CN110227511A - A kind of preparation method of low temperature liquid phase precipitation method silver orthophosphate/graphene oxide visible-light photocatalyst - Google Patents
A kind of preparation method of low temperature liquid phase precipitation method silver orthophosphate/graphene oxide visible-light photocatalyst Download PDFInfo
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- CN110227511A CN110227511A CN201910617824.6A CN201910617824A CN110227511A CN 110227511 A CN110227511 A CN 110227511A CN 201910617824 A CN201910617824 A CN 201910617824A CN 110227511 A CN110227511 A CN 110227511A
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- Prior art keywords
- graphene oxide
- silver orthophosphate
- dyestuff
- light
- silver
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 84
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000001556 precipitation Methods 0.000 title claims abstract description 16
- 239000007791 liquid phase Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000011941 photocatalyst Substances 0.000 title claims description 23
- 239000000975 dye Substances 0.000 claims abstract description 79
- 230000001699 photocatalysis Effects 0.000 claims abstract description 49
- 239000003054 catalyst Substances 0.000 claims abstract description 44
- 238000007146 photocatalysis Methods 0.000 claims abstract description 40
- 230000015556 catabolic process Effects 0.000 claims abstract description 37
- 238000006731 degradation reaction Methods 0.000 claims abstract description 37
- 150000007524 organic acids Chemical class 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 25
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 22
- 238000005286 illumination Methods 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 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 description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 6
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 6
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 6
- 229940012189 methyl orange Drugs 0.000 claims description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical group CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 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 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- DNUYOWCKBJFOGS-UHFFFAOYSA-N 2-[[10-(2,2-dicarboxyethyl)anthracen-9-yl]methyl]propanedioic acid Chemical compound C1=CC=C2C(CC(C(=O)O)C(O)=O)=C(C=CC=C3)C3=C(CC(C(O)=O)C(O)=O)C2=C1 DNUYOWCKBJFOGS-UHFFFAOYSA-N 0.000 claims description 3
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 claims description 3
- KBIWNQVZKHSHTI-UHFFFAOYSA-N 4-n,4-n-dimethylbenzene-1,4-diamine;oxalic acid Chemical compound OC(=O)C(O)=O.CN(C)C1=CC=C(N)C=C1 KBIWNQVZKHSHTI-UHFFFAOYSA-N 0.000 claims description 3
- 239000005711 Benzoic acid Substances 0.000 claims description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 3
- 235000010233 benzoic acid Nutrition 0.000 claims description 3
- IJFXRHURBJZNAO-UHFFFAOYSA-N meta--hydroxybenzoic acid Natural products OC(=O)C1=CC=CC(O)=C1 IJFXRHURBJZNAO-UHFFFAOYSA-N 0.000 claims description 3
- 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 3
- 229940043267 rhodamine b Drugs 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims 1
- NFIYTPYOYDDLGO-UHFFFAOYSA-N phosphoric acid;sodium Chemical compound [Na].OP(O)(O)=O NFIYTPYOYDDLGO-UHFFFAOYSA-N 0.000 claims 1
- JBJWASZNUJCEKT-UHFFFAOYSA-M sodium;hydroxide;hydrate Chemical compound O.[OH-].[Na+] JBJWASZNUJCEKT-UHFFFAOYSA-M 0.000 claims 1
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 claims 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 18
- 238000010521 absorption reaction Methods 0.000 abstract description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 5
- 230000033228 biological regulation Effects 0.000 abstract description 5
- 229910052709 silver Inorganic materials 0.000 abstract description 5
- 239000004332 silver Substances 0.000 abstract description 5
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract description 3
- 239000003446 ligand Substances 0.000 abstract description 3
- AMHXQVUODFNFGR-UHFFFAOYSA-K [Ag+3].[O-]P([O-])([O-])=O Chemical group [Ag+3].[O-]P([O-])([O-])=O AMHXQVUODFNFGR-UHFFFAOYSA-K 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 229920002521 macromolecule Polymers 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 239000000463 material Substances 0.000 description 13
- 229910000161 silver phosphate Inorganic materials 0.000 description 13
- 239000002131 composite material Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 9
- 239000002351 wastewater Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 5
- 239000001048 orange dye Substances 0.000 description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 4
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 239000001045 blue dye Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000003760 hair shine Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- -1 papermaking Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- XRRQZKOZJFDXON-UHFFFAOYSA-N nitric acid;silver Chemical compound [Ag].O[N+]([O-])=O XRRQZKOZJFDXON-UHFFFAOYSA-N 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000003390 teratogenic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- 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
-
- 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
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 present invention prepares silver orthophosphate/graphene oxide photochemical catalyst using organic acid assistant regulating and controlling and the low temperature liquid phase precipitation method, utilize ligand complex and the graphene oxide π of organic acid and silver ion-cation sites regulation silver orthophosphate structure and pattern, the separation that photochemical catalyst promotes the absorption property and satisfactory electrical conductivity of dyestuff light induced electron and hole is improved using graphene oxide high-specific surface area, the absorption enrichment for realizing dyestuff and the absorption enriching-photocatalytic degradation of photocatalytic degradation act synergistically.Silver orthophosphate of the invention/preparation method is simple for graphene oxide photochemical catalyst, it is not necessary that macromolecule or surfactant is added.LED lamplight respectively reaches 85~99.5% and 38~51% according to photocatalysis dyestuff degradation rate of the 25min silver orthophosphate/graphene oxide photochemical catalyst to 10mg/L and 50mg/L dye solution, recycles 66~85% that rear photocatalysis dyestuff degradation rate is first time photocatalysis dyestuff degradation rate for 5 times.
Description
One, technical field
The present invention relates to a kind of preparation sides of low temperature liquid phase precipitation method silver orthophosphate/graphene oxide visible-light photocatalyst
Method, low temperature liquid phase precipitation method silver orthophosphate/graphene oxide visible-light photocatalyst prepared by the present invention are suitable for the visible of dyestuff
Light photocatalytic degradation can be widely applied to the fields such as visible light light degradation and the dye environment pollution control of dyestuff.
Two, background technique
Waste water from dyestuff is mainly derived from dye and dye intermediate production industry and weaving, leather, papermaking, rubber, plastics,
The different industries such as cosmetics, pharmacy and food, with complicated composition, water and change of water quality are big, coloration is high, COD and BOD concentration
High, the features such as suspended matter is more, recalcitrant substance is more, be one of industrial wastewater difficult to deal with.The annual output of China's dyestuff
About 150,000 tons, the 16.7%-18.7% of Zhan Quanqiu dyestuff annual output, wherein there is 10%~15% dyestuff producing and making
With can be discharged into environment in the process, these dyestuff majorities are extremely stable, into environment waters after be difficult to natural degradation, cause to get dirty
Contaminating waters oxygen content reduces, and it is incident to hinder light, and then influence the normal activities of aquatile, destroys the ecology of water body
Balance, more seriously dyestuff is mostly noxious material, has carcinogenic teratogenic effect, is discharged into the healthy structure in environment to the mankind
It is threatened at great, therefore dyeing waste water is all the reluctant industrial wastewater in various countries in the world for a long time, at environment-friendly high-efficiency
Reason waste water from dyestuff has become today's society great environmental problem urgently to be resolved.
The method of processing waste water from dyestuff mainly has chemistry, biology, physical method etc. at present.It is easy to operate to precipitate flocculence, at
This is low, but a large amount of sludge generated increase operation cost.Electricity is consumed when Treatment of Wastewater by Electrolysis and metal electrode amount is big.Photocatalysis
Oxidation is only good to low concentration waste water from dyestuff effect.The more single and microorganism of bioanalysis selectivity is environmentally sensitive.Absorption method operation
Simply, at low cost, effect is good, adsorbent is easily recycled.The active charcoal of common adsorbent, mineral, resinae adsorbent
Deng.Activated carbon adsorption power is strong, and removal rate is high, but at high cost, is normally only used for the lower treatment of dyeing wastewater of concentration or depth
Reason.Mineral include natural zeolite, bentonite etc., and ion-exchange capacity and absorption property are preferable, but activity is low, and regeneration is difficult.
And resinae adsorbent treatment effeciency is high, can regenerate under certain condition, can still keep efficiently, being suitable for waste water from dyestuff after regeneration
Processing, but higher cost.
Since Fujishima] find that TiO2 photocatalytic water is used to, conductor photocatalysis material starts to be widely used in ring
Border purification, wastewater treatment and solar energy conversion etc..TiO2 has photocatalytic activity height, stability good, cheap, less toxic
The advantages that property, but its band gap is larger, can only absorb ultraviolet light, can not efficiently use solar energy, significantly limits photocatalysis and answers
With therefore, people have been working hard the catalysis material found and have visible light absorption capacity.Ag3PO4 is a kind of novel, high
The visible-light response type semiconductor light-catalyst of effect, space structure are body-centered cubic, forbidden bandwidth 2.43ev, and Absorption edge reaches
To 530nm, the ultraviolet-visible light that sunlight medium wavelength is lower than 530nm can be absorbed, solar energy can be efficiently utilized, when shorter
It is interior that organic pollutant exhaustive oxidation is degraded, but Ag3PO4 solubility is bigger than normal, can generate corrosion by slightly soluble in water, reduce its knot
The stability of structure, conduction band positions (0.45e V) are corrected than hydrogen, and easy photoetch is reduced into silver-colored simple substance under illumination, and photolytic activity is lasting
Time is shorter, and photostability is poor, therefore how to improve the photocatalytic activity and light stabilization of such semiconductor visible light catalyst
Property become the hot spot studied at present.
Graphene oxide is a kind of with biggish specific surface area, higher chemical stability, stronger absorption property
Dimensional thinlayer carbon material, a large amount of hydrophilic functional groups in surface (hydroxyl, carboxyl, carbonyl etc.) can significantly improve prepared
The solubility to dispersion of composite material in a solvent, in addition, the negative electrical charge of its band can charge drive under the action of by band just
The metal ion of charge is effectively adsorbed on its surface, and only functional material does not provide largely in the growth of surface of graphene oxide
Active Growth point, and the nucleation of functional material and growth can also be controlled on the surface thereof, it is compound so as to Effective Regulation
The size and shape of material.Liang etc. is not under conditions of using surfactant, by the Ag+ of positive charge in solution and negative
Electrostatic interaction between the graphene oxide of charge makes Ag3PO4 nanometer spherical structure be deposited on thin graphene oxide layer
GO-Ag3PO4 nanocomposite is formed in structure, this composite material has stronger photocatalytic activity, excellent chemistry steady
Qualitative and preferable solubility to dispersion.The research not only shows that graphene oxide is a kind of excellent auxiliary material, is also system
Standby synthesis Ag3PO4 base composite photocatalyst material provides a kind of effective ways.Liu et al. has synthesized the nano combined material of GO-Ag3PO4
Material, the discovery biggish GO of specific surface area greatly improve the absorption property of composite material, and a large amount of organic dyestuff are adsorbed on composite wood
Surface is expected, so that the ability of its degradating organic dye (AO7) under visible light illumination significantly increases.After graphene oxide is added,
The photostability of composite material greatly improves.Cui and Yang etc. prepares graphene-phosphoric acid silver composite material using hydro-thermal method, sends out
Obtained graphene-phosphoric acid silver composite material is relative to not thermally treated graphene oxide-silver orthophosphate after existing hydro-thermal process
For composite material, the photocatalytic activity and photochemical stability of enhancing are shown under visible light illumination, it is anti-in photocatalysis
Multiple situation should be recycled and still show higher photocatalytic degradation efficiency and stability, the activity and stability of enhancing can
To be attributed to the fact that the electron mobility of the big specific surface area of grapheme material and high speed, so that fast after the light induced electron separation generated
Speed transfer, to substantially reduce the probability of light induced electron and hole-recombination and Ag+ is reduced into the several of simple substance Ag by light induced electron
Rate.Chen synthesizes Ag3PO4/GO composite photo-catalyst by liquid deposition.Ag3PO4/GO composite photocatalyst has dyestuff good
Good adsorptivity, improves photocatalysis efficiency.Simultaneously because GO outstanding conductive capability, can in time by electronics fast transfer,
Reduce the probability of light induced electron and hole-recombination, to improve the photocatalytic activity of catalysis material.Chang tree sides etc. are to aoxidize
Graphene (GO) is presoma, prepares GO/Ag2MoO4/Ag3PO4 tri compound conductor photocatalysis by the simple precipitation method
Agent, the photocatalysis performance of enhancing may be attributed to the ability that stannic oxide/graphene nano piece efficiently separated and shifted electron-hole pair.
Text etc. is opened using graphene oxide as carrier, and technological parameter is controlled using simple precipitation method, is prepared for GO/Ag3PO4 at room temperature
Nano-particles reinforcement photochemical catalyst, the Ag3PO4 nanoparticle size that is loaded of experiment discovery graphene surface is small, good dispersion,
Is firmly combined due to the excellent absorption property of graphene oxide and to the high mobility of carrier, GO/Ag3PO4 with graphene
Composite photo-catalyst shows higher visible light photocatalysis active and photostability, to the photocatalytic degradation efficiency of rhodamine B
It is improved by about one time compared with Ag3PO4 particle.
Correlative study shows that organic acid can form complex, regulation gold as co-ordination complex with metal cation
Belong to the rate of release of cation, to regulate and control the speed of growth of crystal nucleus, structure and pattern, is conducive to improve photochemical catalyst
Photocatalysis performance.Although silver orthophosphate/graphene oxide photochemical catalyst gets more and more extensive concerning of people and is increasingly becoming state
Inside and outside research hotspot, but at present both at home and abroad without preparing silver orthophosphate/graphene oxide photochemical catalyst using organic acid regulation
Research and report.
Three, summary of the invention
In view of this, the object of the invention is to be to provide a kind of low temperature liquid phase precipitation method silver orthophosphate/graphene oxide
The preparation method of visible-light photocatalyst.The present invention using organic acid assistant regulating and controlling and the low temperature liquid phase precipitation method prepare silver orthophosphate/
Graphene oxide photochemical catalyst is regulated and controled using ligand complex and the graphene oxide π of organic acid and silver ion-cation sites
The structure and pattern of silver orthophosphate improve photochemical catalyst to the absorption property of dyestuff and good using graphene oxide high-specific surface area
Good electric conductivity promotes the separation of light induced electron and hole, rich by the absorption enrichment of dyestuff and the absorption of visible light photocatalytic degradation
Collection-photocatalytic degradation synergistic effect, realize temperate condition under support type visible-light photocatalyst efficient degradation dyestuff, for efficiently,
Stable visible-light photocatalyst provides New methods in working.
Purpose according to the present invention proposes a kind of low temperature liquid phase precipitation method silver orthophosphate/graphene oxide visible light light and urges
The preparation method of agent, feature have following processing step:
A) silver nitrate and organic acid are dissolved in the mixed solution of alcohols solvent and deionized water composition, quality is then added
Volumetric concentration is the graphene oxide aqueous dispersions of 5mg/mL, and 25 DEG C of constant temperature stir 0.5~1.5h, and being eventually adding mass concentration is
10% biphosphate sodium water solution, 25~45 DEG C of constant temperature are stirred to react 1~5h, and reaction process mass concentration is 10%
It is 4~8 that NaOH aqueous solution, which adjusts reaction system pH, and product is centrifuged after reaction, with deionized water and anhydrous
It ethanol washing 3~5 times, is dried after centrifuge separation, grinds, obtain silver orthophosphate/graphene oxide visible-light photocatalyst；Nitric acid
Silver, sodium dihydrogen phosphate, graphene oxide, alcohols solvent and deionized water mass ratio be 0.5~2:0.5~2:0.005~
The molar ratio of 0.15:25~50:25~50, organic acid and silver nitrate is 1~2:1~2；
B) when 18~25min of white LED lamp illumination, silver orthophosphate/graphene oxide photochemical catalyst urges the light of dye solution
Change degradation and basically reach balance, when white LED lamp illumination 25min, silver orthophosphate/graphene oxide photochemical catalyst to 10mg/L with
The photocatalysis dyestuff degradation rate of 50mg/L dye solution respectively reaches 85~99.5% and 38~51%, recycles rear phosphorus 5 times
Sour silver/graphene oxide photochemical catalyst photocatalysis dyestuff degradation rate is the 66~85% of first time photocatalysis dyestuff degradation rate.
Organic acid of the present invention is selected from ethanedioic acid, malonic acid, benzoic acid, phthalic acid, terephthalic acid (TPA), isophthalic
Dioctyl phthalate, P-hydroxybenzoic acid, septichen and m-hydroxybenzoic acid.
Alcohols solvent of the present invention is selected from dehydrated alcohol, propyl alcohol, isopropanol, ethylene glycol and 1,3- propylene glycol.
White LED lamp power of the present invention is 20~30 watts, and service life 30,000~100,000 hour, colour temperature is 4500
Between~7000, formed by the yellow light combine that the blue light of wavelength 400~500 is sent out with the fluorescent powder being stimulated by blue light.
Dyestuff of the present invention is selected from methyl orange, methylene blue, crystal violet and rhodamine B.
Advantages of the present invention and effect are:
1) present invention prepares silver orthophosphate/graphene oxide photocatalysis using organic acid assistant regulating and controlling and the low temperature liquid phase precipitation method
Agent utilizes ligand complex and the graphene oxide π of organic acid and silver ion-cation sites regulation silver orthophosphate structure and shape
Looks improve photochemical catalyst using graphene oxide high-specific surface area and promote photoproduction to the absorption property and satisfactory electrical conductivity of dyestuff
The separation of electrons and holes is cooperateed with by the absorption enrichment of dyestuff with the degradation of the absorption enriching-photocatalytic of visible light photocatalytic degradation
Effect realizes support type visible-light photocatalyst efficient degradation dyestuff under temperate condition, is efficient, stable silver orthophosphate/oxidation
Graphene visible-light photocatalyst provides New methods in working.
2) silver orthophosphate of the invention/operation is simple for graphene oxide photochemical catalyst preparation method, low temperature or room temperature item
It is reacted under part, low energy consumption, and the reaction time is short.
3) silver orthophosphate of the invention/graphene oxide photochemical catalyst Photocatalytic Activity for Degradation dyestuff speed is fast, photocatalysis
Dyestuff degradation rate and recycling performance are high.
4) traditional visible light photocatalysis experiment uses xenon lamp for simulated visible light light source, and ultraviolet thermoradiation efficiency is larger,
Service life is shorter (1500~3000 hours).The present invention is using white LED lamp as simulated visible light light source, thermoradiation efficiency
Very low, service life is very long (30,000~100,000 hours), more green and environmental-friendly compared with xenon lamp.
Silver orthophosphate of the present invention/graphene oxide photochemical catalyst Photocatalytic Activity for Degradation dyestuff performance and circulation
Recycling utilization performance measurement method is as follows.
Taking 100mL mass concentration is the dye solution of 10~50mg/L, and addition dosage is 0.05~0.15g silver orthophosphate/oxygen
Graphite alkene photochemical catalyst, is placed on magnetic stirring apparatus and stirs evenly, and white LED lamp is used to carry out light for simulated visible light light source
Catalytic degradation dyestuff samples every 2~5min during light-catalyzed reaction, clear liquid is packed into cuvette after being filtered with filter, uses
Ultraviolet-uisible spectrophotometer tests its absorbance in dyestuff maximum absorption wavelength, investigates phosphoric acid by the variation of dye strength
Silver/graphene oxide photochemical catalyst dyestuff Photocatalytic Degradation Property.
Photocatalytic activity (Y) calculation formula of dyestuff is as follows:
Y=(C0-Ct)/C0× 100%
In formula: C0For the dyestuff initial concentration before dye solution light-catalyzed reaction；CtWhen for dye solution light-catalyzed reaction t
Between after dye strength.
After silver orthophosphate/graphene oxide photochemical catalyst photocatalytic degradation of dye is primary, silver orthophosphate/graphene oxide light is urged
Agent centrifuge separation is washed, dried recovered, carries out second of photocatalytic degradation of dye performance test, Zong Gongjin under the same terms
5 circulation experiments of row, and compared with first time photocatalytic degradation of dye performance, investigate silver orthophosphate/graphene oxide photocatalysis
The recycling performance of agent.
Four, specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is further explained, described reality
A part of the embodiment that example is only the present patent application is applied, instead of all the embodiments.Based on the implementation in the present patent application
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The scope of protection of the invention.
Embodiment 1:
1g silver nitrate and 0.8131g P-hydroxybenzoic acid are dissolved in the mixing of 50g dehydrated alcohol and 50g deionized water composition
In solution, the graphene oxide aqueous dispersions that 2mL mass-volume concentration is 5mg/mL are then added, 25 DEG C of constant temperature stir 0.5h,
It is eventually adding the biphosphate sodium water solution that 10g mass concentration is 10%, 45 DEG C of constant temperature are stirred to react 1h, reaction process quality
It is 4 that the NaOH aqueous solution that concentration is 10%, which adjusts reaction system pH, and product is centrifuged after reaction, uses deionization
Water and dehydrated alcohol wash 3 times, dry after centrifuge separation, grind, obtain silver orthophosphate/graphene oxide visible-light photocatalyst；
Silver orthophosphate/graphene oxide photochemical catalyst is basic to the photocatalytic degradation of Crystal Violet Dye solution when white LED lamp illumination 25min
Reach balance, when white LED lamp illumination 25min, silver orthophosphate/graphene oxide photochemical catalyst is to 10mg/L and 50mg/L crystal violet
The photocatalysis dyestuff degradation rate of dye solution respectively reaches 85% and 38%, recycles rear silver orthophosphate/graphene oxide light 5 times
The photocatalysis dyestuff degradation rate of catalyst is the 66% of first time photocatalysis dyestuff degradation rate.
Embodiment 2:
The mixing that 2g silver nitrate and 1.0841g m-hydroxybenzoic acid are dissolved in 50g ethylene glycol and 50g deionized water composition is molten
In liquid, the graphene oxide aqueous dispersions that 20mL mass-volume concentration is 5mg/mL are then added, 25 DEG C of constant temperature stir 1.5h, most
The biphosphate sodium water solution that 20g mass concentration is 10% is added afterwards, 25 DEG C of constant temperature are stirred to react 5h, and reaction process quality is dense
Degree is 8 for 10% NaOH aqueous solution adjusting reaction system pH, and product is centrifuged after reaction, uses deionized water
It washs 5 times with dehydrated alcohol, is dried after centrifuge separation, grind, obtain silver orthophosphate/graphene oxide photochemical catalyst；White LED lamp
When illumination 23min, silver orthophosphate/graphene oxide photochemical catalyst basically reaches the photocatalytic degradation of methylene blue dye solution flat
Weighing apparatus, when white LED lamp illumination 25min, silver orthophosphate/graphene oxide photochemical catalyst is to 10mg/L and 50mg/L methylene blue dye
The photocatalysis dyestuff degradation rate of solution respectively reaches 90% and 42.6%, recycles rear silver orthophosphate/graphene oxide light and urges for 5 times
The photocatalysis dyestuff degradation rate of agent is the 70% of first time photocatalysis dyestuff degradation rate.
Embodiment 3:
0.9g silver nitrate and 0.6098g septichen are dissolved in the mixed of 50g dehydrated alcohol and 40g deionized water composition
It closes in solution, the graphene oxide aqueous dispersions that 2.7mL mass-volume concentration is 5mg/mL, 25 DEG C of constant temperature stirrings is then added
1.5h, is eventually adding the biphosphate sodium water solution that 7.5g mass concentration is 10%, and 25 DEG C of constant temperature are stirred to react 2h, reaction process
It is 6 that the NaOH aqueous solution for being 10% with mass concentration, which adjusts reaction system pH, and product is centrifuged after reaction, is used
Deionized water and dehydrated alcohol wash 5 times, dry after centrifuge separation, grind, obtain silver orthophosphate/graphene oxide photochemical catalyst；
When white LED lamp illumination 18min, photocatalytic degradation base of the silver orthophosphate/graphene oxide photochemical catalyst to methyl orange dye solution
Originally reach balance, when white LED lamp illumination 25min, silver orthophosphate/graphene oxide photochemical catalyst is to 10mg/L and 50mg/L methyl
The photocatalysis dyestuff degradation rate of orange dye solution respectively reaches 99.5% and 51%, recycles rear silver orthophosphate/graphite oxide 5 times
The photocatalysis dyestuff degradation rate of alkene photochemical catalyst is the 85% of first time photocatalysis dyestuff degradation rate.
Embodiment 4:
1.35g silver nitrate and 0.8941g ethanedioic acid are dissolved in the mixed solution of 40g isopropanol and 50g deionized water composition
In, the graphene oxide aqueous dispersions that 5.4mL mass-volume concentration is 5mg/mL are then added, 25 DEG C of constant temperature stir 1.2h, most
The biphosphate sodium water solution that 16.2g mass concentration is 10% is added afterwards, 35 DEG C of constant temperature are stirred to react 1.5h, reaction process matter
Measure concentration be 10% NaOH aqueous solution adjust reaction system pH be 5, product is centrifuged after reaction, spend from
Sub- water and dehydrated alcohol wash 5 times, dry after centrifuge separation, grind, obtain silver orthophosphate/graphene oxide photochemical catalyst；White light
When LED lamplight shines 21min, silver orthophosphate/graphene oxide photochemical catalyst reaches the photocatalytic degradation of methyl orange dye solution substantially
To balance, when white LED lamp illumination 25min, silver orthophosphate/graphene oxide photochemical catalyst contaminates 10mg/L and 50mg/L methyl orange
The photocatalysis dyestuff degradation rate of material solution respectively reaches 96.5% and 48%, recycles rear silver orthophosphate/graphene oxide light 5 times
The photocatalysis dyestuff degradation rate of catalyst is the 79% of first time photocatalysis dyestuff degradation rate.
Embodiment 5:
0.5g silver nitrate and 0.3594g benzoic acid are dissolved in the mixed solution of 50g propyl alcohol and 40g deionized water composition,
Then the graphene oxide aqueous dispersions that 2.5mL mass-volume concentration is 5mg/mL are added, 25 DEG C of constant temperature stir 1.5h, finally plus
Enter the biphosphate sodium water solution that 7.5g mass concentration is 10%, 25 DEG C of constant temperature are stirred to react 2h, reaction process mass concentration
For 10% NaOH aqueous solution, to adjust reaction system pH be 6, and product is centrifuged after reaction, with deionized water and
Dehydrated alcohol washs 5 times, dries after centrifuge separation, grinds, obtains silver orthophosphate/graphene oxide visible-light photocatalyst；White light
When LED lamplight shines 22min, silver orthophosphate/graphene oxide photochemical catalyst basically reaches balance to the photocatalytic degradation of dye solution,
When white LED lamp illumination 25min, silver orthophosphate/graphene oxide photochemical catalyst urges the light of 10mg/L and 50mg/L dye solution
Change dyestuff degradation rate and respectively reach 94.8% and 47.6%, recycles rear silver orthophosphate/graphene oxide photochemical catalyst light 5 times
It is catalyzed 75% that dyestuff degradation rate is first time photocatalysis dyestuff degradation rate.
Embodiment 6:
0.96g silver nitrate and 0.9388g phthalic acid are dissolved in 30g 1,3- propylene glycol and 50g deionized water composition
In mixed solution, the graphene oxide aqueous dispersions that 3.8mL mass-volume concentration is 5mg/mL, 25 DEG C of constant temperature stirrings are then added
1.5h is eventually adding the biphosphate sodium water solution that 8g mass concentration is 10%, and 25 DEG C of constant temperature are stirred to react 2h, and reaction process is used
It is 6 that the NaOH aqueous solution that mass concentration is 10%, which adjusts reaction system pH, and product is centrifuged after reaction, spends
Ionized water and dehydrated alcohol wash 5 times, dry after centrifuge separation, grind, obtain silver orthophosphate/graphene oxide visible light photocatalysis
Agent；When white LED lamp illumination 20min, photocatalytic degradation of the silver orthophosphate/graphene oxide photochemical catalyst to methyl orange dye solution
Basically reach balance, when white LED lamp illumination 25min, silver orthophosphate/graphene oxide photochemical catalyst is to 10mg/L and 50mg/L first
The photocatalysis dyestuff degradation rate of base orange dye solution respectively reaches 97.6% and 50%, recycles rear silver orthophosphate/oxidation stone 5 times
The photocatalysis dyestuff degradation rate of black alkene photochemical catalyst is the 82% of first time photocatalysis dyestuff degradation rate.
Claims (5)
1. a kind of preparation method of low temperature liquid phase precipitation method silver orthophosphate/graphene oxide visible-light photocatalyst, it is characterised in that
There is following processing step:
A) silver nitrate and organic acid are dissolved in the mixed solution of alcohols solvent and deionized water composition, quality volume is then added
Concentration is the graphene oxide aqueous dispersions of 5mg/mL, and 25 °C of constant temperature stir 0.5~1.5h, and being eventually adding mass concentration is 10%
Biphosphate sodium water solution, 25~45 °C of constant temperature are stirred to react 1~5h, the NaOH water that reaction process mass concentration is 10%
It is 4~8 that solution, which adjusts reaction system pH, and product is centrifuged after reaction, is washed with deionized water and dehydrated alcohol
It washs 3~5 times, is dried after centrifuge separation, grind, obtain silver orthophosphate/graphene oxide visible-light photocatalyst；Silver nitrate, phosphoric acid
Sodium dihydrogen, graphene oxide, alcohols solvent and deionized water mass ratio be 0.5~2:0.5~2: 0.005~0.15:25
The molar ratio of~50:25~50, organic acid and silver nitrate is 1~2:1~2；
B) when 18~25min of white LED lamp illumination, the photocatalysis of dye solution drops in silver orthophosphate/graphene oxide photochemical catalyst
Solution basically reaches balance, and when white LED lamp illumination 25min, silver orthophosphate/graphene oxide photochemical catalyst is to 10mg/L and 50mg/L
The photocatalysis dyestuff degradation rate of dye solution respectively reaches 85~99.5% and 38~51%, recycles rear silver orthophosphate/oxidation 5 times
The photocatalysis dyestuff degradation rate of graphene photo-catalyst is the 66~85% of first time photocatalysis dyestuff degradation rate.
2. a kind of low temperature liquid phase precipitation method silver orthophosphate/graphene oxide visible-light photocatalyst according to claim 1
Preparation method, it is characterised in that: the organic acid is selected from ethanedioic acid, malonic acid, benzoic acid, phthalic acid, terephthaldehyde
Acid, M-phthalic acid, P-hydroxybenzoic acid, septichen and m-hydroxybenzoic acid.
3. a kind of low temperature liquid phase precipitation method silver orthophosphate/graphene oxide visible-light photocatalyst according to claim 1
Preparation method, it is characterised in that: the alcohols solvent is selected from dehydrated alcohol, propyl alcohol, isopropanol, ethylene glycol and 1,3- the third two
Alcohol.
4. a kind of low temperature liquid phase precipitation method silver orthophosphate/graphene oxide visible-light photocatalyst according to claim 1
Preparation method, it is characterised in that: the white LED lamp power is 20~30 watts, service life 30,000~100,000 hour, colour temperature
Between 4500~7000, formed by the yellow light combine that the blue light of wavelength 400 ~ 500 is sent out with the fluorescent powder being stimulated by blue light.
5. a kind of low temperature liquid phase precipitation method silver orthophosphate/graphene oxide visible-light photocatalyst according to claim 1
Preparation method, it is characterised in that: the dyestuff is selected from methyl orange, methylene blue, crystal violet and rhodamine B.
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Application publication date: 20190913 |