CN104437457A - Preparation method of full-spectrum sunlight catalyst - Google Patents
Preparation method of full-spectrum sunlight catalyst Download PDFInfo
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- CN104437457A CN104437457A CN201410614449.7A CN201410614449A CN104437457A CN 104437457 A CN104437457 A CN 104437457A CN 201410614449 A CN201410614449 A CN 201410614449A CN 104437457 A CN104437457 A CN 104437457A
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Abstract
The invention relates to a preparation method of a full-spectrum sunlight catalyst. The preparation method comprises the following steps: mixing strong acid with deionized water, and dissolving a titanium source in the mixed liquid under acute stirring; further stirring, adding rare earth element and nitrate into the mixed liquid to form a homogeneous solution, carrying out hydro-thermal treatment on suspension liquid, washing, filtering, drying, and grinding the mixture into powder; calcining the obtained powder in a muffle furnace, so as to obtain a surface-heterojunction rare earth element oxide/titanium dioxide composite nanometer photocatalytic material. According to the preparation method, rare earth oxide is successfully loaded to the surface of the nano-titanium dioxide and is good in dispersity, and the characters of the full-spectrum sunlight catalyst are stable; meanwhile, the full-spectrum sunlight catalyst has relatively good photocatalytic effect in visible light and ultraviolet light, the degradation rate of the full-spectrum sunlight catalyst in the visible light can reach 60% within 2 hours, and a new concept is provided for the actual application of the photocatalytic materials.
Description
Technical field
The present invention relates to the preparation method of a kind of full spectrum sunlight catalytic agent, belong to technical field of inorganic nano-material preparation.
Background technology
The photocatalytic degradation utilizing sunshine to carry out organic pollution as continuous energy supply is the important resolution policy utilizing regenerative resource to carry out environmental improvement.Spectrochemical property is stable, catalytic efficiency is high, oxidability is strong owing to having for titanium dioxide, nontoxic, cheap, the advantage such as technological process simple, operating condition easily controls, non-secondary pollution in actual applications, and it receives the increasingly extensive concern of people as photochemical catalyst.The developed countries such as America and Europe have all injected capital into and have carried out the research and development of optically catalytic TiO 2 technology with research effort, and new high-tech industry based on this is also formed.
But, although titania nanoparticles has very strong ultraviolet catalytic effect, its utilizable spectrum, only account for solar energy less than 5%.In recent years, although constantly there is various visible light catalyst to come out, most of visible light catalyst ultraviolet catalytic poor activity.Therefore, all there is the shortcomings such as catalytic efficiency is low, photocatalytic activity spectral region is narrow in the photochemical catalyst existed at present, is difficult to utilize sunshine to realize the high efficiency photocatalysis degraded of organic pollution.Rare earth is one of grand strategy resource of China, the rare earth reserves of China, output and export volume all row the first in the world.Rare earth element has complicated level structure and spectral characteristic, carries out doping vario-property, can effectively improve its photocatalysis efficiency to nano titanium oxide, is that most wishes one of technology solving visible ray utilization rate.Utilize titanium dioxide nano-belts as matrix material, there is in surface-assembled the second-phase nano particle (rare earth oxide) of visible light catalysis activity, not only can retain the efficient ultraviolet catalytic effect of titanium dioxide, give full play to the visible light catalytic effect of visible light catalyst, realize broadband photocatalysis, and owing to heterojunction structure can be formed between two-phase, suppress photo-generated carrier compound, thus obtain photochemical catalyst that is efficient, wide range.This titanium dioxide nano-belts surface heterogeneous medium structure is that full solar spectrum high efficiency photocatalyst provides a brand-new solution.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides the preparation method of a kind of full spectrum sunlight catalytic agent.
A preparation method for full spectrum sunlight catalytic agent, is characterized in that, comprise the steps:
(1) mixed with deionized water by strong acid, under stirring, be dissolved in mixed liquor by titanium source, the volume ratio of strong acid and deionized water is 1:3 to 1:1;
(2) continue to stir, rare earth element nitrate is distributed in above-mentioned mixed liquor, mixed liquor is put into the stainless steel autoclave of teflon lined, carry out hydro-thermal reaction; The mol ratio in wherein said rare earth element nitrate and titanium source is 1:10 to 4:10;
(3) reaction terminate after by precipitated product distilled water, absolute ethanol washing, then dry at 60 ~ 80 DEG C, and products therefrom is pulverized;
(4) product obtained is calcined in Muffle furnace, the agent of full spectrum sunlight catalytic can be obtained.
Titanium source described in step (1) is one in positive four butyl esters of metatitanic acid, isopropyl titanate, tetraethyl titanate or its combination.
The strong acid added described in step (1) is one or both in concentrated hydrochloric acid, red fuming nitric acid (RFNA).
Rare earth element nitrate described in step (2) is one in the cerous nitrate of hydration or non-hydrated, lanthanum nitrate, neodymium nitrate, yttrium nitrate, gadolinium nitrate, europium nitrate, terbium nitrate, samaric nitrate, thulium nitrate, erbium nitrate, ytterbium nitrate or its combination.
In step (2), hydrothermal temperature is 120-160 DEG C, and the time is 8-12 hour.
The present invention's rare earth oxide/titanium dioxide heterogeneous knot composite nano materials that adopted hydro-thermal method to prepare, rare earth oxide successfully can be loaded to the surface of nano titanium oxide by the method, and good dispersion, product property is stablized.Meanwhile, product all has good photocatalysis effect under visible ray and ultraviolet light, and the degradation rate of 2h can reach 60% under visible light, and the practical application for catalysis material provides new thinking.
Accompanying drawing explanation
Fig. 1: the scanning electron microscopic picture of the cerium oxide/titanium dioxide nano material obtained by embodiment 2.
Fig. 2: the X-ray powder diffraction pattern of the cerium oxide/titanium dioxide nano material obtained by embodiment 2.
Fig. 3: the ultraviolet catalytic performance of the cerium oxide/titanium dioxide nano material obtained by embodiment 2.
Fig. 4: the visible light catalytic performance of the cerium oxide/titanium dioxide nano material obtained by embodiment 2.
Detailed description of the invention
Below by embodiment, the present invention is further elaborated, and its object is only better to understand content of the present invention.Therefore, the cited case does not limit the scope of the invention.
Embodiment 1:
(1) concentrated hydrochloric acid is mixed (80ml) with volume ratio 1:3 with deionized water, under stirring, 0.02mol isopropyl titanate is dissolved in mixed liquor;
(2) continue to stir, 0.002mol rare earth lanthanum nitrate is distributed to above-mentioned mixed liquor, mixed liquor is put into the stainless steel autoclave of teflon lined, 150 DEG C of hydro-thermal reaction 8h;
(3) reaction terminate after by precipitated product distilled water, absolute ethanol washing, then dry at 80 DEG C, and products therefrom is pulverized;
(4) product 450 DEG C of calcining 30 min in Muffle furnace will obtained, namely obtain surface heterogeneous medium knot rare earth lanthanum oxide/titanium dioxide composite Nano catalysis material.
Embodiment 2:
(1) concentrated hydrochloric acid is mixed (80ml) with volume ratio 1:2 with deionized water, under stirring, 0.02mol tetra-n-butyl titanate is dissolved in mixed liquor;
(2) continue to stir, 0.002mol rare earth cerous nitrate is distributed to above-mentioned mixed liquor, mixed liquor is put into the stainless steel autoclave of teflon lined, 150 DEG C of hydro-thermal reaction 8h;
(3) reaction terminate after by precipitated product distilled water, absolute ethanol washing, then dry at 80 DEG C, and products therefrom is pulverized;
(4) the product 450 DEG C of calcining 30min in Muffle furnace will obtained, namely obtain surface heterogeneous medium knot rare earth cerium oxide/titanium dioxide composite Nano catalysis material.
Step (4) products therefrom is characterized its structure and crystal formation with SEM, XRD respectively, and tests its photocatalysis performance under visible ray, ultraviolet light.Fig. 1 is the pure titinium dioxide of reaction condition gained and the pattern of cerium oxide/composite titania material for this reason.As can be seen from the figure, pure TiO
2nanosphere is made up of nanometer rods, and every a branch of nanometer rods is made up of countless more tiny nano wire again.Modified, rare earth cerium oxide is nano particle, and particle diameter is approximately about 10 nm, is dispersed in titanium dioxide nano thread surface uniformly.As can be seen from XRD figure, the product of preparation is anatase titanium dioxide and cerium oxide, not assorted peak.0.1 gram of above-mentioned product reaches more than 99% to the degradation rate of 20 mg/litre methyl orange solutions in 60 minutes under the ultraviolet light of 300 watts; Under the visible ray of 500W, in 120 minutes, more than 59.5% is reached to the degradation rate of 20 mg/litre methyl orange solutions.
Embodiment 3
(1) red fuming nitric acid (RFNA) is mixed (80ml) with volume ratio=1:1 with deionized water, under stirring, 0.02mol tetra-n-butyl titanate is dissolved in mixed liquor;
(2) continue to stir, 0.002mol rare earth cerous nitrate is distributed to above-mentioned mixed liquor, mixed liquor is put into the stainless steel autoclave of teflon lined, 160 DEG C of hydro-thermal reaction 8h;
(3) reaction terminate after by precipitated product distilled water, absolute ethanol washing, then dry at 80 DEG C, and products therefrom is pulverized;
(4) the product 450 DEG C of calcining 30min in Muffle furnace will obtained, namely obtain surface heterogeneous medium knot rare earth cerium oxide/titanium dioxide composite Nano catalysis material.
Embodiment 4:
(1) concentrated hydrochloric acid is mixed (80ml) with volume ratio 1:3 with deionized water, under stirring, 0.02mol tetraethyl titanate is dissolved in mixed liquor;
(2) continue to stir, 0.008mol rare earth gadolinium nitrate is distributed to above-mentioned mixed liquor, mixed liquor is put into the stainless steel autoclave of teflon lined, 150 DEG C of hydro-thermal reaction 8h;
(3) reaction terminate after by precipitated product distilled water, absolute ethanol washing, then dry at 80 DEG C, and products therefrom is pulverized;
(4) the product 450 DEG C of calcining 30min in Muffle furnace will obtained, namely obtain surface heterogeneous medium knot rare earth cerium oxide/titanium dioxide composite Nano catalysis material.
Embodiment 5:
(1) concentrated hydrochloric acid is mixed (80ml) with volume ratio 1:3 with deionized water, under stirring, 0.02mol tetra-n-butyl titanate is dissolved in mixed liquor;
(2) continue to stir, 0.006mol rare earth cesium nitrate is distributed to above-mentioned mixed liquor, mixed liquor is put into the stainless steel autoclave of teflon lined, 140 DEG C of hydro-thermal reaction 10h;
(3) reaction terminate after by precipitated product distilled water, absolute ethanol washing, then dry at 80 DEG C, and products therefrom is pulverized;
(4) the product 450 DEG C of calcining 30min in Muffle furnace will obtained, namely obtain surface heterogeneous medium knot rare earth cerium oxide/titanium dioxide composite Nano catalysis material.
Claims (5)
1. a preparation method for full spectrum sunlight catalytic agent, is characterized in that, comprise the steps:
(1) mixed with deionized water by strong acid, under stirring, be dissolved in mixed liquor by titanium source, the volume ratio of strong acid and deionized water is 1:3 to 1:1;
(2) continue to stir, rare earth element nitrate is distributed in above-mentioned mixed liquor, mixed liquor is put into the stainless steel autoclave of teflon lined, carry out hydro-thermal reaction; The mol ratio in wherein said rare earth element nitrate and titanium source is 1:10 to 4:10;
(3) reaction terminate after by precipitated product distilled water, absolute ethanol washing, then dry at 60 ~ 80 DEG C, and products therefrom is pulverized;
(4) product obtained is calcined in Muffle furnace, the agent of full spectrum sunlight catalytic can be obtained.
2. the preparation method of full spectrum sunlight catalytic agent according to claim 1, is characterized in that, the titanium source described in step (1) is one in positive four butyl esters of metatitanic acid, isopropyl titanate, tetraethyl titanate or its combination.
3. the preparation method of full spectrum sunlight catalytic agent according to claim 1, is characterized in that, the strong acid added described in step (1) is one or both in concentrated hydrochloric acid, red fuming nitric acid (RFNA).
4. the preparation method of full spectrum sunlight catalytic agent according to claim 1, it is characterized in that, the rare earth element nitrate described in step (2) is one in the cerous nitrate of hydration or non-hydrated, lanthanum nitrate, neodymium nitrate, yttrium nitrate, gadolinium nitrate, europium nitrate, terbium nitrate, samaric nitrate, thulium nitrate, erbium nitrate, ytterbium nitrate or its combination.
5. the preparation method of full spectrum sunlight catalytic agent according to claim 1, is characterized in that, in step (2), hydrothermal temperature is 120-160 DEG C, and the time is 8-12 hour.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107282067A (en) * | 2017-07-10 | 2017-10-24 | 苏州科技大学 | Alumina substrate loads the photocatalyst material and its preparation method of full spectral absorption |
| CN108636395A (en) * | 2018-04-19 | 2018-10-12 | 浙江工商大学 | A kind of composite photo-catalyst of weakly visible photoresponse and its preparation and application |
| CN111545200A (en) * | 2020-05-21 | 2020-08-18 | 沈阳药科大学 | Ce-Ag-TiO2Nano composite antibacterial material and preparation method thereof |
| CN117511432A (en) * | 2024-01-05 | 2024-02-06 | 山东旭贝新材料有限公司 | Ultraviolet-transparent fluorine-containing polymer film and preparation method thereof |
| CN117563581A (en) * | 2023-09-12 | 2024-02-20 | 安徽农业大学 | Dy single-atom-loaded TiO 2 Photocatalyst, preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104118908A (en) * | 2014-07-31 | 2014-10-29 | 上海交通大学 | Controlled preparation method of ordered titanium dioxide nano-material |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104118908A (en) * | 2014-07-31 | 2014-10-29 | 上海交通大学 | Controlled preparation method of ordered titanium dioxide nano-material |
Non-Patent Citations (1)
| Title |
|---|
| 王瑞芬等: "钇掺杂纳米TiO2的制备及其降解甲基橙研究", 《内蒙古科技大学学报》, vol. 32, no. 4, 31 December 2013 (2013-12-31), pages 334 - 338 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107282067A (en) * | 2017-07-10 | 2017-10-24 | 苏州科技大学 | Alumina substrate loads the photocatalyst material and its preparation method of full spectral absorption |
| CN108636395A (en) * | 2018-04-19 | 2018-10-12 | 浙江工商大学 | A kind of composite photo-catalyst of weakly visible photoresponse and its preparation and application |
| CN111545200A (en) * | 2020-05-21 | 2020-08-18 | 沈阳药科大学 | Ce-Ag-TiO2Nano composite antibacterial material and preparation method thereof |
| CN117563581A (en) * | 2023-09-12 | 2024-02-20 | 安徽农业大学 | Dy single-atom-loaded TiO 2 Photocatalyst, preparation method and application thereof |
| CN117511432A (en) * | 2024-01-05 | 2024-02-06 | 山东旭贝新材料有限公司 | Ultraviolet-transparent fluorine-containing polymer film and preparation method thereof |
| CN117511432B (en) * | 2024-01-05 | 2024-05-07 | 山东旭贝新材料有限公司 | Ultraviolet-transparent fluorine-containing polymer film and preparation method thereof |
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