CN105771988A - Method for preparing high-catalytic-activity hierarchical structure silver molybdate - Google Patents
Method for preparing high-catalytic-activity hierarchical structure silver molybdate Download PDFInfo
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- 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
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- catalytic activity
- high catalytic
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- MHLYOTJKDAAHGI-UHFFFAOYSA-N silver molybdate Chemical compound [Ag+].[Ag+].[O-][Mo]([O-])(=O)=O MHLYOTJKDAAHGI-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 8
- 230000000694 effects Effects 0.000 title abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 230000001699 photocatalysis Effects 0.000 claims abstract description 10
- 230000001954 sterilising effect Effects 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 8
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002086 nanomaterial Substances 0.000 claims abstract description 7
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims description 14
- 230000003197 catalytic effect Effects 0.000 claims description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 238000007146 photocatalysis Methods 0.000 claims description 7
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000006731 degradation reaction Methods 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 claims description 4
- LWZFANDGMFTDAV-BURFUSLBSA-N [(2r)-2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O LWZFANDGMFTDAV-BURFUSLBSA-N 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- 239000000356 contaminant Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 4
- 229940071536 silver acetate Drugs 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 4
- 229950006451 sorbitan laurate Drugs 0.000 claims description 4
- 235000011067 sorbitan monolaureate Nutrition 0.000 claims description 4
- 229950003429 sorbitan palmitate Drugs 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- KQTXIZHBFFWWFW-UHFFFAOYSA-L disilver;carbonate Chemical compound [Ag]OC(=O)O[Ag] KQTXIZHBFFWWFW-UHFFFAOYSA-L 0.000 claims description 3
- 229960002050 hydrofluoric acid Drugs 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 229910001923 silver oxide Inorganic materials 0.000 claims description 3
- RHUVFRWZKMEWNS-UHFFFAOYSA-M silver thiocyanate Chemical compound [Ag+].[S-]C#N RHUVFRWZKMEWNS-UHFFFAOYSA-M 0.000 claims description 3
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 2
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 238000009388 chemical precipitation Methods 0.000 claims description 2
- KWABLUYIOFEZOY-UHFFFAOYSA-N dioctyl butanedioate Chemical compound CCCCCCCCOC(=O)CCC(=O)OCCCCCCCC KWABLUYIOFEZOY-UHFFFAOYSA-N 0.000 claims description 2
- 229920000136 polysorbate Polymers 0.000 claims description 2
- OABYVIYXWMZFFJ-ZUHYDKSRSA-M sodium glycocholate Chemical compound [Na+].C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(=O)NCC([O-])=O)C)[C@@]2(C)[C@@H](O)C1 OABYVIYXWMZFFJ-ZUHYDKSRSA-M 0.000 claims description 2
- 229950011392 sorbitan stearate Drugs 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract 2
- 238000005119 centrifugation Methods 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 241000191940 Staphylococcus Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts 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
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/683—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
- B01J23/686—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with molybdenum
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
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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
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.
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Cited By (4)
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 |
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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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