite felt with the thickness of 2mm and the size of 2 multiplied by 3 cm in the mixed solution for 30 min to obtain the graphite felt adsorbed with the precursor solution containing antimony and tin;
(4) Spreading graphite felt adsorbed with a precursor solution containing antimony and tin on a pretreated titanium sheet substrate, roasting for 2 hours at a temperature rising rate of 3 ℃/min to 450 ℃ by using a thermal decomposition method, and finally naturally cooling to room temperature to obtain the antimony doped tin dioxide Sb-SnO with carbon modification covered on the surface of the titanium sheet 2 Is a metal electrode material.
5. An electrode for electrocatalytic degradation of nitrobenzene, which uses a titanium sheet as a substrate, and is covered with a carbon-modified antimony doped tin dioxide catalyst, characterized in that the electrode is manufactured by the method according to any one of claims 1 to 4.
6. Use of an electrode for electrocatalytically degrading nitrobenzene according to claim 5 as an electrode in electrocatalytically degrading nitrobenzene at room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202111364298.0A CN114044560B (en) | 2021-11-17 | 2021-11-17 | Manufacturing method of electrode for electrocatalytic degradation of nitrobenzene, product and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111364298.0A CN114044560B (en) | 2021-11-17 | 2021-11-17 | Manufacturing method of electrode for electrocatalytic degradation of nitrobenzene, product and application thereof |
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| Publication Number | Publication Date |
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| CN114044560A CN114044560A (en) | 2022-02-15 |
| CN114044560B true CN114044560B (en) | 2023-11-28 |
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| WO2017049466A1 (en) * | 2015-09-22 | 2017-03-30 | 许昌学院 | Composite electrode material, manufacturing method thereof, and use thereof in vanadium flow battery |
| CN112557592A (en) * | 2020-11-23 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of gas-sensitive material for formaldehyde detection, product and application thereof |
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| WO2017049466A1 (en) * | 2015-09-22 | 2017-03-30 | 许昌学院 | Composite electrode material, manufacturing method thereof, and use thereof in vanadium flow battery |
| CN112557592A (en) * | 2020-11-23 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of gas-sensitive material for formaldehyde detection, product and application thereof |
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