CN101279275A - Nano silver/silver chloride visible light photocatalysis material and preparation thereof - Google Patents
Nano silver/silver chloride visible light photocatalysis material and preparation thereof Download PDFInfo
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- CN101279275A CN101279275A CNA2008100166092A CN200810016609A CN101279275A CN 101279275 A CN101279275 A CN 101279275A CN A2008100166092 A CNA2008100166092 A CN A2008100166092A CN 200810016609 A CN200810016609 A CN 200810016609A CN 101279275 A CN101279275 A CN 101279275A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The present invention provides a nanometer silver/silver chloride visible light optical catalyzing material which consists of nanometer silver and silver chloride with a chemical formula of Ag/AgCl. The nanometer silver particles are loaded on the surface of the silver chloride and occupy 18 to 36 percent of the gross weight. The preparation method includes the following steps: (1) adopting a solid phase sintering method to synthesize silver molybdate, and obtain a mixture of molybdena and silver oxide, tabletting and then sintering; the sintered matter is the silver molybdate; (2) mixing the two according to a proportion of 1g of the silver molybdate and 20ml of concentrated hydrochloric acid and then putting into a high pressure kettle, heating to 150 to 220 DEG C and depositing for 48 to 72 hours; flushing the obtained deposit with a pH value of 7 to obtain the silver bromide; (3) mixing the silver chloride prepared by step (2) with the water solution of silver nitrate, stirring and adding glutamic acid, refluxing under a water bath of 70 DEG C, thus obtaining a nanometer silver/ silver chloride optical catalyst. The present invention effectively restrains silver chloride from decomposing by utilizing the plasma effect of the nanometer silver particles and can utilize the energy of solar light more effectively.
Description
Technical field
The present invention relates to a kind of catalysis material that is applied to hydrogen production by water decomposition or decomposition air and water pollutant and preparation method thereof, belong to the catalysis material technical field.
Background technology
Along with increasing the weight of of excessive development and use of resource and environmental pollution, human available resources are shortage more and more, and living environment is subjected to more and more serious destruction, and the energy and environmental problem become the two big subject matters that the world today pays close attention to.At present world energy sources mainly relies on non-renewable fossil resource, China's energy wastage in bulk or weight be non-renewable fossil energy more than 90%; How to solve current energy crisis? solar energy resources is abundant, and 1 year arrives earth total amount is 5.5 * 1026J, is 10,000 times of whole world energy resource consumption in a year now; If can prepare catalysis material efficiently, utilize solar energy to prepare hydrogen and come alleviating energy crisis that great Practical significance will be arranged; Often contain more organic pollution in industry and family expenses waste gas and the waste water, the waste water of this class eutrophication and waste gas can bring seriously to ecological environment and destroy.Along with international environment standard (ISO 14001, and October 1996) requires increasingly stringentization, the improvement technology of organic contamination also is rapidly developed.The application of photocatalysis in recent years in energy development and environmental protection is subject to people's attention day by day.
Catalysis material is one of focus of scientific research always.Last century early seventies, Fujishima of Tokyo Univ Japan and Honda discover, utilize the titanium dioxide single crystalline light-catalyzed reaction to make water resolve into hydrogen and oxygen.After this, the various countries scholar has carried out extensive studies around photocatalysis material of titanium dioxide.Light-catalysed principle can be explained with semi-conductive band theory: when the illumination that is equal to or higher than the energy gap of semi-conducting material with energy was penetrated, the valence band electronics was stimulated and transits to conduction band, produced corresponding hole simultaneously on valence band, formed electron hole pair; Light induced electron, hole are separated under the internal electric field effect and are moved to material surface, and redox reaction takes place.Light-catalyzed reaction is the physical and chemical process under photoinduction, can realize the light hydrogen production by water decomposition and purifies air and the effect of water.
Realize photocatalytic hydrogen production by water decomposition or decompose pollutant in the empty G﹠W, catalysis material must satisfy two conditions: at first, its energy gap is greater than the decomposition voltage of water or pollutant, and secondly valence band location should compare O
2/ H
2The current potential corrigendum of O, and H should be compared in the position of conduction band
+/ H
2More negative.The tradition catalysis material satisfies above-mentioned two conditions, but its can band gap greater than 3.0eV, so can only utilize sunshine medium ultraviolet light.Yet the energy of ultraviolet light only accounts for 4% of solar energy, and visible light accounts for 43%.
Current, the applied main catalysis material of people is the titanium dioxide with specific crystalline form, is called for short P25.It has been widely used in purifying air.Because it is higher that it can be with, too low to the utilization rate of solar energy, so each state is all endeavouring and is seeking visible-light photocatalyst efficiently.
Can expand the absorption region of visible light effectively based on the modified photocatalytic material of titanium dioxide, but cationic modification significantly reduces the light quantum conversion efficiency, anionic modification (N or C) under illumination easily light decompose, have unstability.
Silver chlorate has good response as a kind of light-sensitive material to light, but its can be with than higher, can only absorb ultraviolet light and unstable under illumination, so silver chlorate can not be used as visible-light photocatalyst separately.
Summary of the invention
The present invention is directed to that at present general catalysis material P25 exists low to solar energy utilization rate, be difficult to problem such as separation in the use repeatedly, a kind of photocatalytic activity height, easily separated is provided, solar energy is utilized high Nano Silver/silver/silver chloride visible light photocatalysis material, and a kind of preparation method of this catalysis material is provided.
Nano Silver/silver/silver chloride visible light photocatalysis material of the present invention is made of Nano Silver and silver chlorate, and chemical formula is Ag/AgCl, and nano-Ag particles loads on the surface of silver chlorate.Nano-Ag particles accounts for the 18%-36% of gross weight.
The preparation method of above-mentioned Nano Silver/silver/silver chloride visible light photocatalysis material may further comprise the steps:
(1) preparation silver molybdate adopts the method for solid-phase sintering to synthesize silver molybdate, and 1: 1 in molar ratio ratio is got molybdenum oxide and silver oxide, sintering behind mixing, the compressing tablet, and 300 ℃ of-500 ℃ of temperature, sintering 5 hours-8 hours, sinter is silver molybdate;
(2) preparation silver chlorate: in the 1g silver molybdate with put into autoclave after the ratio of 20ml concentrated hydrochloric acid is mixed both, be heated to 150 ℃-220 ℃, and under this degree, placed 48 hours-72 hours, make it that sufficient ion-exchange take place, the gained sediment is earlier with red fuming nitric acid (RFNA) flushing 3-5 time, use deionized water rinsing up to pH=7 again, products therefrom is silver chlorate;
(3) preparation Nano Silver/silver chlorate photochemical catalyst: with the made silver chlorate of step (2), both are mixed with the ratio of 10ml silver nitrate aqueous solution in the 0.1g-0.2g silver chlorate, the concentration of silver nitrate aqueous solution is 0.025mol/l-0.05mol/l, after stirring 10 minutes-20 minutes, add glutamic acid, the weight ratio of glutamic acid and silver chlorate is 0.3-0.6: 1, refluxed 3 hours-5 hours down for 70 ℃ in water-bath, and promptly get Nano Silver/silver chlorate photochemical catalyst.
The present invention is directed to the shortcoming of silver chlorate, nano-Ag particles is loaded on the surface of silver chlorate, utilize the plasma effect of nano-Ag particles, suppressed the silver chlorate decomposition effectively, guaranteed its stability under illumination, and its absorption bands has been extended to visible light, energy that can the more efficient use sunshine.Silver particle good conductivity is beneficial to spreading out of of electronics, thereby has guaranteed the stability of system.
The specific embodiment
Embodiment 1
(1) preparation silver molybdate: 1: 1 in molar ratio ratio is got molybdenum oxide 2.86g, silver oxide 4.63g, and sintering behind mixing, the compressing tablet, under 300 ℃ of temperature, sintering 8 hours, sinter is silver molybdate;
(2) preparation silver chlorate: get and put into autoclave after 5g silver molybdate and 100ml concentrated hydrochloric acid mix and be heated to 150 ℃ and place and enabled to take place sufficient ion-exchange in 72 hours, the gained sediment is earlier with red fuming nitric acid (RFNA) flushing 5 times, again with the deionized water rinsing number all over up to pH=7, products therefrom is silver chlorate.
(3) preparation Nano Silver/silver chlorate photochemical catalyst: get 0.2g made silver chlorate of (2) step and put into the liquor argenti nitratis ophthalmicus that 10ml concentration is 0.05mol/l, add 0.06g glutamic acid, refluxed 3 hours down for 70 ℃ in water-bath, promptly get Nano Silver/silver chlorate photochemical catalyst.
Embodiment 2
(1) preparation silver molybdate: 1: 1 in molar ratio ratio is got molybdenum oxide 2.86g, silver oxide 4.63g, sintering behind mixing, the compressing tablet.Under 400 ℃ of temperature, sintering 7 hours burns thing and is silver molybdate;
(2) prepare silver chlorate: at first with the synthetic silver molybdate of the method for solid-phase sintering, get and put into autoclave after 5g silver molybdate and 100ml concentrated hydrochloric acid mix and be heated to 170 ℃, place its ion-exchange that can fill of 72 angels, the gained precipitation is earlier with red fuming nitric acid (RFNA) flushing 5 times, again with the deionized water rinsing number all over up to pH=7, products therefrom is silver chlorate.
(3) preparation Nano Silver/silver chlorate photochemical catalyst: get 0.2g made silver chlorate of (2) step and put into the liquor argenti nitratis ophthalmicus that 10ml concentration is 0.05mol/l, add 0.12g glutamic acid, refluxed 4 hours for 70 ℃, promptly get Nano Silver/silver chlorate photochemical catalyst in water-bath.
Embodiment 3
(1) preparation silver molybdate: 1: 1 in molar ratio ratio is got molybdenum oxide 2.86g, silver oxide 4.63g, sintering behind mixing, the compressing tablet.Under 450 ℃ of temperature, sintering 6 hours, sinter is a silver molybdate;
(2) prepare silver chlorate: at first with the synthetic silver molybdate of the method for solid-phase sintering, get and put into autoclave after 5g silver molybdate and 100ml concentrated hydrochloric acid mix and be heated to 190 ℃, place and made it that sufficient ion-exchange can take place in 60 hours, the gained precipitation is earlier with red fuming nitric acid (RFNA) flushing 4 times, again with the deionized water rinsing number all over up to pH=7, products therefrom is silver chlorate.
(3) preparation Nano Silver/silver chlorate photochemical catalyst: get 0.1g made silver chlorate of (2) step and put into the liquor argenti nitratis ophthalmicus that 10ml concentration is 0.025mol/l, add 0.05g glutamic acid, refluxed 4 hours for 70 ℃ in water-bath, promptly get Nano Silver/silver chlorate photochemical catalyst.
Embodiment 4
(1) preparation silver molybdate adopts the method for solid-phase sintering to synthesize silver molybdate.Get molybdenum oxide 2.86g, silver oxide 4.63g, sintering behind mixing, the compressing tablet.Under 500 ℃ of temperature, sintering 5 hours, sinter is silver molybdate;
(2) prepare silver chlorate: at first with the synthetic silver molybdate of the method for solid-phase sintering, get and put into autoclave after 2.5g silver molybdate and 50ml concentrated hydrochloric acid mix and be heated to 220 ℃, place and made it that sufficient ion-exchange can take place in 48 hours, the gained precipitation is earlier with red fuming nitric acid (RFNA) flushing 3 times, again with the deionized water rinsing number all over up to pH=7, products therefrom is silver chlorate.
(3) preparation Nano Silver/silver chlorate photochemical catalyst: get 0.15g made silver chlorate of (2) step and put into the liquor argenti nitratis ophthalmicus that 10ml concentration is 0.025mol/l, add 0.06g glutamic acid, refluxed 5 hours for 70 ℃ in water-bath, promptly get Nano Silver/silver chlorate photochemical catalyst.
The prepared Nano Silver of the various embodiments described above/silver chlorate photochemical catalyst can be used for photodissociation water, decomposing organic matter and sterilization, and its effect is much better than the current catalysis material P25 that generally uses.
Claims (3)
1. a Nano Silver/silver/silver chloride visible light photocatalysis material is characterized in that, is made of Nano Silver and silver chlorate, and chemical formula is Ag/AgCl, and nano-Ag particles loads on the surface of silver chlorate.
2. according to Nano Silver/silver/silver chloride visible light photocatalysis material according to claim 1, it is characterized in that described nano-Ag particles accounts for the 18%-36% of gross weight.
3. the preparation method of the described Nano Silver/silver/silver chloride visible light photocatalysis material of claim 1 is characterized in that, may further comprise the steps:
(1) preparation silver molybdate adopts the method for solid-phase sintering to synthesize silver molybdate, and 1: 1 in molar ratio ratio is got molybdenum oxide and silver oxide, sintering behind mixing, the compressing tablet, and under 300 ℃ of-500 ℃ of temperature, sintering 5 hours-8 hours, sinter is silver molybdate;
(2) preparation silver chlorate: in the 1g silver molybdate with put into autoclave after the ratio of 20ml concentrated hydrochloric acid is mixed both, be heated to 150 ℃-220 ℃, and under this temperature, placed 48 hours-72 hours, make it that sufficient ion-exchange take place, the gained sediment is earlier with red fuming nitric acid (RFNA) flushing 3-5 time, use deionized water rinsing up to pH=7 again, products therefrom is silver chlorate;
(3) preparation Nano Silver/silver chlorate photochemical catalyst: with the made silver chlorate of step (2), both are mixed with the ratio of 10ml silver nitrate aqueous solution in the 0.1g-0.2g silver chlorate, the concentration of silver nitrate aqueous solution is 0.025mol/l-0.05mol/l, after stirring 10 minutes-20 minutes, add glutamic acid, the weight ratio of glutamic acid and silver chlorate is 0.3-0.6: 1, refluxed 3 hours-5 hours down for 70 ℃ in water-bath, and promptly get Nano Silver/silver chlorate photochemical catalyst.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101537350B (en) * | 2009-04-27 | 2010-11-03 | 武汉理工大学 | Ag/AgCl/TiO* nanotube array plasma visible-light photocatalyst and preparation method thereof |
| CN102102221A (en) * | 2011-01-25 | 2011-06-22 | 山东大学 | High-activity silver bromide sphaerocrystal and preparation method thereof |
| CN102350366A (en) * | 2011-08-25 | 2012-02-15 | 武汉理工大学 | Preparation method of Ag-AgCl-TiO2/rectorite composite photochemical catalyst |
| CN102489321A (en) * | 2011-12-28 | 2012-06-13 | 郑州大学 | Preparation method of Ag/AgCl hybrid photocatalyst |
| CN102600867A (en) * | 2012-02-10 | 2012-07-25 | 中国科学院广州地球化学研究所 | Surface plasma nano photocatalytic material CNTs (carbon nanotubes)-AgX as well as preparation method and application thereof |
| CN102614899A (en) * | 2012-02-23 | 2012-08-01 | 常州水木环保科技有限公司 | Synthesis method of load type silver chloride/silver catalyst |
| CN102658177A (en) * | 2012-05-02 | 2012-09-12 | 中国石油大学(华东) | Difunctional visual light responding catalyst, and preparation method and application thereof |
| CN102698777A (en) * | 2012-05-29 | 2012-10-03 | 武汉理工大学 | Method for preparing Ag/AgCl/BiMg2VO6 composite photocatalyst |
| CN102939994A (en) * | 2012-11-26 | 2013-02-27 | 河海大学 | Method for preparing silver/copper modified K4Nb6O17 film |
| CN103382144A (en) * | 2013-05-23 | 2013-11-06 | 河北科技大学 | Alkyl aromatic alpha- halogenation method |
| CN103623850A (en) * | 2013-11-05 | 2014-03-12 | 江苏大学 | Preparation method of high-activity silver bromide nano-photocatalytic material |
| CN103638952A (en) * | 2013-12-13 | 2014-03-19 | 黑龙江大学 | Method for preparing Ag/AgCl visible light catalyst by utilizing bacillus extracellular fluid |
| CN104190449A (en) * | 2014-08-20 | 2014-12-10 | 江苏大学 | Preparation method for hollow Ag/AgCl nano-structure photocatalysis material |
| CN104857551A (en) * | 2015-06-18 | 2015-08-26 | 中国医学科学院生物医学工程研究所 | Silver-bearing ntimicrobial dressing and preparation method thereof |
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2008
- 2008-05-26 CN CNA2008100166092A patent/CN101279275A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101537350B (en) * | 2009-04-27 | 2010-11-03 | 武汉理工大学 | Ag/AgCl/TiO* nanotube array plasma visible-light photocatalyst and preparation method thereof |
| CN102102221B (en) * | 2011-01-25 | 2012-12-26 | 山东大学 | High-activity silver bromide sphaerocrystal and preparation method thereof |
| CN102102221A (en) * | 2011-01-25 | 2011-06-22 | 山东大学 | High-activity silver bromide sphaerocrystal and preparation method thereof |
| CN102350366A (en) * | 2011-08-25 | 2012-02-15 | 武汉理工大学 | Preparation method of Ag-AgCl-TiO2/rectorite composite photochemical catalyst |
| CN102350366B (en) * | 2011-08-25 | 2013-07-17 | 武汉理工大学 | Preparation method of Ag-AgCl-TiO2/rectorite composite photochemical catalyst |
| CN102489321A (en) * | 2011-12-28 | 2012-06-13 | 郑州大学 | Preparation method of Ag/AgCl hybrid photocatalyst |
| CN102489321B (en) * | 2011-12-28 | 2013-07-31 | 郑州大学 | Preparation method of Ag/AgCl hybrid photocatalyst |
| CN102600867A (en) * | 2012-02-10 | 2012-07-25 | 中国科学院广州地球化学研究所 | Surface plasma nano photocatalytic material CNTs (carbon nanotubes)-AgX as well as preparation method and application thereof |
| CN102614899A (en) * | 2012-02-23 | 2012-08-01 | 常州水木环保科技有限公司 | Synthesis method of load type silver chloride/silver catalyst |
| CN102658177A (en) * | 2012-05-02 | 2012-09-12 | 中国石油大学(华东) | Difunctional visual light responding catalyst, and preparation method and application thereof |
| CN102658177B (en) * | 2012-05-02 | 2013-10-30 | 中国石油大学(华东) | Difunctional visual light responding catalyst, and preparation method and application thereof |
| CN102698777A (en) * | 2012-05-29 | 2012-10-03 | 武汉理工大学 | Method for preparing Ag/AgCl/BiMg2VO6 composite photocatalyst |
| CN102698777B (en) * | 2012-05-29 | 2013-12-25 | 武汉理工大学 | Method for preparing Ag/AgCl/BiMg2VO6 composite photocatalyst |
| CN102939994A (en) * | 2012-11-26 | 2013-02-27 | 河海大学 | Method for preparing silver/copper modified K4Nb6O17 film |
| CN103382144A (en) * | 2013-05-23 | 2013-11-06 | 河北科技大学 | Alkyl aromatic alpha- halogenation method |
| CN103623850A (en) * | 2013-11-05 | 2014-03-12 | 江苏大学 | Preparation method of high-activity silver bromide nano-photocatalytic material |
| CN103638952A (en) * | 2013-12-13 | 2014-03-19 | 黑龙江大学 | Method for preparing Ag/AgCl visible light catalyst by utilizing bacillus extracellular fluid |
| CN103638952B (en) * | 2013-12-13 | 2015-06-10 | 黑龙江大学 | Method for preparing Ag/AgCl visible light catalyst by utilizing bacillus extracellular fluid |
| CN104190449A (en) * | 2014-08-20 | 2014-12-10 | 江苏大学 | Preparation method for hollow Ag/AgCl nano-structure photocatalysis material |
| CN104857551A (en) * | 2015-06-18 | 2015-08-26 | 中国医学科学院生物医学工程研究所 | Silver-bearing ntimicrobial dressing and preparation method thereof |
| CN105268458A (en) * | 2015-11-03 | 2016-01-27 | 江苏大学 | Method for preparing plasma composite photo-catalyst |
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Open date: 20081008 |