CN104248954A - Preparation method of in-situ photo-reduction cuprous oxide/titanium dioxide compound - Google Patents
Preparation method of in-situ photo-reduction cuprous oxide/titanium dioxide compound Download PDFInfo
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- CN104248954A CN104248954A CN201410486621.5A CN201410486621A CN104248954A CN 104248954 A CN104248954 A CN 104248954A CN 201410486621 A CN201410486621 A CN 201410486621A CN 104248954 A CN104248954 A CN 104248954A
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- titanium dioxide
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- cuprous oxide
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Abstract
The invention relates to a preparation method of an in-situ photo-reduction cuprous oxide/titanium dioxide compound. The preparation method comprises the following steps: (1) adding 0.1-0.3 part of titanium dioxide nano particles and 0.01-0.03 part of CuCl2<.>2H2O into 10 parts of methyl alcohol/aqueous solution according to mass part, and performing ultrasonic dispersion, wherein the volume ratio of methyl alcohol to water is (1 to 1) to (1 to 6); (2) performing nitrogen aeration treatment on a solution obtained in the step (1) for 10-15min, and under a condition of magnetic stirring, and performing illumination reaction 1.5-2 hours by a 500w high-pressure mercury lamp; (3) after the reaction is ended, centrifugating a product obtained by the reaction, washing the product by absolute ethyl alcohol for two to three times, and drying the product under a condition that the temperature is 60-90 DEG C for 24-30 hours to obtain an earthy yellow solid which is the final products. By the adoption of an ultraviolet deposition reduction method, the products are higher in dispersion and uniform in size; the photocatalysis activity is much higher than that of pure Cu2O or pure TiO2; under the illumination of visible light, dye organic matters can be efficiently degraded; the raw materials of the product are low in cost; a preparation process is environment-friendly; the preparation period is short, the cost is low, the benefit is high, and industrial popularization is facilitated.
Description
Technical field
The present invention relates to a kind of is the preparation method of cuprous oxide/titanium dioxide compound, and especially a kind of preparation method of cuprous oxide/titanium dioxide compound of original position photo-reduction, belongs to catalysis technical field.
Background technology
Precious metal surface deposition improves the effective ways of photocatalyst activity.When noble metal contacts with semiconductor surface, carrier redistributes, and electronics is from the high TiO of fermi level
2to the noble metal flowing that fermi level is low, form micro cell, promotion light induced electron is separated with hole, thus improves photocatalytic activity.But because Precious Metals Resources is rare, expensive, this severely limits the large-scale application of noble metal.Copper is as a kind of common metal element, and resource distribution is extensive, and has unique electronic structure as transition metal, and this is just for ultraviolet light in-situ reducing prepares Cu
2o/TiO
2semiconductors coupling structure provides possibility.Cuprous oxide itself as a kind of can to visible light-responded P-type semiconductor material, its energy gap is only 2.0eV, effectively can produce photo-generated carrier under visible light illumination, and its photoelectric transformation efficiency can reach 18%, and nontoxic; And nano cuprous oxide is because of its superior photocatalysis performance, can effectively catalytic degradation industry nitrogenous agricultural chemicals, dyeing waste water, in organic pollution photocatalytic degradation field, have very large potentiality.Nanometer Cu
2o/TiO
2the preparation of composite has been reported, and main method has physical mixed method, electrochemical deposition method, colloid chemistry methods etc.Achievement in research all shows than pure Cu
2o or TiO
2better photocatalysis effect.But these methods need to add surfactant usually, make system complexity, the unmanageable problem of course of reaction.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art existence, adopt cheap mantoquita and business TiO
2nano particle (P25), as raw material, prepares the nanometer Cu of good dispersion, size uniformity by simple ultraviolet light local reduction way one step
2o/TiO
2composite, especially by under ultraviolet lighting by Cu
2+be reduced to Cu
2o is carried on P25, forms Cu
2o/TiO
2compound also realizes carrying out efficient degradation to dyestuff under visible light.
The object of the invention is to have come by following technical solution, described preparation method comprises the steps:
1) by mass fraction, in the methanol/water solution of 10 parts, the titanium dioxide nano-particle of 0.1-0.3 part and the CuCl of 0.01-0.03 part is added
22H
2o, and carry out ultrasonic disperse; Wherein the volume ratio of methyl alcohol and water is 1:1-1:6;
2) by above-mentioned steps 1) after the solution of gained carries out nitrogen Air Exposure 10-15min, under magnetic agitation condition, with 500w lamp and high pressure mercury reaction 1.5-2 hour;
3) after reaction terminates, by centrifugal for the product obtained and with after absolute ethanol washing 2-3 time, obtain khaki solid after dry 24-30h and be end product under 60-90 DEG C of condition.
The preferred technical scheme of the present invention is:
1) by mass fraction, in the methanol/water solution of 10 parts, the titanium dioxide nano-particle of 0.2 part and the CuCl of 0.02 part is added
22H
2o, and carry out ultrasonic disperse; Wherein the volume ratio of methyl alcohol and water is 1:3;
2) by above-mentioned steps 1) after the solution of gained carries out nitrogen Air Exposure 10min, under magnetic agitation condition, react 2 hours with 500w lamp and high pressure mercury;
3) after reaction terminates, by centrifugal for the product obtained and with after absolute ethanol washing 2 times, obtain khaki solid after dry 24h and be end product under 70 DEG C of conditions.
The present invention utilizes Photodeposition will to be scattered here and there TiO
2the methanol/water solution system of nano particle and Cu presoma carries out UV-irradiation, TiO
2hole/duplet is produced under ultraviolet excitation.Due to methyl alcohol as hole sacrifice agent with excite hole to react, Cu presoma then reacts with excitation electron thus is Cu by in-situ reducing
2o is carried on TiO
22 nanoparticle surface.
Beneficial effect of the present invention:
1) adopt ultraviolet light deposition reducing process, reaction system is pure, method is simple, easily-controlled experimental conditions.
2) product disperses better, size uniformity, and photocatalytic activity is far above pure Cu
2o or pure TiO
2, can efficient degradation dyestuff organic matter under radiation of visible light.
3) this products material is cheap, and preparation process environmental protection, manufacturing cycle is short, and cost ineffective benefit is high, is convenient to industrialization promotion.
Accompanying drawing explanation
Fig. 1 is Cu of the present invention
2o/TiO
2transmission electron microscope figure looks figure (a) TEM.
Fig. 2 is Cu of the present invention
2o/TiO
2transmission electron microscope figure looks figure (b) HRTEM.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described in detail: the preparation method of the cuprous oxide/titanium dioxide compound of original position photo-reduction of the present invention, it comprises the steps:
1) by mass fraction, in the methanol/water solution of 10 parts, the titanium dioxide nano-particle of 0.1-0.3 part and the CuCl of 0.01-0.03 part is added
22H
2o, and carry out ultrasonic disperse; Wherein the volume ratio of methyl alcohol and water is 1:1-1:6;
2) by above-mentioned steps 1) after the solution of gained carries out nitrogen Air Exposure 10-15min, under magnetic agitation condition, with 500w lamp and high pressure mercury reaction 1.5-2 hour;
3) after reaction terminates, by centrifugal for the product obtained and with after absolute ethanol washing 2-3 time, obtain khaki solid after dry 24-30h and be end product under 60-90 DEG C of condition.
Be the Electronic Speculum figure of the cuprous oxide/titanium dioxide compound of original position photo-reduction as shown in Figure 1 and Figure 2.
Protection scope of the present invention is not limited to following embodiment, and therefore, every technical scheme formed by simple numerical value replacement etc., is all formed specific embodiments of the invention, and form protection scope of the present invention.
Embodiment 1: the preparation method of the cuprous oxide/titanium dioxide compound of original position photo-reduction of the present invention, it comprises the steps:
1) by mass fraction, in the methanol/water solution of 10 parts, the titanium dioxide nano-particle of 0.2 part and the CuCl of 0.02 part is added
22H
2o, and carry out ultrasonic disperse; Wherein the volume ratio of methyl alcohol and water is 1:3;
2) by above-mentioned steps 1) after the solution of gained carries out nitrogen Air Exposure 10min, under magnetic agitation condition, react 2 hours with 500w lamp and high pressure mercury;
3) after reaction terminates, by centrifugal for the product obtained and with after absolute ethanol washing 2 times, obtain khaki solid after dry 24h and be end product under 70 DEG C of conditions.
Embodiment 2: the preparation method of the cuprous oxide/titanium dioxide compound of original position photo-reduction of the present invention, it comprises the steps:
1) by mass fraction, in the methanol/water solution of 10 parts, the titanium dioxide nano-particle of 0.1 part and the CuCl of 0.01 part is added
22H
2o, and carry out ultrasonic disperse; Wherein the volume ratio of methyl alcohol and water is 1:1;
2) by above-mentioned steps 1) after the solution of gained carries out nitrogen Air Exposure 10min, under magnetic agitation condition, react 1.5 hours with 500w lamp and high pressure mercury;
3) after reaction terminates, by centrifugal for the product obtained and with after absolute ethanol washing 2 times, obtain khaki solid after dry 24h and be end product under 60 DEG C of conditions.
Embodiment 3: the preparation method of the cuprous oxide/titanium dioxide compound of original position photo-reduction of the present invention, it comprises the steps:
1) by mass fraction, in the methanol/water solution of 10 parts, the titanium dioxide nano-particle of 0.3 part and the CuCl of 0.03 part is added
22H
2o, and carry out ultrasonic disperse; Wherein the volume ratio of methyl alcohol and water is 1:6;
2) by above-mentioned steps 1) after the solution of gained carries out nitrogen Air Exposure 15min, under magnetic agitation condition, react 2 hours with 500w lamp and high pressure mercury;
3) after reaction terminates, by centrifugal for the product obtained and with after absolute ethanol washing 3 times, obtain khaki solid after dry 30h and be end product under 90 DEG C of conditions.
Embodiment 4: the preparation method of the cuprous oxide/titanium dioxide compound of original position photo-reduction of the present invention, it comprises the steps:
1) by mass fraction, in the methanol/water solution of 10 parts, the titanium dioxide nano-particle of 0.2 part and the CuCl of 0.03 part is added
22H
2o, and carry out ultrasonic disperse; Wherein the volume ratio of methyl alcohol and water is 1:4;
2) by above-mentioned steps 1) after the solution of gained carries out nitrogen Air Exposure 12min, under magnetic agitation condition, react 1.5 hours with 500w lamp and high pressure mercury;
3) after reaction terminates, by centrifugal for the product obtained and with after absolute ethanol washing 2-3 time, obtain khaki solid after dry 26h and be end product under 80 DEG C of conditions.
Claims (2)
1. a preparation method for the cuprous oxide/titanium dioxide compound of original position photo-reduction, is characterized in that described preparation method comprises the steps:
1) by mass fraction, in the methanol/water solution of 10 parts, the titanium dioxide nano-particle of 0.1-0.3 part and the CuCl of 0.01-0.03 part is added
22H
2o, and carry out ultrasonic disperse; Wherein the volume ratio of methyl alcohol and water is 1:1-1:6;
2) by above-mentioned steps 1) after the solution of gained carries out nitrogen Air Exposure 10-15min, under magnetic agitation condition, with 500w lamp and high pressure mercury reaction 1.5-2 hour;
3) after reaction terminates, by centrifugal for the product obtained and with after absolute ethanol washing 2-3 time, obtain khaki solid after dry 24-30h and be end product under 60-90 DEG C of condition.
2. the preparation method of the cuprous oxide/titanium dioxide compound of original position photo-reduction according to claim 1, is characterized in that in described step:
1) by mass fraction, in the methanol/water solution of 10 parts, the titanium dioxide nano-particle of 0.2 part and the CuCl of 0.02 part is added
22H
2o, and carry out ultrasonic disperse; Wherein the volume ratio of methyl alcohol and water is 1:3;
2) by above-mentioned steps 1) after the solution of gained carries out nitrogen Air Exposure 10min, under magnetic agitation condition, react 2 hours with 500w lamp and high pressure mercury;
3) after reaction terminates, by centrifugal for the product obtained and with after absolute ethanol washing 2 times, obtain khaki solid after dry 24h and be end product under 70 DEG C of conditions.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105826577A (en) * | 2016-03-16 | 2016-08-03 | 浙江理工大学 | Preparation method of super long branched Te-Pt composite nanowire |
| CN105944716A (en) * | 2016-05-25 | 2016-09-21 | 三明学院 | Method for preparing ultrafine TiO2 powder uniformly loading precious metal |
| CN109939679A (en) * | 2019-04-12 | 2019-06-28 | 齐鲁工业大学 | A kind of atom level dispersion copper CO2Convert co-catalyst and its preparation method and application |
| CN110180554A (en) * | 2019-04-30 | 2019-08-30 | 武汉理工大学 | A kind of method and its composite material of silver nanoparticle cubic block apex angle selective deposition copper oxide |
| CN113368854A (en) * | 2021-06-10 | 2021-09-10 | 西南林业大学 | Nano TiO (titanium dioxide)2/Cu2Preparation method of O porous composite material |
| CN115920887A (en) * | 2022-10-14 | 2023-04-07 | 电子科技大学 | In-situ grown copper-containing photocatalyst, preparation method and application thereof in reduction synthesis of ammonia by nitrate |
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| JPH0884912A (en) * | 1994-09-16 | 1996-04-02 | Sakai Chem Ind Co Ltd | High efficiency nitrogen oxide reduction method |
| CN101537354A (en) * | 2009-04-20 | 2009-09-23 | 大连理工大学 | Preparation method of visible-light activated cuprous oxide/titanium dioxide nano-composite photocatalyst and applications thereof |
| CN102974346A (en) * | 2012-11-27 | 2013-03-20 | 上海工程技术大学 | Cu2O/TiO2 photocatalyst on glass substrate and preparation method and application of Cu2O/TiO2 photocatalyst |
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2014
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Patent Citations (3)
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| JPH0884912A (en) * | 1994-09-16 | 1996-04-02 | Sakai Chem Ind Co Ltd | High efficiency nitrogen oxide reduction method |
| CN101537354A (en) * | 2009-04-20 | 2009-09-23 | 大连理工大学 | Preparation method of visible-light activated cuprous oxide/titanium dioxide nano-composite photocatalyst and applications thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105826577A (en) * | 2016-03-16 | 2016-08-03 | 浙江理工大学 | Preparation method of super long branched Te-Pt composite nanowire |
| CN105944716A (en) * | 2016-05-25 | 2016-09-21 | 三明学院 | Method for preparing ultrafine TiO2 powder uniformly loading precious metal |
| CN109939679A (en) * | 2019-04-12 | 2019-06-28 | 齐鲁工业大学 | A kind of atom level dispersion copper CO2Convert co-catalyst and its preparation method and application |
| CN109939679B (en) * | 2019-04-12 | 2022-03-04 | 齐鲁工业大学 | Atomic-level dispersed copper CO2Transformation promoter, preparation method and application thereof |
| CN110180554A (en) * | 2019-04-30 | 2019-08-30 | 武汉理工大学 | A kind of method and its composite material of silver nanoparticle cubic block apex angle selective deposition copper oxide |
| CN110180554B (en) * | 2019-04-30 | 2021-11-02 | 武汉理工大学 | Method for selectively depositing copper oxide on top angle of silver nano cube and composite material thereof |
| CN113368854A (en) * | 2021-06-10 | 2021-09-10 | 西南林业大学 | Nano TiO (titanium dioxide)2/Cu2Preparation method of O porous composite material |
| CN115920887A (en) * | 2022-10-14 | 2023-04-07 | 电子科技大学 | In-situ grown copper-containing photocatalyst, preparation method and application thereof in reduction synthesis of ammonia by nitrate |
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