CN106268885B - A kind of preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst - Google Patents
A kind of preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst Download PDFInfo
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- CN106268885B CN106268885B CN201610562928.8A CN201610562928A CN106268885B CN 106268885 B CN106268885 B CN 106268885B CN 201610562928 A CN201610562928 A CN 201610562928A CN 106268885 B CN106268885 B CN 106268885B
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- titanium dioxide
- silver orthophosphate
- composite photocatalyst
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- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 32
- UZWUJDJSECQYDJ-UHFFFAOYSA-M silver dihydrogen phosphate oxygen(2-) titanium(4+) Chemical compound [O-2].[O-2].[Ti+4].P(=O)([O-])(O)O.[Ag+] UZWUJDJSECQYDJ-UHFFFAOYSA-M 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims abstract description 11
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 10
- 239000010452 phosphate Substances 0.000 claims abstract description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 229940071536 silver acetate Drugs 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000003054 catalyst Substances 0.000 claims description 21
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 8
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 6
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 6
- 229960004011 methenamine Drugs 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 0.000 claims description 3
- 239000002274 desiccant Substances 0.000 claims 1
- 239000000428 dust Substances 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 12
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000003756 stirring Methods 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 239000004408 titanium dioxide Substances 0.000 abstract description 5
- 230000010748 Photoabsorption Effects 0.000 abstract description 3
- 230000008878 coupling Effects 0.000 abstract description 3
- 238000010168 coupling process Methods 0.000 abstract description 3
- 238000005859 coupling reaction Methods 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 229940043267 rhodamine b Drugs 0.000 description 13
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000004904 UV filter Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 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
- 230000000593 degrading effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- -1 silver orthophosphate-titanium dioxide Titanium Chemical compound 0.000 description 1
- MFPVDOIQNSMNEW-UHFFFAOYSA-N silver oxygen(2-) titanium(4+) Chemical compound [O--].[O--].[Ti+4].[Ag+] MFPVDOIQNSMNEW-UHFFFAOYSA-N 0.000 description 1
- 229940019931 silver phosphate Drugs 0.000 description 1
- 229910000161 silver phosphate Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical group [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/19—Catalysts containing parts with different compositions
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides 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
- 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
-
- 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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- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a kind of preparation methods of fibrous silver orthophosphate-titanium dioxide composite photocatalyst, include the following steps：Silver acetate, phosphate aqueous solution are sequentially added in polyvinyl alcohol water solution, are adjusted pH to 5-6, are reacted under stirring；Butyl titanate is added into the mixture of gained, adjusting pH is 2-4, heating reaction 2-4 hours in the case where temperature is 70-80 DEG C of water bath condition, centrifuging and taking precipitation, washing, up to silver orthophosphate-titanium dioxide composite photocatalyst after drying.The present invention successfully synthesizes silver orthophosphate-titanium dioxide composite photocatalyst, while combining the photo absorption property of titanium dioxide and silver orthophosphate, its light-catalysed activity of significant increase；Preparation method is simple, at low cost, energy conservation and environmental protection and no coupling product；Obtained silver orthophosphate-titanium dioxide composite photocatalyst is novel fibrous structure, and photocatalytic activity is higher.
Description
Technical field
The present invention relates to catalyst technical field more particularly to a kind of fibrous silver orthophosphate-titanic oxide composite photochemical catalysts
The preparation method of agent.
Background technology
Human society and sustainable economic development increasingly face energy shortage and environmental degradation two large problems, are in high speed
The China of developing stage, it is particularly urgent to the research and development demand of clean energy resource and environmental protection technology.Theoretically, solar energy is utilized
Organic pollution during amount produces hydrogen energy source and environment of degrading is the desirable route to solve the above problems, development the relevant technologies and new
Material has bright prospects.
Japanese Scientists Fujishima in 1972 etc. has found TiO2Photochemical catalyzing may be implemented in monocrystalline electricity grade, later
Nano-TiO is found again2Ability with photocatalytic degradation organic matter becomes the hot spot material of scientist's gravity concern.But
TiO2Sunlight absorb section and be limited only to ultraviolet region, and this part light only accounts for and is irradiated to the 5% of ground solar spectrum, and
TiO2Quantum efficiency is relatively low, integrates the utilization ratio of solar energy only 1% or so, utilization ratio is very low.
Silver orthophosphate has good visible light-responded ability and outstanding as a kind of completely new conductor photocatalysis material
Photocatalytic degradation efficiency.In recent years silver orthophosphate has had aroused widespread concern in all circles of society, and is expected to become and realizes industrialized production and reality
The novel photocatalysis environment-friendly materials of border application.Studies show that, its water dispersible energy and organic coating under visible light illumination
Decomposability is the decades of times of current recognized photochemical catalyst.The efficiency and crystal shape of silver orthophosphate photocatalysis degradation organic contaminant
Looks have certain relationship, compared with random phosphoric acid Argent grain, have the silver phosphate photocatalyst of pattern to have better organic dirt
Contaminate object degradation efficiency.
However, silver orthophosphate and titanium dioxide are carried out the compound report with both comprehensive excellent properties in photoresponse at this stage
Road is also seldom, and therefore, the compound photochemical catalyst of silver orthophosphate and titanium dioxide of the exploitation with special appearance is to improve its photocatalysis
Activity and to seek easy environmentally friendly synthesis method significant for researcher.
Invention content
Based on the above the deficiencies in the prior art, technical problem solved by the invention is to provide a kind of fibrous phosphoric acid
The preparation method of silver-titanium dioxide composite photocatalyst, this method is simple and practicable, safety and environmental protection, obtained silver orthophosphate-titanium dioxide
Titanium composite photo-catalyst structure novel, photocatalytic activity are high.
In order to solve the above-mentioned technical problem, the present invention is achieved through the following technical solutions：The present invention provides a kind of fiber
The preparation method of shape silver orthophosphate-titanium dioxide composite photocatalyst, includes the following steps：
(1) silver acetate, phosphate aqueous solution are sequentially added in poly-vinyl alcohol solution, pH to 5-6 are adjusted, under stirring
Reaction；
(2) butyl titanate is added into the mixture obtained by step (1), adjusting pH is 2-4, is 70-80 DEG C in temperature
Water bath condition under heating reaction 2-4 hour, centrifuging and taking precipitation, washing, it is dry after to obtain the final product silver orthophosphate-titanium dioxide complex light urge
Agent.
Preferably, the pH adjusting agent used in step (1) is methenamine, and the middle pH adjusting agent used of step (2) is dilute
Nitric acid.
Preferably, the molar ratio of silver acetate and phosphoric acid in phosphate aqueous solution is 7 in step (1):1~3:1.
Preferably, the molar ratio of polyvinyl alcohol and phosphoric acid is 137 in step (1)：1~68：1.
Preferably, the molar ratio of butyl titanate and silver acetate is 1 in step (2)：2~1：5.
Preferably, the washing methods in step (2) is：Absolute ethyl alcohol and water washing are used successively.
Preferably, the drying temperature in step (2) is 60~80 DEG C, and drying time is 6~8 hours.
Preferably, a diameter of 5-20nm of the fiber of the fibrous silver orthophosphate-titanium dioxide composite photocatalyst, length
For 500-1000nm.
The present invention also provides the fibrous silver orthophosphate-titanic oxide composite photochemical catalysts obtained according to above-mentioned preparation method
Agent.
The present invention also provides obtain fibrous silver orthophosphate-titanium dioxide composite photocatalyst according to above-mentioned preparation method
Application in photocatalytic degradation rhodamine B.
Compared with prior art, technical scheme of the present invention has the advantages that：
(1) successfully synthesize fibrous silver orthophosphate-titanium dioxide composite photocatalyst, which combines dioxy simultaneously
Change the photo absorption property of titanium and silver orthophosphate, its light-catalysed activity of significant increase；
(2) preparation method is simple, at low cost, energy conservation and environmental protection and no coupling product；
(3) obtain silver orthophosphate-titanium dioxide composite photocatalyst be novel fibrous structure, photocatalytic activity compared with
It is high.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, and in order to allow the above and other objects, features and advantages of the present invention can
It is clearer and more comprehensible, below in conjunction with preferred embodiment, and coordinates attached drawing, detailed description are as follows.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 gained silver orthophosphate of embodiment-titanium dioxide composite photocatalyst；
Fig. 2 be 1 gained photochemical catalyst 1 of embodiment catalytic condition under and the decomposition without rhodamine B under catalysts conditions
Journey, wherein ordinate rhodamine B concentration ratio are the ratio of the concentration and rhodamine B initial concentration of different moments rhodamine B.
Specific implementation mode
Below will by specific embodiment, the present invention is further elaborated, but be not intended to limit the invention.
Embodiment 1
A kind of preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst, includes the following steps：
(1) 0.002mol silver acetates and 40 μ L are sequentially added in the poly-vinyl alcohol solution of a concentration of 2mol/L of 40ml,
The phosphate aqueous solution (phosphate aqueous solution density is 1.685g/ml) of 85wt%, the pH to 5.5 of solution is adjusted with methenamine,
It is reacted under stirring；
(2) step (1) after reaction, into gained mixture be added 0.001mol butyl titanates, with 10% it is dilute
The pH of nitre acid-conditioning solution is 3, is reacted 3 hours in the case where temperature is 75 DEG C of water bath condition, centrifuging and taking precipitation, successively with anhydrous second
Alcohol and water washs, and catalyst 1 is obtained after 60 DEG C of dry 8h.
Embodiment 2
A kind of preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst, which is characterized in that including walking as follows
Suddenly：
(1) 0.006mol silver acetates and 60 μ L are sequentially added in the poly-vinyl alcohol solution of a concentration of 2mol/L of 60ml,
85wt% phosphate aqueous solutions adjust pH to 5, are reacted under stirring；The substance for adjusting pH is methenamine；
(2) step (1) after reaction, into gained mixture be added 0.002mol butyl titanates, with 10% it is dilute
The pH of nitre acid-conditioning solution is 2, is reacted 3 hours in the case where temperature is 80 DEG C of water bath condition, centrifuging and taking precipitation, successively with anhydrous second
Alcohol and water washs, and catalyst 2 is obtained after dry 8h under the conditions of 70 DEG C.
Embodiment 3
A kind of preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst, which is characterized in that including walking as follows
Suddenly：
(1) 0.008mol silver acetates and 100 μ L are sequentially added in the poly-vinyl alcohol solution of a concentration of 2mol/L of 80ml,
85wt% phosphate aqueous solutions adjust pH value of solution to 6 with methenamine, are reacted under stirring；
(2) step (1) after reaction, into gained mixture be added 0.004mol butyl titanates, with 10% it is dilute
Nitre acid for adjusting pH is 4, is reacted 4 hours in the case where temperature is 80 DEG C of water bath condition, and centrifuging and taking precipitation uses absolute ethyl alcohol and water successively
It washs, catalyst 3 is obtained after dry 8h under the conditions of 70 DEG C.
Embodiment 4
A kind of preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst, which is characterized in that including walking as follows
Suddenly：
(1) 0.02mol silver acetates, 200uL are sequentially added in the poly-vinyl alcohol solution of a concentration of 2mol/L of 100ml,
85wt% phosphate aqueous solutions adjust pH value of solution to 5.5 with methenamine, are reacted under stirring；
(2) step (1) after reaction, into gained mixture be added 0.004mol butyl titanates, with 10% it is dilute
Nitre acid for adjusting pH is 3, is reacted 2 hours in the case where temperature is 75 DEG C of water bath condition, and centrifuging and taking precipitation uses absolute ethyl alcohol and water successively
It washs, catalyst 4 is obtained after dry 8h under the conditions of 70 DEG C.
Application Example 1
Using catalyst degradation rhodamine B obtained by embodiment 1-4.
0.1g catalyst 1,2,3,4 is weighed respectively, and is added separately in 200mL rhodamine B solutions (10~20mg/L),
It is protected from light stirring half an hour, rhodamine B solution is made to reach absorption/desorption equilibrium in catalyst surface.It is then turned on light source and carries out light
Catalysis reaction, takes 5ml reaction solutions, after being centrifuged, supernatant is taken to be detected with spectrophotometer at intervals of two minutes.The light of reaction
Source is xenon lamp, through UV filters optical filter, to ensure incident light as visible light (420nm ﹤ λ ﹤ 800nm).Wherein photochemical catalyst 1
The case where being catalyzed rhodamine B degradation is as shown in Figure 2.Figure it is seen that when not adding catalyst, rhodamine B shows minimum
Degradation trend, and after photochemical catalyst 1 of the present invention is added, rhodamine B is substantially completely degraded in 10 minutes, display institute of the present invention
Obtain good result of the fibrous silver orthophosphate-titanium dioxide composite photocatalyst in photocatalytic degradation rhodamine B.Catalyst 2,3,
4 effect in terms of being catalyzed rhodamine B degradation is also fine.
In conclusion the present invention successfully synthesizes silver orthophosphate-titanium dioxide composite photocatalyst, the catalyst is comprehensive simultaneously
The photo absorption property of titanium dioxide and silver orthophosphate, its light-catalysed activity of significant increase.In addition, preparation method letter of the present invention
Single, at low cost, energy conservation and environmental protection and no coupling product.Using the method for the present invention, obtaining silver orthophosphate-titanium dioxide composite photocatalyst is
Novel fibrous structure, photocatalytic activity are higher.
The above is the preferred embodiment of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, it is noted that for those skilled in the art, without departing from the principle of the present invention, may be used also
To make several improvement and variation, these are improved and variation is also considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst, which is characterized in that including walking as follows
Suddenly：
(1) silver acetate, phosphate aqueous solution are sequentially added in poly-vinyl alcohol solution, and pH to 5-6 is adjusted using methenamine, is being stirred
It mixes and is reacted under state；
(2) butyl titanate is added into the mixture obtained by step (1), adjusting pH is 2-4, the water for being 70-80 DEG C in temperature
Heating reaction 2-4 hours under the conditions of bath, centrifuging and taking precipitation, washing, up to silver orthophosphate-titanic oxide composite photochemical catalyst after drying
Agent.
2. the preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst according to claim 1, feature exist
In：The pH adjusting agent used in step (2) is dust technology.
3. the preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst according to claim 1, feature exist
In：The molar ratio of silver acetate and phosphoric acid in phosphate aqueous solution is 7 in step (1):1~3:1.
4. the preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst according to claim 1, feature exist
In：The molar ratio of polyvinyl alcohol and phosphoric acid is 137 in step (1)：1~68：1.
5. the preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst according to claim 1, feature exist
In：The molar ratio of butyl titanate and silver acetate is 1 in step (2)：2~1：5.
6. the preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst according to claim 1, feature exist
In：Washing methods in step (2) is：Absolute ethyl alcohol and water washing are used successively.
7. the preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst according to claim 1, feature exist
In：Drying temperature in step (2) is 60~80 DEG C, and drying time is 6~8 hours.
8. the preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst according to claim 1, feature exist
In：The a diameter of 5-20nm, length 500- of the fiber of the threadiness silver orthophosphate-titanium dioxide composite photocatalyst
1000nm。
9. fibrous silver orthophosphate-titanic oxide composite photochemical catalyst that a kind of any one of claim 1-8 the methods are prepared
Agent.
10. fibrous silver orthophosphate-titanium dioxide composite photocatalyst described in a kind of claim 9 is in photocatalytic degradation rhodamine
Application in B.
Priority Applications (1)
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