CN106268885A - A kind of preparation method of threadiness silver phosphate titanium dioxide composite photocatalyst - Google Patents
A kind of preparation method of threadiness silver phosphate titanium dioxide composite photocatalyst Download PDFInfo
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- CN106268885A CN106268885A CN201610562928.8A CN201610562928A CN106268885A CN 106268885 A CN106268885 A CN 106268885A CN 201610562928 A CN201610562928 A CN 201610562928A CN 106268885 A CN106268885 A CN 106268885A
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- titanium dioxide
- silver phosphate
- composite photocatalyst
- dioxide composite
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 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 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims abstract description 11
- 229940071536 silver acetate Drugs 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
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000003054 catalyst Substances 0.000 claims description 17
- 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
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 8
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229960004011 methenamine Drugs 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 239000003002 pH adjusting agent Substances 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 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
- 229940019931 silver phosphate Drugs 0.000 abstract description 10
- 229910000161 silver phosphate Inorganic materials 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 239000004408 titanium dioxide Substances 0.000 abstract description 4
- 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
- 239000000047 product Substances 0.000 abstract description 3
- 229940043267 rhodamine b Drugs 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 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
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium 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
- 239000004904 UV filter Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000019771 cognition Effects 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
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000008187 granular material 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
- 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
- 239000000376 reactant Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method Methods 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
- 238000001228 spectrum Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 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
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
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- 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)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention discloses the preparation method of a kind of threadiness silver phosphate titanium dioxide composite photocatalyst, comprise the steps: in polyvinyl alcohol water solution, be sequentially added into silver acetate, phosphate aqueous solution, regulate pH to 56, react under stirring；Adding butyl titanate in the mixture of gained, regulation pH is 24, reacting by heating 24 hours under the water bath condition that temperature is 70 80 DEG C, and centrifuging and taking precipitates, and washing the most i.e. obtains silver phosphate titanium dioxide composite photocatalyst.The present invention successfully synthesizes silver phosphate titanium dioxide composite photocatalyst, combines the photo absorption property of titanium dioxide and silver phosphate simultaneously, its light-catalysed activity of significant increase；Preparation method is simple, low cost, energy-conserving and environment-protective and no coupling product；The silver phosphate titanium dioxide composite photocatalyst obtained is novel filamentary structure, and its photocatalytic activity is higher.
Description
Technical field
The present invention relates to catalyst technical field, particularly relate to a kind of threadiness silver phosphate-titanic oxide composite photochemical catalyst
The preparation method of agent.
Background technology
Human society and sustainable economic development face energy shortage and ecological deterioration two large problems day by day, are at a high speed
The China of developmental stage, the most urgent to the research and development demand of clean energy resource and environmental protection technology.In theory, solar energy is utilized
Organic pollution in the amount preparing hydrogen energy and degraded environment is the desirable route solving the problems referred to above, and development correlation technique is with new
Material has bright prospects.
Japanese Scientists Fujishima in 1972 etc. find TiO2Monocrystalline electricity level can realize photochemical catalyzing, later
Find again nano-TiO2There is the organic ability of photocatalytic degradation so that it is become the focus material that scientist's gravity is paid close attention to.But
TiO2Sunlight absorb interval 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 about 1%, and utilization ratio is the lowest.
Silver phosphate, as a kind of brand-new conductor photocatalysis material, has good visible light-responded ability and outstanding
Photocatalytic degradation efficiency.In recent years silver phosphate has caused the extensive concern of various circles of society, is expected to become and realizes industrialized production and reality
The novel photocatalysis environment-friendly materials of border application.Show according to the study, its water decomposition performance under visible light illumination and organic coating
Decomposability is the decades of times of at present institute's cognition photocatalyst.The efficiency of silver phosphate photocatalysis degradation organic contaminant and crystal shape
Looks have certain relation, compared with random silver phosphate granule, have the silver phosphate photocatalyst of pattern to have more preferable organic dirt
Dye thing degradation efficiency.
But, silver phosphate and titanium dioxide are carried out compound with the two report of excellent properties in photoresponse comprehensive by present stage
Road is also little, and therefore, exploitation has the silver phosphate of special appearance and the compound photocatalyst of titanium dioxide to improve its photocatalysis
Activity and to seek easy environmentally friendly synthesis method significant for researcher.
Summary of the invention
Based on above the deficiencies in the prior art, technical problem solved by the invention is to provide a kind of threadiness phosphoric acid
The preparation method of silver-titanium dioxide composite photocatalyst, the method is simple, safety and environmental protection, the silver phosphate-titanium dioxide obtained
Titanium composite photo-catalyst novel structure, photocatalytic activity is high.
In order to solve 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 phosphate-titanium dioxide composite photocatalyst, comprises the steps:
(1) in poly-vinyl alcohol solution, it is sequentially added into silver acetate, phosphate aqueous solution, regulates pH to 5-6, under stirring
Reaction；
(2) adding butyl titanate in the mixture of step (1) gained, regulation pH is 2-4, is 70-80 DEG C in temperature
Water bath condition under reacting by heating 2-4 hour, centrifuging and taking precipitate, washing, the most i.e. obtain silver phosphate-titanium dioxide complex light and urge
Agent.
Preferably, the pH adjusting agent used in step (1) is hexamethylenamine, and the pH adjusting agent used in step (2) is dilute
Nitric acid.
Preferably, in step (1), silver acetate is 7:1～3:1 with the mol ratio of phosphoric acid in phosphate aqueous solution.
Preferably, in step (1), the mol ratio of polyvinyl alcohol and phosphoric acid is 137:1～68:1.
Preferably, in step (2), the mol ratio of butyl titanate and silver acetate is 1:2～1:5.
Preferably, the washing methods in step (2) is: successively with dehydrated alcohol and water washing.
Preferably, the baking 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 described threadiness silver phosphate-titanium dioxide composite photocatalyst, length
For 500-1000nm.
Present invention also offers the fibrous silver phosphate-titanic oxide composite photochemical catalyst obtained according to above-mentioned preparation method
Agent.
Present invention also offers and obtain threadiness silver phosphate-titanium dioxide composite photocatalyst according to above-mentioned preparation method
Application in photocatalytic degradation rhodamine B.
Compared with prior art, technical scheme has the advantages that
(1) successfully synthesizing threadiness silver phosphate-titanium dioxide composite photocatalyst, this catalyst combines dioxy simultaneously
Change titanium and the photo absorption property of silver phosphate, its light-catalysed activity of significant increase；
(2) preparation method is simple, low cost, energy-conserving and environment-protective and no coupling product；
(3) obtaining silver phosphate-titanium dioxide composite photocatalyst is novel filamentary structure, and its photocatalytic activity is relatively
High.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of description, and in order to allow the above and other objects, features and advantages of the present invention can
Become apparent, below in conjunction with preferred embodiment, and coordinate accompanying drawing, describe in detail as follows.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 1 gained silver phosphate-titanium dioxide composite photocatalyst；
Fig. 2 be embodiment 1 gained photocatalyst 1 catalytic condition under and without the decomposition of rhodamine B under catalysts conditions
Journey, wherein vertical coordinate rhodamine B concentration is than the concentration ratio with rhodamine B initial concentration being rhodamine B the most in the same time.
Detailed description of the invention
Below will by specific embodiment, the present invention is further elaborated, but not in order to limit the present invention.
Embodiment 1
The preparation method of a kind of threadiness silver phosphate-titanium dioxide composite photocatalyst, comprises the steps:
(1) in the poly-vinyl alcohol solution that 40ml concentration is 2mol/L, 0.002mol silver acetate and 40 μ L it are sequentially added into,
The phosphate aqueous solution (phosphate aqueous solution density is 1.685g/ml) of 85wt%, regulates the pH to 5.5 of solution with hexamethylenamine,
React under stirring；
(2) step (1) reaction terminate after, in gained mixture add 0.001mol butyl titanate, with 10% dilute
The pH of nitre acid-conditioning solution is 3, reacts 3 hours under the water bath condition that temperature is 75 DEG C, and centrifuging and taking precipitates, and uses anhydrous second successively
Alcohol and water washs, and obtains catalyst 1 after 60 DEG C of dry 8h.
Embodiment 2
The preparation method of a kind of threadiness silver phosphate-titanium dioxide composite photocatalyst, it is characterised in that include walking as follows
Rapid:
(1) in the poly-vinyl alcohol solution that 60ml concentration is 2mol/L, 0.006mol silver acetate and 60 μ L it are sequentially added into,
85wt% phosphate aqueous solution, regulates pH to 5, reacts under stirring；The material of regulation pH is hexamethylenamine；
(2) step (1) reaction terminate after, in gained mixture add 0.002mol butyl titanate, with 10% dilute
The pH of nitre acid-conditioning solution is 2, reacts 3 hours under the water bath condition that temperature is 80 DEG C, and centrifuging and taking precipitates, and uses anhydrous second successively
Alcohol and water washs, and obtains catalyst 2 after being dried 8h under the conditions of 70 DEG C.
Embodiment 3
The preparation method of a kind of threadiness silver phosphate-titanium dioxide composite photocatalyst, it is characterised in that include walking as follows
Rapid:
(1) in the poly-vinyl alcohol solution that 80ml concentration is 2mol/L, 0.008mol silver acetate and 100 μ L it are sequentially added into,
85wt% phosphate aqueous solution, with hexamethylenamine regulation pH value of solution to 6, reacts under stirring；
(2) step (1) reaction terminate after, in gained mixture add 0.004mol butyl titanate, with 10% dilute
Nitre acid for adjusting pH is 4, reacts 4 hours under the water bath condition that temperature is 80 DEG C, and centrifuging and taking precipitates, successively with dehydrated alcohol and water
Washing, obtains catalyst 3 after being dried 8h under the conditions of 70 DEG C.
Embodiment 4
The preparation method of a kind of threadiness silver phosphate-titanium dioxide composite photocatalyst, it is characterised in that include walking as follows
Rapid:
(1) in the poly-vinyl alcohol solution that 100ml concentration is 2mol/L, it is sequentially added into 0.02mol silver acetate, 200uL,
85wt% phosphate aqueous solution, with hexamethylenamine regulation pH value of solution to 5.5, reacts under stirring；
(2) step (1) reaction terminate after, in gained mixture add 0.004mol butyl titanate, with 10% dilute
Nitre acid for adjusting pH is 3, reacts 2 hours under the water bath condition that temperature is 75 DEG C, and centrifuging and taking precipitates, successively with dehydrated alcohol and water
Washing, obtains catalyst 4 after being dried 8h under the conditions of 70 DEG C.
Application Example 1
Use embodiment 1-4 gained catalyst degradation rhodamine B.
Weigh 0.1g catalyst 1,2,3,4 respectively, and be added separately in 200mL rhodamine B solution (10～20mg/L),
Lucifuge stirs half an hour, makes rhodamine B solution reach absorption/desorption equilibrium at catalyst surface.It is then turned on light source and carries out light
Catalytic reaction, takes 5ml reactant liquor at intervals of two minutes, after being performing centrifugal separation on, takes supernatant spectrophotometer and detects.The light of reaction
Source is xenon lamp, through UV filters optical filter, to guarantee that incident illumination is as visible ray (420nm λ 800nm).Wherein photocatalyst 1
The situation of catalysis rhodamine B degraded is as shown in Figure 2.During figure it is seen that do not add catalyst, rhodamine B demonstrates minimum
Degraded trend, and after adding photocatalyst 1 of the present invention, rhodamine B was substantially completely degraded in 10 minutes, showed institute of the present invention
Obtain fibrous silver phosphate-titanium dioxide composite photocatalyst good result in photocatalytic degradation rhodamine B.Catalyst 2,3,
4 effects in terms of catalysis rhodamine B degraded are the most fine.
In sum, the present invention successfully synthesizes silver phosphate-titanium dioxide composite photocatalyst, and this catalyst is the most comprehensive
The photo absorption property of titanium dioxide and silver phosphate, its light-catalysed activity of significant increase.It addition, preparation method of the present invention is simple
List, low cost, energy-conserving and environment-protective and no coupling product.Using the inventive method, obtaining silver phosphate-titanium dioxide composite photocatalyst is
Novel filamentary structure, its photocatalytic activity is higher.
The above is the preferred embodiment of the present invention, certainly can not limit the right model of the present invention with this
Enclose, it is noted that for those skilled in the art, under the premise without departing from the principles of the invention, also may be used
To make some improvement and variation, these improve and variation is also considered as protection scope of the present invention.
Claims (10)
1. the preparation method of fibrous silver phosphate-titanium dioxide composite photocatalyst, it is characterised in that include walking as follows
Rapid:
(1) in poly-vinyl alcohol solution, it is sequentially added into silver acetate, phosphate aqueous solution, regulates pH to 5-6, anti-under stirring
Should；
(2) adding butyl titanate in the mixture of step (1) gained, regulation pH is 2-4, is the water of 70-80 DEG C in temperature
Reacting by heating 2-4 hour under the conditions of bath, centrifuging and taking precipitates, and washing the most i.e. obtains silver phosphate-titanic oxide composite photochemical catalyst
Agent.
The preparation method of threadiness silver phosphate-titanium dioxide composite photocatalyst the most according to claim 1, its feature exists
In: the pH adjusting agent used in step (1) is hexamethylenamine, and the pH adjusting agent used in step (2) is dust technology.
The preparation method of threadiness silver phosphate-titanium dioxide composite photocatalyst the most according to claim 1, its feature exists
In: in step (1), silver acetate is 7:1～3:1 with the mol ratio of phosphoric acid in phosphate aqueous solution.
The preparation method of threadiness silver phosphate-titanium dioxide composite photocatalyst the most according to claim 1, its feature exists
In: in step (1), polyvinyl alcohol is 137:1～68:1 with the mol ratio of phosphoric acid.
The preparation method of threadiness silver phosphate-titanium dioxide composite photocatalyst the most according to claim 1, its feature exists
In: in step (2), butyl titanate is 1:2～1:5 with the mol ratio of silver acetate.
The preparation method of threadiness silver phosphate-titanium dioxide composite photocatalyst the most according to claim 1, its feature exists
In: the washing methods in step (2) is: successively with dehydrated alcohol and water washing.
The preparation method of threadiness silver phosphate-titanium dioxide composite photocatalyst the most according to claim 1, its feature exists
In: the baking temperature in step (2) is 60～80 DEG C, and drying time is 6～8 hours.
The preparation method of threadiness silver phosphate-titanium dioxide composite photocatalyst the most according to claim 1, its feature exists
In: a diameter of 5-20nm, a length of 500-of the fiber of described threadiness silver phosphate-titanium dioxide composite photocatalyst
1000nm。
9. fibrous silver phosphate-titanic oxide composite photochemical catalyst that method described in an any one of claim 1-8 prepares
Agent.
10. the fibrous silver phosphate-titanium dioxide composite photocatalyst described in a claim 9 is at photocatalytic degradation rhodamine
Application in B.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610562928.8A CN106268885B (en) | 2016-07-15 | 2016-07-15 | A kind of preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610562928.8A CN106268885B (en) | 2016-07-15 | 2016-07-15 | A kind of preparation method of threadiness silver orthophosphate-titanium dioxide composite photocatalyst |
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| Publication Number | Publication Date |
|---|---|
| CN106268885A true CN106268885A (en) | 2017-01-04 |
| CN106268885B CN106268885B (en) | 2018-10-26 |
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