CN105771988A - Method for preparing high-catalytic-activity hierarchical structure silver molybdate - Google Patents

Method for preparing high-catalytic-activity hierarchical structure silver molybdate Download PDF

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Publication number
CN105771988A
CN105771988A CN201610241281.9A CN201610241281A CN105771988A CN 105771988 A CN105771988 A CN 105771988A CN 201610241281 A CN201610241281 A CN 201610241281A CN 105771988 A CN105771988 A CN 105771988A
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molybdate
silver
preparation
catalytic activity
high catalytic
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代凯
王中辽
吕佳丽
梁长浩
朱光平
李栋佩
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Huaibei Normal University
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Huaibei Normal University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/66Silver or gold
    • B01J23/68Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/683Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
    • B01J23/686Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with molybdenum
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16Heavy metals; Compounds thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
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    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00Compounds of molybdenum
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    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

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Abstract

The invention discloses a method for preparing high-catalytic-activity hierarchical structure silver molybdate. Silver salt, surface active agent and molybdate are dissolved in deionized water, stirring and ultrasonic treatment are conducted to achieve sufficient dispersion, and the hierarchical micro-nano-structure silver molybdate is obtained through heating reaction and centrifugation to be used for photo-catalytic degradation of organic pollutants, sterilization and photo-catalytic hydrogen production. According to the synthesis method, operation is easy and quick, raw material cost is low, yield is high, repeatability is high, service life cycle is long, absolutely sustainable development and use are realized, and industrial prospects are broad; the prepared hierarchical micro-nano-structure silver molybdate has high organic pollutant photo-catalytic degradation property, high sterilization property and high photo-catalytic hydrogen production property, and an ideal approach is provided for fundamentally solving the environment and energy problems.

Description

A kind of preparation method of high catalytic activity graded structure silver molybdate
Technical field
The preparation method that the present invention relates to a kind of high catalytic activity graded structure silver molybdate, belongs to Chemical Engineering, energy environment and technical field of nano material.
Background technology
Environment and the energy are the mankind in 21 century encountered two big subject matters.Hydrogen Energy is as reproducible secondary energy sources carrier, there is the plurality of advantages such as cleaning, storage transport efficient, convenient, oneself is generally believed that it is a kind of optimal free of contamination green energy resource of new century, is described as " following oil ", is subject to showing great attention to of countries in the world.Considering from energy angle, photocatalytic hydrogen production by water decomposition is the optimal path of solar energy chemical conversion and storage.Photocatalysis technology is a kind of green technology having important application prospect at the energy and environmental area.Utilizing photocatalysis purifying technology remove organic pollution, sterilization and produce hydrogen and have the following characteristics that reaction condition is gentle, organic pollution can be decomposed into the inorganic molecules such as carbon dioxide and water, clean-up effect is thoroughly, photocatalyst stable chemical nature, cost are low, oxidation-reduction quality is strong, be absent from adsorbing saturated phenomenon, service life cycle is long.
But traditional catalysis material, can only be excited by ultraviolet light.A kind of high activity two dimension doping vario-property TiO2 nano-powder catalysis material and preparation method thereof such as patent disclosure that application number is 2013101022821, ultraviolet excitation can only be adopted, photocatalysis efficiency is relatively low, and ultraviolet light only accounts for about the 4% of solar energy, contrary visible ray then accounts for about the 46% of solar energy.Therefore researching and developing visible light-responded catalysis material is current letter key issue to be solved.Application number a kind of galapectite base optic catalytic composite material that has been the patent disclosure of 2013102615877 and preparation method thereof, this complicated process of preparation, Repeatability is relatively low, it is impossible to reach the purpose that industrialization uses.
Summary of the invention
In order to solve the deficiencies in the prior art, the preparation method that it is an object of the invention to provide a kind of high catalytic activity graded structure silver molybdate efficiently utilizing solar energy to remove organic pollution, sterilization and hydrogen production by water decomposition, synthesis simple and fast, Repeatability is good, service life cycle is long, the process of sustainable exploitation and use completely, fundamentally solves environment for the mankind and energy problem provides desirable approach.
For reaching above-mentioned purpose, the technology used in the present invention means are: the preparation method of a kind of high catalytic activity graded structure silver molybdate, silver salt, surfactant, molybdate are dissolved in deionized water, stirring, ultrasonic make it fully dispersed, pass through reacting by heating, it is centrifuged and obtains graduation micro nano structure silver molybdate, for photocatalysis degradation organic contaminant, sterilization and Photocatalyzed Hydrogen Production.
Further, the concentration of described silver salt is 0.01~5mol/L;The addition of surfactant is 0.01~10g/L;Molybdate concentration is 0.01~5mol/L.
Further, described silver salt is the one or more combination in silver nitrate, silver acetate, Disilver carbonate, silver oxide, boron fluoric acid silver, silver thiocyanate.
Further, described surfactant is the one or more combination in polyvinylpyrrolidone, ethylenediaminetetraacetic acid, sodium lauryl sulphate, dioctyl succinate disulfonate acid, sodium glycocholate, Polyethylene Glycol, sorbitan laurate, Sorbitan Palmitate, sorbitan stearate, tween, sodium laurylsulfate, 18-amine..
Further, described molybdate is one or both in ammonium molybdate and sodium molybdate.
Further, the stir speed (S.S.) of described stirring 10~10000 revs/min, mixing time 0.5~3h;Described ultrasonic power 20~2000W, ultrasonic time 0.5~4h;The temperature of described reacting by heating is 20~220 DEG C, and the reacting by heating time is 3min~10h, described is centrifuged as rotating speed 100~14000 revs/min, until product pH is neutral.
Further, described reacting by heating includes hydro-thermal or direct-fired chemical precipitation method.
The invention has the beneficial effects as follows: synthetic method is simple and quick, low raw-material cost, productivity is significantly high, and Repeatability is good, and service life cycle is long, completely the process of sustainable exploitation and use, has industrial prospect widely;Prepared graduation micro nano structure silver molybdate has the performance of significantly high photocatalysis degradation organic contaminant, sterilization and Photocatalyzed Hydrogen Production, fundamentally solves environment for the mankind and energy problem provides desirable approach.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further elaborated.
Fig. 1 is the photo of the silver molybdate in the embodiment of the present invention 1 with graded structure.
Detailed description of the invention
Embodiment 1
Weigh in the beaker that the silver acetate of 1mmol, 1g polyvinylpyrrolidone and 50ml deionized water add 100ml, stir under 2 hours 1000W power ultrasonic 1 hour and fully dissolve, add 0.1mol/L ammonium molybdate solution, react 3 hours under 30 DEG C of conditions, be centrifuged to neutrality, dry 6 hours in 80 DEG C of baking ovens.Its SEM photograph is as shown in Figure 1.Product is the molecular butterfly-like structure of granule.
Being put in 20mg/L methylene blue, under 410nmLED light source activation, degradation rate reaches more than 96%.
Embodiment 2
Weigh in the beaker that the silver nitrate of 5mmol, 3g Polyethylene Glycol and 50ml deionized water add 100ml, stir under 2 hours 1200W power ultrasonic 1 hour and fully dissolve, add 0.5mol/L sodium molybdate solution, 120 DEG C of hydro-thermals 4 hours, are centrifuged to neutrality, in 60 DEG C of baking ovens dry 10 hours.
Being put in staphylococcus, under 410nmLED light source activation, sterilizing rate reaches 100%.
Embodiment 3
Weigh in the beaker that the silver nitrate of 5mmol, 2g ethylenediaminetetraacetic acid and 50ml deionized water add 100ml, stir under 0.5 hour 1200W power ultrasonic 2 hours and fully dissolve, add 0.5mol/L sodium molybdate solution, react 4 hours under 50 DEG C of conditions, be centrifuged to neutrality, dry 6 hours in 80 DEG C of baking ovens.
Being put in photolysis water hydrogen reaction unit, the sub-efficiency of hydrogen output reaches 2%.
Embodiment 4
Weighing the mixture of the silver acetate of 5mol, Disilver carbonate, silver oxide, 1g polyvinylpyrrolidone, 1g Polyethylene Glycol, 1g sorbitan laurate, 1g Sorbitan Palmitate and 1L deionized water add in container, stir speed (S.S.) 8000 revs/min, mixing time 3 hours;Under 1200W power, abundant dissolving in ultrasonic 3 hours, adds 0.1mol/L ammonium molybdate solution, reacts 3 hours, centrifugal rotational speed 100~14000 revs/min when reacting by heating temperature 50 C, until product pH is neutral, dries 6 hours in 80 DEG C of baking ovens.
Embodiment 5
Weighing the mixture of the boron fluoric acid silver of 2mol, 3mol silver thiocyanate, 1g polyvinylpyrrolidone, 0.5g Polyethylene Glycol, 0.5g sorbitan laurate, 1g Sorbitan Palmitate and 1L deionized water add in container, stir speed (S.S.) 10000 revs/min, mixing time 2 hours;Under 1200W power, abundant dissolving in ultrasonic 3 hours, adds 1mol/L sodium molybdate solution, reacts 3 hours, centrifugal rotational speed 100~14000 revs/min when reacting by heating temperature 50 C, until product pH is neutral, dries 6 hours in 80 DEG C of baking ovens.
Synthetic method of the present invention is simple and quick, low raw-material cost, and productivity is significantly high, and Repeatability is good, and service life cycle is long, completely the process of sustainable exploitation and use, has industrial prospect widely;Prepared graduation micro nano structure silver molybdate has the performance of significantly high photocatalysis degradation organic contaminant, sterilization and Photocatalyzed Hydrogen Production, fundamentally solves environment for the mankind and energy problem provides desirable approach.
Disclosed embodiment of this invention is the explanation to technical scheme, it is impossible to as the restriction to present invention, and the those skilled in the art's simple change on basis of the present invention, still in protection scope of the present invention.

Claims (7)

1. the preparation method of a high catalytic activity graded structure silver molybdate, it is characterized in that: silver salt, surfactant, molybdate are dissolved in deionized water, stirring, ultrasonic make it fully dispersed, pass through reacting by heating, it is centrifuged and obtains graduation micro nano structure silver molybdate, for photocatalysis degradation organic contaminant, sterilization and Photocatalyzed Hydrogen Production.
2. the preparation method of high catalytic activity graded structure silver molybdate according to claim 1, it is characterised in that: the concentration of described silver salt is 0.01~5mol/L;The addition of surfactant is 0.01~10g/L;Molybdate concentration is 0.01~5mol/L.
3. the preparation method of high catalytic activity graded structure silver molybdate according to claim 2, it is characterised in that: described silver salt is the one or more combination in silver nitrate, silver acetate, Disilver carbonate, silver oxide, boron fluoric acid silver, silver thiocyanate.
4. the preparation method of high catalytic activity graded structure silver molybdate according to claim 2, it is characterised in that: described surfactant is the one or more combination in polyvinylpyrrolidone, ethylenediaminetetraacetic acid, sodium lauryl sulphate, dioctyl succinate disulfonate acid, sodium glycocholate, Polyethylene Glycol, sorbitan laurate, Sorbitan Palmitate, sorbitan stearate, tween, sodium laurylsulfate, 18-amine..
5. the preparation method of high catalytic activity graded structure silver molybdate according to claim 2, it is characterised in that: described molybdate is one or both in ammonium molybdate and sodium molybdate.
6. the preparation method of high catalytic activity graded structure silver molybdate according to claim 1, it is characterised in that: the stir speed (S.S.) of described stirring 10~10000 revs/min, mixing time 0.5~3h;Described ultrasonic power 20~2000W, ultrasonic time 0.5~4h;The temperature of described reacting by heating is 20~220 DEG C, and the reacting by heating time is 3min~10h, described is centrifuged as rotating speed 100~14000 revs/min, until product pH is neutral.
7. the preparation method of high catalytic activity graded structure silver molybdate according to claim 6, it is characterised in that: described reacting by heating includes hydro-thermal or direct-fired chemical precipitation method.
CN201610241281.9A 2016-04-19 2016-04-19 Method for preparing high-catalytic-activity hierarchical structure silver molybdate Pending CN105771988A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106345466A (en) * 2016-07-31 2017-01-25 上田环境修复股份有限公司 Method for preparing hydroxylation graphene oxide-magnesium titanate/silver molybdate composite materials
CN106915773A (en) * 2017-05-04 2017-07-04 洛阳理工学院 A kind of preparation method of strontium molybdate skeleton
CN110605119A (en) * 2019-09-27 2019-12-24 肇庆学院 Ag capable of rapidly degrading malachite green2MoO4/Ag2Preparation method of O material
CN116371406A (en) * 2023-03-10 2023-07-04 上海腾灵建设集团有限公司 Preparation, product and application of copper-supported oxygen defect mesoporous silver molybdate photocatalytic material

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CN102580739A (en) * 2012-03-06 2012-07-18 江苏大学 Graphene/silver molybdenum oxide compound visible-light catalyst and preparation method thereof
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CN1799691A (en) * 2006-01-13 2006-07-12 南京大学 Visible light responsible photocatalytic material of Ag2ZO4 type composite oxide, its preparation and application
CN101780980A (en) * 2010-02-05 2010-07-21 河北理工大学 Method for preparing ultrafine silver molybdate antibacterial powder by using ultrasonic wave
CN102580739A (en) * 2012-03-06 2012-07-18 江苏大学 Graphene/silver molybdenum oxide compound visible-light catalyst and preparation method thereof
JP2014123554A (en) * 2012-10-09 2014-07-03 Chiba Univ Fuel cell

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106345466A (en) * 2016-07-31 2017-01-25 上田环境修复股份有限公司 Method for preparing hydroxylation graphene oxide-magnesium titanate/silver molybdate composite materials
CN106345466B (en) * 2016-07-31 2020-05-01 江苏长三角环境科学技术研究院有限公司 Preparation method of hydroxylated graphene oxide-magnesium titanate/silver molybdate composite material
CN106915773A (en) * 2017-05-04 2017-07-04 洛阳理工学院 A kind of preparation method of strontium molybdate skeleton
CN106915773B (en) * 2017-05-04 2018-03-06 洛阳理工学院 A kind of preparation method of strontium molybdate skeleton
CN110605119A (en) * 2019-09-27 2019-12-24 肇庆学院 Ag capable of rapidly degrading malachite green2MoO4/Ag2Preparation method of O material
CN110605119B (en) * 2019-09-27 2022-07-19 肇庆学院 Ag capable of rapidly degrading malachite green2MoO4/Ag2Preparation method of O material
CN116371406A (en) * 2023-03-10 2023-07-04 上海腾灵建设集团有限公司 Preparation, product and application of copper-supported oxygen defect mesoporous silver molybdate photocatalytic material
CN116371406B (en) * 2023-03-10 2024-01-16 上海腾灵建设集团有限公司 Preparation, product and application of copper-supported oxygen defect mesoporous silver molybdate photocatalytic material

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Application publication date: 20160720