CN105948140A - Preparation method of semiconductor-carried manganese cobalt composite oxide nanometer material - Google Patents
Preparation method of semiconductor-carried manganese cobalt composite oxide nanometer material Download PDFInfo
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- CN105948140A CN105948140A CN201610406573.3A CN201610406573A CN105948140A CN 105948140 A CN105948140 A CN 105948140A CN 201610406573 A CN201610406573 A CN 201610406573A CN 105948140 A CN105948140 A CN 105948140A
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Abstract
The invention discloses a preparation method of a semiconductor-carried manganese cobalt composite oxide nanometer material. The method includes the steps that 1, 0.05-50 g of semiconductor carriers are dispersed in 160 mL of deionized water, a semiconductor suspension solution is obtained, 0.01-1 g of potassium permanganate is added to 50mL-5L of deionized water, a potassium permanganate solution is obtained, and the concentration of the potassium permanganate solution is 0.002-20 g/l; 2, the semiconductor suspension solution and the potassium permanganate solution are mixed and irradiated by a 300 W xenon light source, irradiation time is 10-24 hours, by mass, 0.01-50 g of Co salt is added to the solution, then irradiation is conducted for 2 hours, and suction filtration and washing are conducted; 3, an obtained sample is dried, ground and then calcined for 0.5-12 hours at the temperature of 200-1000 DEG C after being ground, and the semiconductor-carried manganese cobalt composite oxide nanometer material is prepared. The preparation method has the advantages of being simple in process, easy and convenient to operate, low in production cost and environmentally friendly.
Description
Technical field
The present invention relates to nano-functional material preparation field, be specifically related to a kind of quasiconductor and support the preparation method of manganese cobalt composite oxide nano material.
Background technology
Manganese cobalt composite oxide nano material because of its have uniqueness architectural characteristic, prominent physicochemical properties and superior optics, magnetics, electrochemistry and catalytic performance and the most concerned, but this is also nowhere near and meets the actual demand of people, researcher by manganese cobalt composite oxide and quasiconductor (such as TiO2、CeO2) etc. combine, improve further its performance and extend its application prospect.
Generally, the method of sedimentation manganese cobalt composite oxide has hydro-thermal method, infusion process and sol-gal process etc. on the semiconductor, but, above synthetic method typically requires high temperature or strong acid and strong base environment, and the response time is long, therefore production cost height is found a kind of simple and rapid synthetic method and is particularly important.
Solar energy is green, energy-conservation, cleaning, sustainable, use the method in-situ deposition manganese cobalt composite oxide on the semiconductor of illumination, illumination method green non-pollution, having universality and versatility, the application in fields such as catalysis material, electrode material, ultracapacitor and sensors has latent prospect simultaneously.
Summary of the invention
The deficiency existed for prior art, it is an object of the invention to provide a kind of quasiconductor and supports the preparation method of manganese cobalt composite oxide nano material, and this material has higher activity；The method preparation technology is simple, and environment green is friendly.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of quasiconductor supports the preparation method of manganese cobalt composite oxide nano material, and it comprises the following steps:
(1). being scattered in 160 mL deionized waters by the semiconductor carrier of 0.05～50 g, ultrasonic disperse is uniform, obtains quasiconductor suspension solution, by 0.01～1g potassium permanganate, joining in the deionized water of 50 mL～5 L, obtain potassium permanganate solution, its concentration is 0.002～20 g/L；
(2). by above-mentioned steps (1) gained semi-conducting material suspension solution and above-mentioned potassium permanganate solution mix homogeneously, it is placed under 300 W xenon sources irradiation, light application time is 10 min～24 h, after illumination reaction, the Co salt that quality is 0.01～50 g is added in solution, illumination 2 h again, sucking filtration, washing, obtain sample；
(3). the sample of above-mentioned steps (2) gained being dried, ground, calcines 0.5～12 h after grinding at 200～1000 DEG C, prepared quasiconductor supports manganese cobalt composite oxide nano material；
Semiconductor carrier described in above-mentioned steps (1) is titanium dioxide nano-rod shape or titanium dioxide nanoplate shape or titania nanotube shape or the carrier of titanium dioxide nano-sphere shape,.
Semiconductor carrier described in above-mentioned steps (1) is the carrier with photocatalytic activity.Co salt described in above-mentioned steps (2) is one or more in cabaltous nitrate hexahydrate, Cobalt monosulfate heptahydrate, cobalt chloride hexahydrate and four acetate hydrate cobalts etc..
The invention has the beneficial effects as follows:
Compared with existing technology of preparing, the preparation method of the present invention can photocatalytic deposition manganese cobalt composite oxide the most on the semiconductor, can control to support thickness and loading, this material has higher activity；The method preparation technology is simple, and environment green is friendly, pollution-free.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) figure that the titanium dioxide nano-rod that embodiment 1 prepares supports manganese cobalt composite oxide nano material.
Fig. 2 is high resolution transmission electron microscopy (HRTEM) figure that the titanium dioxide nano-rod that embodiment 1 prepares supports manganese cobalt composite oxide nano material.
Fig. 3 is the denitration catalyst performance evaluation curve chart that the titanium dioxide nano-rod that embodiment 1 prepares supports manganese cobalt composite oxide nano material.
Fig. 4 is the denitration catalyst estimation of stability curve chart that the titanium dioxide nano-rod that embodiment 1 prepares supports manganese cobalt composite oxide nano material.
Fig. 5 is transmission electron microscope (TEM) figure that the titanium dioxide nanoplate that embodiment 2 prepares supports manganese cobalt composite oxide nano material.
Fig. 6 is the denitration catalyst performance evaluation curve chart that the titanium dioxide nano-rod that embodiment 3 prepares supports manganese cobalt composite oxide nano material.
Detailed description of the invention
Below in conjunction with specific embodiment, explanation that the present invention is further elaborated, but the enforceable situation of the present invention is not limited in following example.
Embodiment
1
Seeing Fig. 1, a kind of quasiconductor of the present invention supports the preparation method of manganese cobalt composite oxide nano material, and it comprises the following steps:
(1). by 0.1 g titanium dioxide nano-rod (TiO2), add 160 mL deionized waters, mix homogeneously, obtain TiO2Suspension solution；By 0.0395 g potassium permanganate, add 40 mL deionized waters, mix homogeneously, obtain potassium permanganate solution；
(2). by above-mentioned steps (1) gained TiO2Suspension solution and potassium permanganate solution mixing, mix homogeneously, irradiate above-mentioned mixed solution with 300 W xenon lamps, light application time 2 h, adds the cabaltous nitrate hexahydrate of 0.21825 g of 5 mL, then light application time 2 h after reaction, after reaction, sucking filtration, washing, obtain sample；
(3). the sample of above-mentioned steps (2) gained is dried, grinds, 2 h are calcined at 350 DEG C, prepared titanium dioxide nano-rod supports manganese cobalt composite oxide nano material, its transmission electron microscope (TEM) figure, as shown in Figure 1.
Above-mentioned titanium dioxide nano-rod supports the elimination reaction of nitrogen oxides in stationary source and moving source of manganese cobalt composite oxide nano material, titanium dioxide nano-rod supports manganese cobalt composite oxide nano material and puts into and carry out flue gas denitration catalyst reaction in fixed bed quartz tube reactor: be 3000～100000 h in air speed-1, temperature carries out NH under the conditions of being 90～350 DEG C3-SCR denitration is reacted, and the flue gas in its denitration reaction is by N2、O2, NO and NH3Composition, wherein, NO volumetric concentration is 200～1000 ppm, NH3Volumetric concentration is 200～1000 ppm, O2Concentration is 2～10 %, and Balance Air is N2, its denitration catalyst performance evaluation figure and denitration catalyst estimation of stability figure, as shown in Figure 3 and Figure 4.
Embodiment
2
See Fig. 5, the concrete steps of the present embodiment 2 with the concrete steps difference in embodiment 1 only: the described titanium dioxide nano-rod (TiO in the step (1) of the present embodiment2) it is titanium dioxide nanoplate (TiO2), other each step of the present embodiment 2 is identical with each step in embodiment 1, and the titanium dioxide nanoplate prepared supports the structure chart of the transmission electron microscope (TEM) of manganese cobalt composite oxide, as shown in Figure 5.
Embodiment
3
The concrete steps of the present embodiment 3 are with the concrete steps difference in embodiment 1 only: described in the step (2) of the present embodiment irradiates above-mentioned mixed solution with 300 W xenon lamps, the illumination reaction time is 1 h, add the cabaltous nitrate hexahydrate of 0.21825 g of 5 mL, light application time 1 h again, other each step of the present embodiment is identical with each step in embodiment 1, the titanium dioxide nano-rod prepared supports the denitration catalyst performance evaluation figure of manganese cobalt composite oxide, as shown in Figure 6.
Claims (4)
1. a quasiconductor supports the preparation method of manganese cobalt composite oxide nano material, it is characterised in that the method comprises the following steps:
(1). the semiconductor carrier of 0.05～50 g is scattered in 160 mL deionized waters, ultrasonic disperse is uniform, obtain quasiconductor suspension solution, by 0.01～1 g potassium permanganate, add 50 mL～5 L deionized waters, mix homogeneously, obtains potassium permanganate solution, and its concentration is 0.002～20 g/L；
(2). by above-mentioned steps (1) gained semi-conducting material suspension solution and above-mentioned potassium permanganate solution mix homogeneously, being placed under 300 W xenon sources irradiation, light application time is 10
Min～24 h, after illumination reaction, adds the Co salt that quality is 0.01～50 g, then illumination 2 h, sucking filtration, washing in solution, obtains sample；
(3). the sample of above-mentioned steps (2) gained being dried, ground, calcines 0.5～12 h after grinding at 200～1000 DEG C, prepared quasiconductor supports manganese cobalt composite oxide nano material.
A kind of quasiconductor the most according to claim 1 supports the preparation method of manganese cobalt composite oxide nano material, it is characterized in that, the semiconductor carrier described in above-mentioned steps (1) is titanium dioxide nano-rod shape or titanium dioxide nanoplate shape or titania nanotube shape or the carrier of titanium dioxide nano-sphere shape.
A kind of quasiconductor the most according to claim 1 supports the preparation method of manganese cobalt composite oxide nano material, it is characterised in that the semiconductor carrier described in above-mentioned steps (1) is the carrier with photocatalytic activity.
A kind of quasiconductor the most according to claim 1 supports the preparation method of manganese cobalt composite oxide nano material, it is characterized in that, the Co salt described in above-mentioned steps (2) is one or more in cabaltous nitrate hexahydrate, Cobalt monosulfate heptahydrate, cobalt chloride hexahydrate and four acetate hydrate cobalts etc..
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1698940A (en) * | 2005-04-11 | 2005-11-23 | 南京工业大学 | Improved method for preparing palladium-supported membrane by photocatalytic deposition |
| CN103127930A (en) * | 2013-03-13 | 2013-06-05 | 国电环境保护研究院 | High-activity nano-grade flue gas denitrification catalyst and low-temperature liquid-phase preparation method thereof |
-
2016
- 2016-06-12 CN CN201610406573.3A patent/CN105948140A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1698940A (en) * | 2005-04-11 | 2005-11-23 | 南京工业大学 | Improved method for preparing palladium-supported membrane by photocatalytic deposition |
| CN103127930A (en) * | 2013-03-13 | 2013-06-05 | 国电环境保护研究院 | High-activity nano-grade flue gas denitrification catalyst and low-temperature liquid-phase preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| HANG HU, ET AL.: "Mechanistic Aspects of deNOx Processing over TiO2 Supported Co-Mn Oxide Catalysts: Structure-Activity Relationships and In Situ DRIFTs Analysis", 《ACS CATALYSIS》 * |
| HYUNWOONG PARK, ET AL.: "Effects of the preparation method of the ternary CdS/TiO/Pt hybrid photocatalysts on visible light-induced hydrogen production", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| 翁玉攀: "光沉积法负载型金属催化剂及其在光电催化中的应用", 《感光科学与光化学》 * |
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Application publication date: 20160921 |