CN107043096A - A kind of nanometer spherical Ag3PO4And its preparation method and application - Google Patents
A kind of nanometer spherical Ag3PO4And its preparation method and application Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002608 ionic liquid Substances 0.000 claims abstract description 23
- 229910000161 silver phosphate Inorganic materials 0.000 claims abstract description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 12
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical group [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 11
- 229940012189 methyl orange Drugs 0.000 claims description 11
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 11
- 238000006555 catalytic reaction Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 5
- 239000005416 organic matter Substances 0.000 claims description 4
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000010276 construction Methods 0.000 claims description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 1
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- 230000006872 improvement Effects 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005286 illumination Methods 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000001782 photodegradation Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 241000555268 Dendroides Species 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000003851 biochemical process Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002115 bismuth titanate Inorganic materials 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical class [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical group 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 description 1
- 230000002186 photoactivation Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
-
- B01J35/39—
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- B01J35/51—
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- B01J35/61—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/32—Spheres
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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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
Abstract
The invention discloses a kind of nanometer spherical Ag3PO4And its preparation method and application.The present invention takes to be added ionic liquid to synthesize nano silver in hydrothermal system.Ionic liquid provides a unique growing environment for new material, and ionic liquid can play a part of solvent, template during the course of the reaction, and a small amount of ionic liquid is added in hydro-thermal reaction and has prepared nanometer spherical silver orthophosphate.Nanometer spherical specific grain surface product is than larger, the organic pollution in degrading waste water under visible light, and degradation efficiency is higher, can save the energy, the environmental improvement tool of China is of great significance.
Description
Technical field
The present invention relates to novel nano-material, and in particular to a kind of nanometer spherical Ag3PO4And its preparation method and application.
Background technology
Energy crisis and environmental pollution are two hang-ups of 21st century facing mankind.China is both current world economy
Fastest-rising big country, is also world today's environmental pollution the most serious big country.With the development of society and science and technology, people's people's livelihood
The flat raising of running water, people propose higher and higher requirement, discharge of the China to industrial wastewater waste gas to the environment lived
Also strict discharge standard has been formulated.A large amount of waste water that factory produces, are handled, this is different using traditional materialization or biochemical process more
It there is to degree the rate of recovery low, consumption is high, processed waste water is difficult to the shortcoming for reaching discharging standards.From 1976
J.H.Carey etc. reports nano-TiO2Since photocatalytic oxidation is employed successfully in the degraded of useless Organic substance in water, semiconductor
Multiphase photocatalysis causes extensive attention in water treatment field.Conductor photocatalysis material can degrade in air or in water
Pollutant., organic pollution of bio-refractory big to some toxicity, the strong oxidizer of photoactivation agent catalysis generation,
Can be H thoroughly by oxidation operation under normal temperature, normal pressure2O、CO2Etc. small molecule.Compared with traditional desmear process, photocatalytic-oxidation
Change method has the advantages that nontoxic, safe and stable property is good, catalytic activity is high, instant effect, energy consumption are low, reusable.Current people
The catalysis material of most study is metal-oxide semiconductor (MOS), but these photochemical catalysts only have response to ultraviolet light, to visible
Light does not have response, and ultraviolet region is only account in solar energy less than 5%, and wavelength account for 43% for 460-750nm visible ray.For
Utilize visible ray, people are by In Researches On Modified Techniques of Photocatalysts, such as noble metal loading, doped transition metal ionses, it is nonmetallic from
Son adulterates, semiconductors coupling, and organic dyestuff photosensitizer etc. carrys out synthesizing visible light catalyst, and develops some novel visibles
Catalyst, such as bismuth titanates, bismuth molybdate, pucherite, BiOX etc., although these catalyst are to visible light-responded, but catalysis
Efficiency is not high.Therefore it is still current to design and prepare with unique texture, the novel visible catalysis material of efficient stable
One difficult point of research
In May, 2010, leaf golden flower seminars reported a kind of new, efficient Ag on nature materials3PO4Light
Catalysis material.Silver orthophosphate is cubic, and energy gap is 2.36ev, 525nm visible ray can be less than with absorbing wavelength, can
Very strong oxidability and the ability of photocatalysis Decomposition organic dyestuff are shown under the irradiation for seeing light, is containing silver orthophosphate sacrifice
In the aqueous solution of reagent, its quantum efficiency of more than 420nm wavelength illumination is up to 92%, and its photocatalysis efficiency is far above current institute
The visible light catalyst known.Leaf golden flower seminars use the Ag that ion-exchange is synthesized3PO4It is micron order, it is well known that catalysis
The granular size and pattern of agent have an impact to its catalytic efficiency.Dinh C T seminars have studied the synthesis of phosphoric acid Nano silver grain
Method, they make surfactant with oleyl amine, by controlling the amount of silver ion, oleyl amine, phosphoric acid to synthesize not in toluene solvant
With the phosphoric acid Nano silver grain (8-16nm) of particle diameter, because specific surface area increases to 14.5m2g-1, the photocatalytic activity of silver orthophosphate
It is greatly improved.A.Khan has synthesized phosphoric acid silver nano-grain (200nm) with sol method, and its photocatalytic activity is far above by sinking
The photocatalytic activity for the silver orthophosphate that shallow lake method is obtained.Yi in reaction system by adding a certain amount of PVP
(PVP) as surfactant, suppress the too fast growth of crystal grain, obtain particle diameter about 100nm nanometer Ag3PO4.Bi is utilized
H2O2Direct oxidation Ag nano wires have synthesized new two-dimentional dendroid Ag at room temperature3PO4Nanostructured.
Either above-mentioned preparation method is using toxic reagent (such as toluene), or reaction condition is bad to control (such as sol method),
Expensive starting materials (such as Ag nano wires).
The content of the invention
In order to solve the deficiencies in the prior art, the invention provides a kind of nanometer spherical Ag3PO4And preparation method thereof and should
With.
The technical scheme is that：A kind of nanometer spherical Ag3PO4Preparation method, with AgNO3And Na2HPO4For raw material,
Ionic liquid is added in hydrothermal system to synthesize nano silver.
Further improvement of the present invention includes：
Described ionic liquid is [C14Omim]Cl。
Ionic liquid is added in distilled water, after stirring, AgNO is added3, stirring to AgNO3It is completely dissolved, adds dropwise
Enter Na2HPO4Solution, ultrasonic agitation 30min is transferred in polytetrafluoroethyllining lining reactor, and 8h is reacted at 100-160 DEG C, from
Room temperature so is cooled to, product is washed for several times with deionized water and absolute ethyl alcohol, 24h is dried at 80 DEG C.
Add the 5%-10% that the ionic liquid scale of construction is solvent gross weight.
Ionic liquid [C is added in building-up process14Omim]Cl。
Another object of the present invention is to provide a kind of nanometer spherical Ag3PO4Preparation method, be specifically according to above-mentioned side
Method is made.
A kind of nanometer spherical Ag3PO4Preparation method, its product morphology is spherical, and particle diameter is in 100-200nm.
Invention further provides a kind of nanometer spherical Ag3PO4Application in photocatalytic degradation organic matter.
Described application, described organic matter is methyl orange, and specific biodegrading process is：By 0.3g Ag3PO4Add 250mL
Concentration for 20mg/L methyl orange solution in, after ultrasonic 30min, be transferred to multifunctional light chemical reaction instrument in, in 350W xenon lamps
Irradiation is lower to carry out light-catalyzed reaction.
The present invention takes to be added ionic liquid to synthesize nano silver in hydrothermal system.Ionic liquid carries for new material
For a unique growing environment, ionic liquid can play a part of solvent, template during the course of the reaction, in hydro-thermal reaction
The middle a small amount of ionic liquid of addition has prepared nanometer spherical silver orthophosphate.Nanometer spherical specific grain surface product is than larger, in visible ray
Organic pollution in lower degrading waste water, degradation efficiency is higher, can save the energy, and the environmental improvement to China has very
Important meaning.
It is an advantage of the invention that the silver orthophosphate being synthesized is spheric granules, specific surface area is right under visible light than larger
Organic pollutant degradation efficiency is high.
It is characteristic of the invention that adding a small amount of ionic liquid in hydrothermal system to synthesize nano silver, reaction condition holds
Easy to control, preparation method is simple and easy to apply, is conducive to large-scale promotion.
Brief description of the drawings
The XRD of nano silver in Fig. 1 examples 1.
The SEM photograph of nano silver in Fig. 2 examples 1.
The TEM photos of nano silver in Fig. 3 examples 1.
The photodegradation rate curve of nano silver under visible light illumination to methyl orange in Fig. 4 examples 1.
Fig. 5 is the transmission electron micrograph of sample in comparative example.
Fig. 6 is degradation rate curve of the comparative example under visible light illumination to methyl orange.
Embodiment
The present invention is elaborated with reference to embodiment.
Example 1
(1) ionic liquid [C14Mim] Cl source：Purchased from the prompt Chemical Co., Ltd. of upper marine origin
(2) nanometer Ag3PO4Preparation：7% (mass percent) [C is added in distilled water14Mim] Cl, stir
Afterwards, AgNO is added3, the solution that concentration is 0.05mol/L is made into, 0.05mol/L diammonium hydrogen phosphates are added dropwise in magnetic agitation 30min
The aqueous solution, ultrasonic agitation 30min is transferred in polytetrafluoroethyllining lining reactor, is reacted certain time at 120 DEG C, naturally cold
But room temperature is arrived, product is washed for several times with deionized water and absolute ethyl alcohol, 12h is dried at 80 DEG C and produces silver orthophosphate.
(3) degraded methyl orange：By 0.3g Ag3PO4Add in the methyl orange solution that 250mL concentration is 20mg/L, ultrasound
After 30min, it is transferred in multifunctional light chemical reaction instrument, light-catalyzed reaction is carried out under the irradiation of 350W xenon lamps.Taken every 10min
Sample, is centrifuged, take supernatant liquor wavelength at 300nm-500nm with the suction of spectrophotometer measurement methyl orange solution
Luminosity, calculates its degradation rate:R%=(A.- A)/A.Wherein A., A be respectively absorbance before and after photocatalysis.
(4) the thing phase of sample is analyzed on SIMENS companies D5005X- x ray diffractometer xs, is swept in JEOL JEM-6390LV
Retouch the pattern and size that product is observed on Electronic Speculum (SEM) and NEC company's 100CX transmission electron microscopes.
Fig. 1 is the XRD of sample, shows pure Ag3PO4Diffraction maximum.
Fig. 2 is the scanning electron micrograph of sample, and Fig. 3 is the transmission electron micrograph of sample, from this two figures
It can be seen that the Ag being synthesized3PO4To be spherical, particle diameter is in 100nm or so.
Fig. 4 is degradation rate curve of the sample under visible light illumination to methyl orange, it is seen that 60min is irradiated under light to methyl orange
Photodegradation rate be 94.3%.
Example 2
Step is prepared poly- with example 1, except that it is 5%, the silver orthophosphate particle diameter being synthesized to add the amount of ionic liquid
In 180nm or so, the photodegradation rate to methyl orange is 90.6%.
Example 3
Step is prepared poly- with example 1, except that it is 10%, the silver orthophosphate particle diameter being synthesized to add the amount of ionic liquid
In 130nm or so, the photodegradation rate to methyl orange is 92.1%.
Comparative example
Prepare step poly- with example 1, except that being not added with ionic liquid, the silver orthophosphate being synthesized is cube, particle
Size is at 1-3 μm, and Fig. 5 is the transmission electron micrograph of sample in comparative example.
Fig. 6 is degradation rate curve of the comparative example under visible light illumination to methyl orange, it is seen that 60min pairs is irradiated under light
The photodegradation rate of methyl orange is 82.4%.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (9)
1. a kind of nanometer spherical Ag3PO4Preparation method, it is characterised in that with AgNO3And Na2HPO4For raw material, in hydrothermal system
It is middle to add ionic liquid to synthesize nano silver.
2. a kind of nanometer spherical Ag according to claim 13PO4Preparation method, it is characterised in that described ionic liquid
Body is [C14Omim]Cl。
3. a kind of nanometer spherical Ag according to claim 13PO4Preparation method, it is characterised in that in distilled water plus
Enter ionic liquid, after stirring, add AgNO3, stirring to AgNO3It is completely dissolved, Na is added dropwise2HPO4Solution, ultrasound is stirred
30min is mixed, is transferred in polytetrafluoroethyllining lining reactor, 8h is reacted at 100-160 DEG C, room temperature is naturally cooled to, product is used
Deionized water and absolute ethyl alcohol washing for several times, dry 24h at 80 DEG C.
4. a kind of nanometer spherical Ag according to claim any one of 1-33PO4Preparation method, it is characterised in that add
The ionic liquid scale of construction is the 5%-10% of solvent gross weight.
5. a kind of nanometer spherical Ag according to claim any one of 1-33PO4Preparation method, it is characterised in that close
Ionic liquid [C is added during14Omim]Cl。
6. a kind of nanometer spherical Ag3PO4Preparation method, it is characterised in that according to claim 1-3 either method be made.
7. a kind of nanometer spherical Ag according to claim 63PO4Preparation method, it is characterised in that product morphology is ball
Shape, particle diameter is in 100-200nm.
8. a kind of nanometer spherical Ag3PO4Application in photocatalytic degradation organic matter.
9. application according to claim 8, it is characterised in that described organic matter is methyl orange, specific biodegrading process is：
By 0.3g Ag3PO4250mL concentration is added in 20mg/L methyl orange solution, after ultrasonic 30min, to be transferred to multi-functional photochemical
Learn in reaction instrument, light-catalyzed reaction is carried out under the irradiation of 350W xenon lamps.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108971512A (en) * | 2018-09-14 | 2018-12-11 | 江西科技师范大学 | A kind of the green preparation and its application of the rectangular particle of porous spongy Ag |
| CN113952981A (en) * | 2021-10-14 | 2022-01-21 | 扬州大学 | Bismuth vanadate organic-inorganic composite photocatalyst for self-assembly of perylene diimide and preparation method thereof |
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2017
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108971512A (en) * | 2018-09-14 | 2018-12-11 | 江西科技师范大学 | A kind of the green preparation and its application of the rectangular particle of porous spongy Ag |
| CN108971512B (en) * | 2018-09-14 | 2021-04-02 | 江西科技师范大学 | Green preparation method and application of porous spongy Ag square particles |
| CN113952981A (en) * | 2021-10-14 | 2022-01-21 | 扬州大学 | Bismuth vanadate organic-inorganic composite photocatalyst for self-assembly of perylene diimide and preparation method thereof |
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