CN108187754A - A kind of support type Ag/Ag3PO4Photochemical catalyst and preparation method thereof - Google Patents
A kind of support type Ag/Ag3PO4Photochemical catalyst and preparation method thereof Download PDFInfo
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- CN108187754A CN108187754A CN201711457931.4A CN201711457931A CN108187754A CN 108187754 A CN108187754 A CN 108187754A CN 201711457931 A CN201711457931 A CN 201711457931A CN 108187754 A CN108187754 A CN 108187754A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 116
- 238000002360 preparation method Methods 0.000 title description 4
- 210000002268 wool Anatomy 0.000 claims abstract description 95
- 229910000161 silver phosphate Inorganic materials 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 230000009467 reduction Effects 0.000 claims abstract description 5
- 239000004332 silver Substances 0.000 claims abstract description 5
- 230000001678 irradiating effect Effects 0.000 claims abstract description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 34
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 230000015556 catabolic process Effects 0.000 claims description 20
- 238000006731 degradation reaction Methods 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000011941 photocatalyst Substances 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 239000000908 ammonium hydroxide Substances 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 5
- 235000019800 disodium phosphate Nutrition 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 239000001488 sodium phosphate Substances 0.000 claims description 5
- 235000010265 sodium sulphite Nutrition 0.000 claims description 5
- 239000003403 water pollutant Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 235000019388 lanolin Nutrition 0.000 claims description 3
- 238000009991 scouring Methods 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims 1
- 238000007654 immersion Methods 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000000356 contaminant Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 description 15
- 238000007146 photocatalysis Methods 0.000 description 14
- 238000004064 recycling Methods 0.000 description 9
- 238000006555 catalytic reaction Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 239000003344 environmental pollutant Substances 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite Substances 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
- B01J35/30—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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
-
- 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
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0217—Pretreatment of the substrate before coating
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/345—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of ultraviolet wave energy
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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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Abstract
The present invention relates to environmental contaminants processing technology fields, and in particular to a kind of support type Ag/Ag3PO4Photochemical catalyst, support type Ag/Ag3PO4Photochemical catalyst is by wool carrier and the Ag/Ag being carried on the wool carrier3PO4Photochemical catalyst forms.Support type Ag/Ag3PO4The method of photochemical catalyst, includes the following steps：Wool pre-processes；Prepare wool loaded Ag3PO4Photochemical catalyst；Prepare wool loaded Ag/Ag3PO4Photochemical catalyst：Pretreated wool is added to prepared wool loaded Ag3PO4Photochemical catalyst is filtered after impregnating 6~10h using filter paper；Reduction generates a small amount of elemental silver after irradiating 8~15min in the UV lamp, and wool loaded Ag/Ag is obtained after drying3PO4Photochemical catalyst.Prepared loaded Ag/Ag3PO4Photochemical catalyst has good catalytic activity, and recycles convenient and efficient；Wool is as loaded Ag/Ag3PO4The advantages of carrier of photochemical catalyst makes photochemical catalyst be provided simultaneously with floating type catalyst and loaded catalyst has very wide application prospect in water treatment field.
Description
Technical field
The present invention relates to environmental contaminants processing technology field more particularly to a kind of support type Ag/Ag3PO4Photochemical catalyst and
Preparation method.
Background technology
With the continuous aggravation of China's environmental pollution, develop novel environmental pollution substance treating method and be increasingly subject to people
Concern.Photocatalysis is a kind of advanced oxidation treatment technology, environmentally protective that last century late nineteen seventies gradually grow up
Treatment process, the pollutant being mainly used in degradation water.Photocatalytic pollutant degradation is compared with other pollution degradation technologies
Compared with, have many advantages, such as it is easy to operate, to the degradation of pollutant without selectivity, reaction condition is mild, reaction rate is fast.Therefore,
More and more scientists are dedicated to the research of photocatalysis reagent and photo catalysis reactor in the world.
Photochemical catalyst in the utilization of photocatalytic degradation water pollutant, mainly with floating type and support type this two
Kind.Floating type is that photochemical catalyst is evenly dispersed in solution, forms suspension, and catalyst is uniformly mixed with sewage at this time,
Sunlight can be made full use of, achievees the purpose that extraordinary photocatalytic pollutant degradation.But it recycles catalyst and compares
Difficulty, so as to limit practical application of the photocatalysis technology in water process.
Loaded catalyst is made on carrier for photocatalyst, it can be achieved that photochemical catalyst and the solid-liquid of reaction system point
From, but another aspect photocatalyst can cause the reduction of its specific surface area to these material surfaces, be urged so as to weaken light
Change ability.If using the suspension system of photochemical catalyst, photo-catalysis capability can be effectively improved in this way, however this photocatalysis
The recycling of agent is a problem.This allow for photochemical catalyst load and improve photo-catalysis capability between there is contradictions.
It solves the problems, such as above-mentioned, it is necessary to find a kind of carrying method of effective photochemical catalyst, realize the repetition of catalyst
It utilizes, and does not reduce the catalytic performance of photochemical catalyst as possible.
There is researcher by the surface of the materials such as photocatalyst to glass, aluminosilicate, quartz, zeolite, be made negative
The photochemical catalyst of load type realizes the cycling and reutilization of photochemical catalyst.But another aspect photochemical catalyst is fixed to these materials
Surface can cause the reduction of its specific surface area, so as to weaken photo-catalysis capability.If using the suspension system of photochemical catalyst, in this way
Photo-catalysis capability can be effectively improved, however the recycling of catalyst is a problem again.
Invention content
In order to solve the above-mentioned technical problem the present invention, provides a kind of support type Ag/Ag3PO4Photochemical catalyst, it is ensured that light
Catalyst has good catalytic activity, and recycling is convenient and efficient, can realize the recycling of photochemical catalyst.
In order to reach above-mentioned technique effect, the present invention includes following technical scheme：A kind of support type Ag/Ag3PO4Photocatalysis
Agent, the support type Ag/Ag3PO4Photochemical catalyst is by wool carrier and the Ag/Ag being carried on the wool carrier3PO4Light is urged
Agent forms.
It is a kind of to prepare above-mentioned support type Ag/Ag3PO4The method of photochemical catalyst, includes the following steps：
(1) wool pre-processes：The wool being collected into is cleaned, shredded after dry, degreasing it is spare；
(2) wool loaded Ag is prepared3PO4Photochemical catalyst；
(3) wool loaded Ag/Ag is prepared3PO4Photochemical catalyst：
Pretreated wool in step (1) is added in step (2) and prepares wool loaded Ag3PO4Photochemical catalyst, leaching
It is filtered after steeping 6~10h using filter paper；Reduction generates a small amount of elemental silver after irradiating 8~15min in the UV lamp, is obtained after drying
Wool loaded Ag/Ag3PO4Photochemical catalyst.
Further, in the step (1) wool pre-process the specific steps are：
1) wool being collected into distilled water is cleaned up, is dried simultaneously after the 1.5~3h that then flows back in ethanol solution
It shreds；
2) wool after being shredded in step 1) adds in KMnO4In the mixed solution of NaCl, stirred at 40~50 DEG C
10~15min, wool become dark-brown by white；
3) by treated in step 2), wool is added in the mixed solution of sodium sulfite and acetic acid, is stirred at 40~50 DEG C
10~15min is mixed, wool gradually becomes white from dark-brown；
4) by treated in step 3) wool grease scouring, it is dry after it is spare.
The wool pre-treatment step can carry out effective ungrease treatment to wool, and the lipid for avoiding containing in wool is to light
Reducing agent forms serious barrier, and degreasing effect is good and efficient.
Further, 5.00g wools are taken in the step (1)；KMnO in the step (1)4With the mixed solution of NaCl,
Its KMnO4A concentration of 3.00g/L, a concentration of 25.00g/L of NaCl；The mixed solution of the sodium sulfite and acetic acid, it is sub-
A concentration of 20.00g/L of sodium sulphate, a concentration of 10.00mol/L of acetic acid.
Further, the step (2) is specially：
It weighs silver nitrate to be dissolved in deionized water, after stirring 15~25min in the dark, it is treated to add in 1.00g
Wool is gradually added into a certain amount of ammonium hydroxide, and solution becomes white, continues dropwise addition ammonium hydroxide and obtains colourless transparent solution；
Disodium phosphate soln is added dropwise with constant pressure funnel, continues 3.5~4.5h of stirring, with deionized water and nothing
Water-ethanol intersection washes three times removal reactive ions, obtains photochemical catalyst wool loaded Ag3PO4。
Further, the silver nitrate that the step (2) weighs 0.60g is dissolved in the deionized water of 300.00mL；Use constant pressure
The 0.15mol/L disodium phosphate solns of 47.10mL are added dropwise in dropping funel.
Further, the Ag of wool load prepared in the step (2)3PO4Photochemical catalyst, load capacity 10%；It is described
It is 1.00g that wool is taken in step (2).Load capacity is 10% Ag/Ag3PO4Photochemical catalyst catalytic effect is best.
Preferably, the support type Ag/Ag3PO4Photochemical catalyst is applied to pollute in degradation water under conditions of being 4 in pH
Object.
In addition, the present invention provides a kind of above-mentioned support type Ag/Ag3PO4The application of photochemical catalyst, the support type Ag/
Ag3PO4Photocatalyst applications are in degradation water pollutant.
Using above-mentioned technical proposal, including following advantageous effect：Support type Ag/Ag provided by the present invention3PO4Photocatalysis
Agent using wool as carrier, has big specific surface area and good recycling characteristic, realizes Ag/Ag3PO4Photochemical catalyst
Immobilized recycling, loaded Ag/Ag3PO4Photochemical catalyst has good catalytic activity, and recycles convenient and efficient；Wool is as negative
Carry Ag/Ag3PO4The advantages of carrier of photochemical catalyst makes photochemical catalyst be provided simultaneously with floating type catalyst and loaded catalyst,
There is very wide application prospect in water treatment field.
Description of the drawings
Fig. 1 is the common Ag/Ag provided in embodiment 23PO4Photochemical catalyst and wool loaded Ag/Ag3PO4Photochemical catalyst
XRD spectra；
The common Ag/Ag that Fig. 2 is provided by embodiment 23PO4The SEM figures of photochemical catalyst；
Wool loaded Ag/Ag that Fig. 3 is provided by embodiment 23PO4The SEM figures of photochemical catalyst；
Fig. 4 is wool loaded Ag/Ag of different loads amount in embodiment 33PO4Photocatalyst for degrading rate
Relational graph at any time；
Fig. 5 is wool loaded Ag/Ag of different loads amount in embodiment 33PO4Photochemical catalyst kinetic curve；
Fig. 6 is wool loaded Ag/Ag in embodiment 43PO4Photochemical catalyst is in the catalysis degradation modulus figure of condition of different pH；
Fig. 7 is wool loaded Ag/Ag in embodiment 53PO4Photochemical catalyst is repeated 5 times light-catalysed degradation rate figure.
Specific embodiment
The present invention is described in further detail below by specific embodiment and with reference to attached drawing.
Embodiment 1：
Present embodiments provide a kind of support type Ag/Ag3PO4Photochemical catalyst, the support type Ag/Ag3PO4Photochemical catalyst
By wool carrier and the Ag/Ag being carried on the wool carrier3PO4Photochemical catalyst forms.
Above-mentioned support type Ag/Ag3PO4The preparation method of photochemical catalyst, includes the following steps：
Step S1, wool pre-processes：
(1) wool being collected into distilled water is cleaned up, is dried simultaneously after the 1.5~3h that then flows back in ethanol solution
It shreds；
(2) wool after being shredded in step (1) adds in 3.00g/L KMnO4With the mixed solution of 25.00g/L NaCl
In, 10~15min is stirred at 40~50 DEG C, wool becomes dark-brown by white；
(3) treated in step (2) wool is added in the mixing of 20.00g/L sodium sulfites and 10.00mol/L acetic acid
In solution, 10~15min is stirred at 40~50 DEG C, wool gradually becomes white from dark-brown；By treated in step (3)
It is spare after wool grease scouring, drying.
Step S2, wool loaded Ag is prepared3PO4Photochemical catalyst：
The silver nitrate for weighing 0.60g is dissolved in the deionized water of 300.00mL, is added in 1.00g wools, is stirred in the dark
After 15~25min, a certain amount of ammonium hydroxide is gradually added into, solution becomes white, continues dropwise addition ammonium hydroxide and obtains colourless transparent solution；
The 0.15mol/L disodium phosphate solns of 47.10mL are added dropwise with constant pressure funnel, continue stirring 3.5~
4.5h washes three times removal reactive ions with deionized water and absolute ethyl alcohol intersection, obtains photochemical catalyst wool loaded Ag3PO4, light
Catalyst wool loaded Ag3PO4Load capacity be 10%；
Step S3, wool loaded Ag/Ag is prepared3PO4Photochemical catalyst：
Take wool loaded Ag prepared in step S23PO4Photochemical catalyst restores after irradiating 8~15min in the UV lamp
A small amount of elemental silver is generated, the Ag/Ag of the wool load of different loads amount is obtained after drying3PO4Photochemical catalyst.
In the present embodiment, the support type Ag/Ag3PO4Photochemical catalyst is applied to dirty in degradation water under conditions of being 4 in pH
Contaminate object.
Embodiment 2：
Wool loaded Ag/Ag that the present embodiment will be prepared in embodiment 13PO4Photochemical catalyst and common Ag/Ag3PO4Light
The characterization and catalytic effect of catalyst are compared：
Refering to Fig. 1, a is wool loaded Ag/Ag3PO4Photochemical catalyst, b are common Ag/Ag3PO4Photochemical catalyst, can by figure
See the position of each diffraction maximum, relative intensity, Ag3PO4It coincide (JCPDS 06-0505) with standard spectrogram, it was demonstrated that product is
Ag3PO4；In 42.5 and 61.8 characteristic diffraction peak for silver-colored simple substance, show there is the presence of elemental silver in the catalyst really, from a, b
Visible each peak position does not change in comparison diagram, illustrates Ag/Ag before and after catalyst load3PO4Crystal form does not change.
Referring to Fig.2, Fig. 2 is Ag/Ag3PO4The SEM figures of photochemical catalyst, it can be seen from the figure that Ag/Ag3PO4Granular size
Than more uniform, grain size is 160nm or so, crystal perfection, soilless sticking, and favorable catalyst agent is uniformly carried on wool surfaces.The crystalline substance
The reason of body occurs be：The addition of ammonium hydroxide is to synthesizing Ag3PO4Crystal has played important auxiliary catalysis, is formed with [Ag (NH3)2]+
As presoma, the Ag in system+Can by with H+ and NH3Between neutralization reaction release, then with PO4 3-Reaction generation
Ag3PO4Crystal, Na2HPO4Ag can be controlled+Rate of release and Ag3PO4The growth rate of crystal, promotes Ag3PO4Crystal crystal face
Generation, the Ag of formation rule3PO4Structure.
Refering to Fig. 3, Fig. 3 is the wool loaded Ag/Ag prepared using liquid phase method3PO4The SEM figures of photochemical catalyst.It can from figure
To find out, Ag/Ag3PO4Photochemical catalyst is evenly distributed in the surface of wool, illustrates wool loaded Ag/Ag3PO4Photochemical catalyst
Effect is relatively good, reaches the expected requirement of experiment.
Embodiment 3：
The present embodiment is to support type Ag/Ag prepared in embodiment 13PO4Photochemical catalyst carries out catalysis degeneration experiment：
(1) load capacity that the method for using above-described embodiment 1 obtains when preparing wool as 1.00g is 1%, 5%, 10%,
20%th, 50% wool loaded Ag/Ag3PO4Catalyst；
(2) experiment tests and the load of different loads amount wool is added in forward reaction device using 50mL test tubes as reactor
Ag/Ag3PO4Photochemical catalyst；
(3) MB photocatalytic degradations are carried out under the irradiation of simulated visible light, using the xenon lamp of 800W as light source, by 50.00mL
Methylene blue (5.00mol/L) is placed in photo catalysis reactor；
(4) photocatalytic degradation experiment is carried out after being protected from light stirring 30min, illumination takes a small amount of solution to carry out centrifugation point per 10min
From, take supernatant measure MB solution absorbance, after 1 hour stop reaction.
(5) Ag/Ag of recycling wool load is filtered with Buchner funnel3PO4Photochemical catalyst.
Methylene blue weighs the photocatalysis performance of catalyst as a kind of representative dyestuff, and maximum absorption wave is a length of
664nm。
Refering to Fig. 4, wool loaded Ag/Ag of 1%, 5%, 10%, 20%, 50% load capacity of Fig. 43PO4Photochemical catalyst
Degradation rate, respectively 76.8%, 86.1%, 97.4%, 94.1%, 93.1%.Wherein 10% wool shows best catalysis
Effect, degradation rate 97.4%.Due to Ag/Ag3PO4The increase of load capacity, the catalyst loadings of wool surfaces become
Greatly, so as to improve photocatalysis efficiency；But work as Ag/Ag3PO4When load capacity is more than 10%, because catalyst is in wool surfaces
Mutually covering reduces the translucency of liquid so that the photochemical catalyst being irradiated by light and the catalytic amount being excited by light reduce.
So the efficiency of catalytic degradation is declined slightly.
According to First-order kinetics equation：
Draw time and In (C0/ C) relation function figure as shown in figure 5, comparing the size of slope, it is evident that 10% sheep
Hair load silver orthophosphate shows maximum rate constant under visible light illumination.The wool load silver orthophosphate of different modifying load capacity
The rate constant of catalyst is as shown in the figure, 1%, 5%, 10%, 20%, 50% wool load silver orthophosphate light-catalyzed reaction rate is normal
Number is respectively 0.00848,0.05379,0.10128,0.05779,0.05136, wherein 10% load capacity catalytic rate is much larger than
Other load capacity, rate constant 0.10128.
Embodiment 4：
The present embodiment is to support type Ag/Ag prepared in embodiment 13PO4The pH conditions of photochemical catalyst are tested：Ginseng
Fig. 6 is read, MB solution was with the situation of change of pH value in the degradation rate of 60 minutes：Degradation rate highest when pH value is 4.0, in neutrality slightly
Difference, alkalinity are worst.This is because Ag/Ag3PO4The isoelectric point of photochemical catalyst in water is about in pH=5.1, when pH value is relatively low,
Ag/Ag3PO4Photocatalyst surface protonates, the Ag/Ag of protonation3PO4Photocatalyst surface carries positive charge；MB molecules are in water
It is ionized in solution so that MB groups are negatively charged, and electronegative MB groups are easy to close in positively charged catalyst surface.
On the other hand, the catalyst surface of protonation is positively charged, is conducive to light induced electron and is migrated to catalyst surface, with adsorption
Oxygen reaction, it is suppressed that electrons and holes it is compound, therefore increase photocatalytic activity.When pH value is higher, Ag/Ag3PO4Table
Face is negatively charged, is unfavorable for absorption of the electronegative MB groups in catalyst surface, while be also unfavorable for light induced electron to catalysis
The migration on agent surface is unfavorable for the progress of light-catalyzed reaction.
Embodiment 5：
The present embodiment is to support type Ag/Ag prepared in embodiment 13PO4The recycling performance of photochemical catalyst carries out real
It tests：By wool loaded Ag/Ag that load capacity is 1O%3PO4Photochemical catalyst carries out MB photocatalytic degradations, mistake at identical conditions
Filter recycling catalyst, the above-mentioned experimentation of repetition 5 times, and calculate degradation rate.
It refering to Fig. 7, is found in circulation experiment, wool loaded Ag/Ag3PO4The activity of photochemical catalyst is with number of repetition
Increase, degradation efficiency is declined slightly；60% catalytic effect can also be reached after reusing five times, therefore, wool loaded Ag/
Ag3PO4Photochemical catalyst not only has the ability of excellent catalytic degradation methylene blue, also recycles and reuses energy with good
Power can realize being used repeatedly for catalyst, and can also keep higher activity.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, that is made any repaiies
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of support type Ag/Ag3PO4Photochemical catalyst, which is characterized in that the support type Ag/Ag3PO4Photochemical catalyst is by wool
Carrier and the Ag/Ag being carried on the wool carrier3PO4Photochemical catalyst forms.
2. a kind of prepare support type Ag/Ag described in claim 13PO4The method of photochemical catalyst, which is characterized in that including as follows
Step：
(1) wool pre-processes：The wool being collected into is cleaned, is shredded after dry spare；
(2) wool loaded Ag is prepared3PO4Photochemical catalyst；
(3) wool loaded Ag/Ag is prepared3PO4Photochemical catalyst：
Pretreated wool in step (1) is added in step (2) and prepares wool loaded Ag3PO4Photochemical catalyst, immersion 6~
It is filtered after 10h using filter paper；Reduction generates a small amount of elemental silver after irradiating 8~15min in the UV lamp, and wool is obtained after drying and is born
Carry Ag/Ag3PO4Photochemical catalyst.
3. according to the method described in claim 2, it is characterized in that, in the step (1) wool pre-process the specific steps are：
1) wool being collected into distilled water is cleaned up, dries and shred after the 1.5~3h that then flows back in ethanol solution；
2) wool after being shredded in step 1) is added in the mixed solution of KMnO4 and NaCl, stir 10 at 40~50 DEG C~
15min, wool become dark-brown by white；
3) by treated in step 2), wool is added in the mixed solution of sodium sulfite and acetic acid, and 10 are stirred at 40~50 DEG C
~15min, wool gradually become white from dark-brown；
4) by treated in step 3) wool grease scouring, it is dry after it is spare.
4. according to the method described in claim 3, it is characterized in that, take 5.00g wools in the step (1)；The step (1)
Middle KMnO4With the mixed solution of NaCl, KMnO4A concentration of 3.00g/L, a concentration of 25.00g/L of NaCl；The sulfurous acid
The mixed solution of sodium and acetic acid, a concentration of 20.00g/L of sodium sulfite, a concentration of 10.00mol/L of acetic acid.
5. according to the method described in claim 4, it is characterized in that, the step (2) is specially：
It weighs silver nitrate to be dissolved in deionized water, adds in treated wool, after stirring 15~25min in the dark, gradually
A certain amount of ammonium hydroxide is added in, solution becomes white, continues dropwise addition ammonium hydroxide and obtains colourless transparent solution；
Disodium phosphate soln is added dropwise with constant pressure funnel, continues 3.5~4.5h of stirring, with deionized water and anhydrous second
Alcohol intersection washes three times removal reactive ions, obtains photochemical catalyst wool loaded Ag3PO4。
6. according to the method described in claim 5, it is characterized in that, the silver nitrate that the step (2) weighs 0.60g is dissolved in
300.00mL deionized water in；The treated wools of 1.00g are added in, are added dropwise 47.10mL's with constant pressure funnel
0.15mol/L disodium phosphate solns.
7. the method according to claim 1 or 6, which is characterized in that the wool load prepared in the step (2)
Ag3PO4Photochemical catalyst, load capacity 10%.
8. the method according to the description of claim 7 is characterized in that it is 1.00g that wool is taken in the step (3).
9. one kind support type Ag/Ag as described in claim 1~8 any one3PO4The application of photochemical catalyst, which is characterized in that
The support type Ag/Ag3PO4Photocatalyst applications are in degradation water pollutant.
10. support type Ag/Ag according to claim 93PO4The application of photochemical catalyst, which is characterized in that the support type Ag/
Ag3PO4Photochemical catalyst is applied to degradation water pollutant under conditions of being 4 in pH.
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| JP2009078211A (en) * | 2007-09-26 | 2009-04-16 | National Institute For Materials Science | Photocatalyst |
| CN103111334A (en) * | 2013-03-07 | 2013-05-22 | 西北师范大学 | Preparation method of photocatalyst containing double-promoting catalyst |
| CN106311292A (en) * | 2016-08-25 | 2017-01-11 | 闽南师范大学 | Ag/Ag3PO4 photocatalyst and preparing method and application thereof |
| CN106492854A (en) * | 2016-11-16 | 2017-03-15 | 陕西科技大学 | The composite nano Ag with photocatalysis performance is prepared using two-step method3PO4/TiO2Material and methods and applications |
| JP2017096967A (en) * | 2016-12-27 | 2017-06-01 | 二葉商事株式会社 | Method for manufacturing radioactive cesium adsorptive fabric |
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|---|---|---|---|---|
| JP2009078211A (en) * | 2007-09-26 | 2009-04-16 | National Institute For Materials Science | Photocatalyst |
| CN103111334A (en) * | 2013-03-07 | 2013-05-22 | 西北师范大学 | Preparation method of photocatalyst containing double-promoting catalyst |
| CN106311292A (en) * | 2016-08-25 | 2017-01-11 | 闽南师范大学 | Ag/Ag3PO4 photocatalyst and preparing method and application thereof |
| CN106492854A (en) * | 2016-11-16 | 2017-03-15 | 陕西科技大学 | The composite nano Ag with photocatalysis performance is prepared using two-step method3PO4/TiO2Material and methods and applications |
| JP2017096967A (en) * | 2016-12-27 | 2017-06-01 | 二葉商事株式会社 | Method for manufacturing radioactive cesium adsorptive fabric |
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