CN113333013A - 一种Ag3PO4-CoFe2O4/g-C3N4复合高效光催化剂及其制备方法 - Google Patents
一种Ag3PO4-CoFe2O4/g-C3N4复合高效光催化剂及其制备方法 Download PDFInfo
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- CN113333013A CN113333013A CN202110695767.0A CN202110695767A CN113333013A CN 113333013 A CN113333013 A CN 113333013A CN 202110695767 A CN202110695767 A CN 202110695767A CN 113333013 A CN113333013 A CN 113333013A
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- 229910002518 CoFe2O4 Inorganic materials 0.000 title claims abstract description 70
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910000161 silver phosphate Inorganic materials 0.000 claims abstract description 49
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 45
- 239000000243 solution Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 37
- 239000004005 microsphere Substances 0.000 claims abstract description 36
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 27
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 26
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000004793 Polystyrene Substances 0.000 claims abstract description 24
- 229920002223 polystyrene Polymers 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 13
- 239000000839 emulsion Substances 0.000 claims abstract description 13
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000010452 phosphate Substances 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000000034 method Methods 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
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 5
- 150000001868 cobalt Chemical class 0.000 claims abstract description 5
- 150000002505 iron Chemical class 0.000 claims abstract description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims abstract description 3
- 239000002244 precipitate Substances 0.000 claims abstract 4
- 239000002994 raw material Substances 0.000 claims abstract 2
- 230000015572 biosynthetic process Effects 0.000 claims description 40
- 238000003786 synthesis reaction Methods 0.000 claims description 40
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 11
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 7
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 7
- -1 FeCl)3·6H2O Chemical class 0.000 claims description 6
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 6
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 5
- 229940044175 cobalt sulfate Drugs 0.000 claims description 5
- 229910003321 CoFe Inorganic materials 0.000 claims description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 4
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 229960002089 ferrous chloride Drugs 0.000 claims description 2
- 229910001448 ferrous ion Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 235000011008 sodium phosphates Nutrition 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 239000012065 filter cake Substances 0.000 description 36
- 239000008367 deionised water Substances 0.000 description 18
- 229910021641 deionized water Inorganic materials 0.000 description 18
- 238000003756 stirring Methods 0.000 description 17
- 239000000126 substance Substances 0.000 description 12
- 238000001914 filtration Methods 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- 238000005303 weighing Methods 0.000 description 9
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 238000004064 recycling Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000004098 Tetracycline Substances 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 2
- 229940019931 silver phosphate Drugs 0.000 description 2
- 229960002180 tetracycline Drugs 0.000 description 2
- 229930101283 tetracycline Natural products 0.000 description 2
- 235000019364 tetracycline Nutrition 0.000 description 2
- 150000003522 tetracyclines Chemical class 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910017677 NH4H2 Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- NNGHIEIYUJKFQS-UHFFFAOYSA-L hydroxy(oxo)iron;zinc Chemical compound [Zn].O[Fe]=O.O[Fe]=O NNGHIEIYUJKFQS-UHFFFAOYSA-L 0.000 description 1
- ZMFWDTJZHRDHNW-UHFFFAOYSA-N indium;trihydrate Chemical compound O.O.O.[In] ZMFWDTJZHRDHNW-UHFFFAOYSA-N 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 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 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 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 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- 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
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B01J35/39—
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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- 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
- B01J37/346—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 microwave 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
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- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
本发明提供一种Ag3PO4‑CoFe2O4/g‑C3N4复合高效光催化剂及其制备方法。其特征在于：将中空Ag3PO4微球、CoFe2O4和g‑C3N4三者混合球磨后放入管式炉中在通氮气条件下煅烧一定时间，即可得到所需目标产物Ag3PO4‑CoFe2O4/g‑C3N4。所采取的技术方案是：先分别合成中空Ag3PO4微球、CoFe2O4和g‑C3N4，即将硝酸银水溶液、聚苯乙烯乳液、磷酸盐或酸式磷酸盐水溶液混合，再将沉淀物于管式炉中煅烧除去聚苯乙烯后得到中空Ag3PO4微球；将铁盐和钴盐的乙醇水溶液用氨水调节pH至10～11后再将沉淀物干燥得到CoFe2O4；将三聚氰胺、硫脲和氯化铵于坩埚中混合研磨后再微波加热而得到g‑C3N4；最后将中空Ag3PO4微球、CoFe2O4和g‑C3N4按一定质量百分比混合并球磨后置于管式炉中，在通氮气条件下于400～600℃煅烧，得到H‑Ag3PO4‑CoFe2O4/g‑C3N4复合光催化剂。
Description
技术领域
本发明涉及一种Ag3PO4-CoFe2O4/g-C3N4复合高效光催化剂及其制备方法，属于光催化材料领域。
背景技术
磷酸银(Ag3PO4)具有良好的可见光响应能力，在自然光照射下有很高的光催化性能。由于其制备简单，环境友好，是光催化降解和光电化学领域最有应用前景的材料之一。但 Ag3PO4的自身稳定性较差，在光催化中易自蚀，即在光催化条件下，Ag3PO4逐渐变成单质Ag，最后完全变成单质Ag，导致Ag3PO4的稳定性和循环使用性能差，也难以得到回收利用。为提高Ag3PO4的稳定性和循环使用性能，不少研究工作者制备了Ag3PO4/AgX (X＝Cl，Br，I)，Ag3PO4/TiO2，Ag3PO4/SnO2，Ag3PO4/CeO2，Ag/Ag3PO4/TiO2，Ag3PO4/In(OH)3， A3PO4/氧化石墨烯(GO)，Ag3PO4/TiO2石墨烯，Ag3PO4/Fe3O4，Ag3PO4/GO/ZnFe2O4， Ag3PO4/C3N4，等复合光催化剂，这些复合光催化剂在一定程度上提高了Ag3PO4的稳定性和循环使用性能，但与纯Ag3PO4相比，光催化性能有所下降。另外，有的掺杂剂如氧化石墨烯(GO)的比表面积虽大，导电性能较好，能够有效地促进光生电子-空穴对的分离，但成本高，重复回收利用也十分困难。再者，这些复合光催化剂很多采用高温水热法或高温溶剂热法或者溶胶凝胶法制备，受设备条件限制，这些方法难以实现工业规模化生产。
类石墨烯g-C3N4能形成由三嗪环单元组成的高度离域的π共轭体系，具有理想的电子结构和稳定性。因此在可见光催化应用方面受到广泛的关注。但由于g-C3N4层间主要是通过弱范德华力相互作用，不利于电子的转移，从而导致了其光催化效率不高。
发明内容为克服现有磷酸银复合光催化剂及其制备方法的不足，本发明提供了一种 Ag3PO4-CoFe2O4/g-C3N4复合高效光催化剂及其制备方法。该发明申请首先分别合成中空Ag3PO4微球、CoFe2O4和g-C3N4，然后将三者混合球磨后放入管式炉中在通氮气条件下煅烧一定时间，即可得到所需目标产物Ag3PO4-CoFe2O4/g-C3N4。所采取的技术方案是：(1)中空Ag3PO4微球的合成：在带搅拌的500mL烧杯中加入一定浓度的硝酸银水溶液和一定量的固含量为10％的聚苯乙烯(模板剂)乳液，然后逐滴滴加一定浓度的磷酸盐或酸式磷酸盐水溶液，滴加完毕后继续反应0.5～1h后过滤，用去离子水洗涤滤饼3次，最后将滤饼置于 500℃管式炉中煅烧3～6h除去模板剂聚苯乙烯，即可得到金黄色的中空Ag3PO4微球，记为H-Ag3PO4；(2)CoFe2O4的合成：将一定量铁盐和钴盐(Fe/Co＝2∶1，物质的量之比)溶于100mL50％乙醇水溶液中，滴加1mol·L-1氨水溶液调节溶液的pH调至10～11，继续磁力搅拌1～2 h后过滤，用去离子水洗涤滤饼3次，将所得滤饼在120℃干燥1～2h，得到CoFe2O4；(3) g-C3N4的合成：称取一定量三聚氰胺、硫脲和氯化铵于坩埚中充分研磨混合后，放入微波炉中在800W功率下加热20～60min，得到g-C3N4样品；(4)H-Ag3PO4-CoFe2O4/g-C3N4的合成：将H-Ag3PO4微球、CoFe2O4和g-C3N4按一定质量百分比混合并球磨1～3h后置于管式炉中，通入氮气，于400～600℃煅烧2～5h，得到H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂。
如上所述的H-Ag3PO4的制备中，AgNO3的浓度为：0.1～0.3mol·L-1。
如上所述的H-Ag3PO4的制备中，所采用的固含量为10％聚苯乙烯乳液的使用量为硝酸银水溶液总体积的1.0～3.0％。
如上所述的H-Ag3PO4的制备中，所采用的磷酸盐或酸式磷酸盐为磷酸钠[Na3PO4]，磷酸铵[(NH4)3PO4]，磷酸氢二铵[(NH4)2HPO4]、磷酸二氢铵[NH4H2PO4]、磷酸氢二钠[Na2HPO4]、磷酸二氢钠[NaH2PO4]、磷酸氢二钾[K2HPO4]、磷酸二氢钾[KH2PO4]或者它们的混合物等，磷酸根(PO4 3-)浓度范围为：0.3～0.9mol·L-1。
如上所述的CoFe2O4的制备中，所采用的铁盐为氯化铁(FeCl3)、氯化亚铁(FeCl2)、硝酸铁[Fe(NO3)3]、硫酸铁[Fe2(SO4)3]或它们的水合盐(如FeCl3·6H2O，FeCl2·4H2O， Fe(NO3)3·9H2O，Fe2(SO4)3·9H2O)等，铁离子(Fe3+)或亚铁离子(Fe2+)浓度为0.1～0.5mol·L-1。
如上所述的CoFe2O4的制备中，所采用的钴盐为氯化钴(CoCl2)、硝酸钴[Co(NO3)2]、硫酸钴或它们的水合盐(如CoCl2·6H2O，Co(NO3)2·6H2O)，CoSO4·7H2O)，钴离子(Co2+) 的浓度为0.05～0.25mol·L-1。
如上所述的g-C3N4的合成中，三聚氰胺、硫脲和氯化铵的质量比为三聚氰胺∶硫脲∶氯化铵＝1∶1∶1～2。
如上所述的H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂的合成中，三者的质量分数分别为： H-Ag3PO4(15～30％)，CoFe2O4(5～20％)，g-C3N4(50～80％)。
本发明所制备的H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂具有优异的光催化性能。在固液比(即光催化剂质量/水溶液体积)为20mg/100mL，以模拟太阳光照射浓度为10mg/L亚甲基蓝的水溶液，照射时间3min时，脱色率达到99％以上，照射罗丹明B、或者甲基橙水溶液，照射时间30min时，脱色率达到90％以上，降解效果比纯Ag3PO4光催化剂好，没有观察到Ag3PO4变成单质Ag的自蚀现象。该光催化剂用于四环素废水降解时，模拟太阳光光照30min时，四环素去除率在90％以上。所制备的复合光催化剂经简单抽滤后即可回收，可循环使用10次。
具体实施方式
通过以下实施例进一步阐述本发明，但本发明不仅局限于以下实施例。
实施例1
(1)H-Ag3PO4微球的合成：在带搅拌的500mL烧杯中加入100mL0.1mol·L-1AgNO3水溶液和1.0mL固含量为10％的聚苯乙烯(模板剂)乳液，然后逐滴滴加0.3mol·L-1的Na3PO4水溶液，滴加完毕后继续反应0.5h后过滤，用去离子水洗涤滤饼3次，最后将滤饼置于500℃管式炉中煅烧3h除去模板剂聚苯乙烯，即可得到金黄色的H-Ag3PO4微球；(2)CoFe2O4的合成：在带搅拌的250mL烧杯中加入100mL 50％乙醇水溶液，然后加入0.2mol氯化铁和0.1mol氯化钴(Fe/Co＝2∶1，物质的量之比)，溶解完全后，滴加1mol·L-1氨水溶液调节溶液的pH至10～11，继续磁力搅拌1～2h后过滤，用去离子水洗涤滤饼3次，将所得滤饼在 120℃干燥1～2h，得到CoFe2O4；(3)g-C3N4的合成：称取20g三聚氰胺、20g硫脲和20 g氯化铵于坩埚中充分研磨混合后，放入微波炉中在800W功率下加热20min，得到g-C3N4样品；(4)H-Ag3PO4-CoFe2O4/g-C3N4的合成：将3.0g H-Ag3PO4微球、1.0g CoFe2O4和16.0 g-C3N4按一定质量百分比混合并球磨1h后置于管式炉中，通入氮气，于400～600℃煅烧2h，得到H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂。
实施例2
(1)H-Ag3PO4微球的合成：在带搅拌的500mL烧杯中加入100mL0.2mol·L-1AgNO3水溶液和2.0mL固含量为10％的聚苯乙烯(模板剂)乳液，然后逐滴滴加0.6mol·L-1的Na2HPO4水溶液，滴加完毕后继续反应0.5h后过滤，用去离子水洗涤滤饼3次，最后将滤饼置于500℃管式炉中煅烧3h除去模板剂聚苯乙烯，即可得到金黄色的H-Ag3PO4微球；
(2)CoFe2O4的合成：在带搅拌的250mL烧杯中加入100mL 50％乙醇水溶液，然后加入 0.2mol氯化铁和0.1mol氯化钴(Fe/Co＝2∶1，物质的量之比)，溶解完全后，滴加1mol·L-1氨水溶液调节溶液的pH至10～11，继续磁力搅拌1～2h后过滤，用去离子水洗涤滤饼3次，将所得滤饼在120℃干燥1～2h，得到CoFe2O4；(3)g-C3N4的合成：称取20g三聚氰胺、 20g硫脲和30g氯化铵于坩埚中充分研磨混合后，放入微波炉中在800W功率下加热30 min，得到g-C3N4样品；(4)H-Ag3PO4-CoFe2O4/g-C3N4的合成：将4.0g H-Ag3PO4微球、 2.0g CoFe2O4和14.0g-C3N4按一定质量百分比混合并球磨1.5h后置于管式炉中，通入氮气，于400～600℃煅烧3h，得到H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂。
实施例3
(1)H-Ag3PO4微球的合成：在带搅拌的500mL烧杯中加入100mL0.3mol·L-1AgNO3水溶液和3.0mL固含量为10％的聚苯乙烯(模板剂)乳液，然后逐滴滴加0.9mol·L-1的NaH2PO4水溶液，滴加完毕后继续反应1h后过滤，用去离子水洗涤滤饼3次，最后将滤饼置于500℃管式炉中煅烧3h除去模板剂聚苯乙烯，即可得到金黄色的H-Ag3PO4微球；(2) CoFe2O4的合成：在带搅拌的250mL烧杯中加入100mL50％乙醇水溶液，然后加入0.2mol 氯化铁和0.1mol硝酸钴(Fe/Co＝2∶1，物质的量之比)，溶解完全后，滴加1mol·L-1氨水溶液调节溶液的pH至10～11，继续磁力搅拌2h后过滤，用去离子水洗涤滤饼3次，将所得滤饼在120℃干燥1～2h，得到CoFe2O4；(3)g-C3N4的合成：称取20g三聚氰胺、20g硫脲和40g氯化铵于坩埚中充分研磨混合后，放入微波炉中在800W功率下加热60min，得到 g-C3N4样品；(4)H-Ag3PO4-CoFe2O4/g-C3N4的合成：将6.0g H-Ag3PO4微球、4.0g CoFe2O4和10.0g-C3N4按一定质量百分比混合并球磨1h后置于管式炉中，通入氮气，于400～600℃煅烧4h，得到H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂。
实施例4
(1)H-Ag3PO4微球的合成：在带搅拌的500mL烧杯中加入100mL0.2mol·L-1AgNO3水溶液和2.0mL固含量为10％的聚苯乙烯(模板剂)乳液，然后逐滴滴加0.6mol·L-1的 (NH4)2HPO4水溶液，滴加完毕后继续反应1h后过滤，用去离子水洗涤滤饼3次，最后将滤饼置于500℃管式炉中煅烧3h除去模板剂聚苯乙烯，即可得到金黄色的H-Ag3PO4微球；(2)CoFe2O4的合成：在带搅拌的250mL烧杯中加入100mL 50％乙醇水溶液，然后加入 0.2mol氯化铁和0.1mol氯化钴(Fe/Co＝2∶1，物质的量之比)，溶解完全后，滴加1mol·L-1氨水溶液调节溶液的pH至10～11，继续磁力搅拌2h后过滤，用去离子水洗涤滤饼3次，将所得滤饼在120℃干燥1～2h，得到CoFe2O4；(3)g-C3N4的合成：称取20g三聚氰胺、20 g硫脲和40g氯化铵于坩埚中充分研磨混合后，放入微波炉中在800W功率下加热60min，得到g-C3N4样品；(4)H-Ag3PO4-CoFe2O4/g-C3N4的合成：将6.0g H-Ag3PO4微球、4.0g CoFe2O4和10.0g-C3N4按一定质量百分比混合并球磨1h后置于管式炉中，通入氮气，于 400～600℃煅烧5h，得到H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂。
实施例5
(1)H-Ag3PO4微球的合成：在带搅拌的500mL烧杯中加入100mL0.2mol·L-1AgNO3水溶液和2.0mL固含量为1O％的聚苯乙烯(模板剂)乳液，然后逐滴滴加100mL0.6mol·L-1的(NH4)H2PO4水溶液，滴加完毕后继续反应1h后过滤，用去离子水洗涤滤饼3次，最后将滤饼置于500℃管式炉中煅烧3h除去模板剂聚苯乙烯，即可得到金黄色的H-Ag3PO4微球； (2)CoFe2O4的合成：在带搅拌的250mL烧杯中加入100mL 50％乙醇水溶液，然后加入 0.2mol氯化铁和0.1mol硫酸钴(Fe/Co＝2∶1，物质的量之比)，溶解完全后，滴加1mol·L-1氨水溶液调节溶液的pH至10～11，继续磁力搅拌2h后过滤，用去离子水洗涤滤饼3次，将所得滤饼在120℃干燥1～2h，得到CoFe2O4；(3)g-C3N4的合成：称取20g三聚氰胺、20 g硫脲和40g氯化铵于坩埚中充分研磨混合后，放入微波炉中在800W功率下加热60min，得到g-C3N4样品；(4)H-Ag3PO4-CoFe2O4/g-C3N4的合成：将6.0g H-Ag3PO4微球、4.0g CoFe2O4和10.0g-C3N4按一定质量百分比混合并球磨1h后置于管式炉中，通入氮气，于400～600℃煅烧4h，得到H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂。
实施例6
(1)H-Ag3PO4微球的合成：在带搅拌的500mL烧杯中加入100mL0.2mol·L-1AgNO3水溶液和2.0mL固含量为1O％的聚苯乙烯(模板剂)乳液，然后逐滴滴加100mL0.6mol·L-1的K2HPO4水溶液，滴加完毕后继续反应1h后过滤，用去离子水洗涤滤饼3次，最后将滤饼置于500℃管式炉中煅烧3小时除去模板剂聚苯乙烯，即可得到金黄色的H-Ag3PO4微球； (2)CoFe2O4的合成：在带搅拌的250mL烧杯中加入100mL 50％乙醇水溶液，然后加入 0.2mol硝酸铁和0.1mol氯化钴(Fe/Co＝2∶1，物质的量之比)，溶解完全后，滴加1mol·L-1氨水溶液调节溶液的pH至10～11，继续磁力搅拌2h后过滤，用去离子水洗涤滤饼3次，将所得滤饼在120℃干燥1～2h，得到CoFe2O4；(3)g-C3N4的合成：称取20g三聚氰胺、20 g硫脲和40g氯化铵于坩埚中充分研磨混合后，放入微波炉中在800W功率下加热60min，得到g-C3N4样品；(4)H-Ag3PO4-CoFe2O4/g-C3N4的合成：将6.0g H-Ag3PO4微球、4.0g CoFe2O4和10.0g-C3N4按一定质量百分比混合并球磨1h后置于管式炉中，通入氮气，于 400～600℃煅烧4h，得到H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂。
实施例7
(1)H-Ag3PO4微球的合成：在带搅拌的500mL烧杯中加入100mL0.2mol·L-1AgNO3水溶液和2.0mL固含量为10％的聚苯乙烯(模板剂)乳液，然后逐滴滴加50mL0.3mol·L-1的Na2HPO4水溶液和50mL0.3mol·L-1的NaH2PO4水溶液，滴加完毕后继续反应1h后过滤，用去离子水洗涤滤饼3次，最后将滤饼置于500℃管式炉中煅烧3h除去模板剂聚苯乙烯，即可得到金黄色的H-Ag3PO4微球；(2)CoFe2O4的合成：在带搅拌的250mL烧杯中加入 100mL 50％乙醇水溶液，然后加入0.1mol硫酸铁和0.1mol硫酸钴(Fe/Co＝2∶1，物质的量之比)，溶解完全后，滴加1mol·L-1氨水溶液调节溶液的pH至10～11，继续磁力搅拌2h后过滤，用去离子水洗涤滤饼3次，将所得滤饼在120℃干燥1～2h，得到CoFe2O4；(3)g-C3N4的合成：称取20g三聚氰胺、20g硫脲和40g氯化铵于坩埚中充分研磨混合后，放入微波炉中在800W功率下加热60min，得到g-C3N4样品；(4)H-Ag3PO4-CoFe2O4/g-C3N4的合成：将6.0g H-Ag3PO4微球、4.0gCoFe2O4和10.0g-C3N4按一定质量百分比混合并球磨1h后置于管式炉中，通入氮气，于400～600℃煅烧4h，得到H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂。
实施例8
(1)H-Ag3PO4微球的合成：在带搅拌的500mL烧杯中加入100mL0.2mol·L-1AgNO3水溶液和2.0mL固含量为10％的聚苯乙烯(模板剂)乳液，然后逐滴滴加50mL0.3mol·L-1的Na2HPO4水溶液和50mL0.3mol·L-1的NH4H2PO4水溶液，滴加完毕后继续反应1h后过滤，用去离子水洗涤滤饼3次，最后将滤饼置于500℃管式炉中煅烧3小时除去模板剂聚苯乙烯，即可得到金黄色的H-Ag3PO4微球；(2)CoFe2O4的合成：在带搅拌的250mL烧杯中加入100mL 50％乙醇水溶液，然后加入0.2mol氯化铁和0.1mol硫酸钴(Fe/Co＝2∶1，物质的量之比)，溶解完全后，滴加1mol·L-1氨水溶液调节溶液的pH至10～11，继续磁力搅拌2h后过滤，用去离子水洗涤滤饼3次，将所得滤饼在120℃干燥1～2h，得到CoFe2O4； (3)g-C3N4的合成：称取20g三聚氰胺、20g硫脲和30g氯化铵于坩埚中充分研磨混合后，放入微波炉中在800W功率下加热40min，得到g-C3N4样品；(4)H-Ag3PO4-CoFe2O4/g-C3N4的合成：将6.0g H-Ag3PO4微球、4.0gCoFe2O4和10.0g-C3N4按一定质量百分比混合并球磨 1h后置于管式炉中，通入氮气，于400～600℃煅烧4h，得到H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂。
Claims (8)
1.一种Ag3PO4-CoFe2O4/g-C3N4复合高效光催化剂及其制备方法，其特征在于：将中空Ag3PO4微球、CoFe2O4和g-C3N4三者混合球磨后放入管式炉中在通氮气条件下煅烧一定时间，即可得到所需目标产物Ag3PO4-CoFe2O4/g-C3N4。。所采取的技术方案是：先分别合成中空Ag3PO4微球、CoFe2O4和g-C3N4，即将硝酸银水溶液、聚苯乙烯乳液、磷酸盐或酸式磷酸盐水溶液混合，再将沉淀物于管式炉中煅烧除去聚苯乙烯后得到中空Ag3PO4微球；将铁盐和钴盐的乙醇水溶液用氨水调节pH至10～11后再将沉淀物干燥得到CoFe2O4；将三聚氰胺、硫脲和氯化铵于坩埚中混合研磨后再微波加热而得到g-C3N4；最后将中空Ag3PO4微球、CoFe2O4和g-C3N4按一定质量百分比混合并球磨后置于管式炉中，在通氮气条件下于400～600℃煅烧，得到H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂。
2.根据权利要求1所述的制备方法，其特征在于：如上所述的H-Ag3PO4的制备中，AgNO3的浓度为：0.1～0.3mol·L-1。
3.根据权利要求1所述的制备方法，其特征在于：如上所述的H-Ag3PO4的制备中，所采用的固含量为10％聚苯乙烯乳液的使用量为硝酸银水溶液总体积的1.0～3.0％。
4.根据权利要求1所述的制备方法，其特征在于：如上所述的H-Ag3PO4的制备中，所采用的磷酸盐或酸式磷酸盐为磷酸钠[Na3PO4]，磷酸铵[(NH4)3PO4]，磷酸氢二铵[(NH4)2HPO4]、磷酸二氢铵[NH4H2PO4]、磷酸氢二钠[Na2HPO4]、磷酸二氢钠[NaH2PO4]、磷酸氢二钾[K2HPO4]、磷酸二氢钾[KH2PO4]或者它们的混合物等，磷酸根(PO4 3-)浓度范围为：0.3～0.9mol·L-1。
5.根据权利要求1所述的制备方法，其特征在于：如上所述的CoFe2O4的制备中，所采用的铁盐为氯化铁(FeCl3)、氯化亚铁(FeCl2)、硝酸铁[Fe(NO3)3]、硫酸铁[Fe2(SO4)3]或它们的水合盐(如FeCl3·6H2O，FeCl2·4H2O，Fe(NO3)3·9H2O，Fe2(SO4)3·9H2O)等，铁离子(Fe3+)或亚铁离子(Fe2+)浓度为0.1～0.5mol·L-1。
6.根据权利要求1所述的制备方法，其特征在于：如上所述的CoFe2O4的制备中，所采用的钴盐为氯化钴(CoCl2)、硝酸钴[Co(NO3)2]、硫酸钴或它们的水合盐(如CoCl2·6H2O，Co(NO3)2·6H2O)，CoSO4·7H2O)，钴离子(Co2+)的浓度为0.05～0.25mol·L-1。
7.根据权利要求1所述的制备方法，其特征在于：如上所述的g-C3N4的合成中，三聚氰胺、硫脲和氯化铵的质量比为三聚氰胺∶硫脲∶氯化铵＝1∶1∶1～2。
8.根据权利要求1所述的制备方法，其特征在于：如上所述的H-Ag3PO4-CoFe2O4/g-C3N4复合光催化剂的合成中，三者的质量分数分别为：H-Ag3PO4(15～30％)，CoFe2O4(5～20％)，g-C3N4(50～80％)。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105601266A (zh) * | 2015-12-16 | 2016-05-25 | 同济大学 | 气液界面法制备磷酸银二维有序纳米网薄膜及其方法 |
| CN106542509A (zh) * | 2016-10-19 | 2017-03-29 | 张家港市东大工业技术研究院 | 一种高效制备类石墨烯氮化碳的方法 |
| CN111326810A (zh) * | 2018-12-13 | 2020-06-23 | 多氟多化工股份有限公司 | 光催化降解废旧锂离子电池极片中有机物的方法、极片中集流体和活性物质的回收方法 |
| CN111659450A (zh) * | 2020-07-13 | 2020-09-15 | 安徽汇泽通环境技术有限公司 | 一种Ag3PO4/g-C3N4@MoS2复合光催化材料及制备方法和应用 |
-
2021
- 2021-06-22 CN CN202110695767.0A patent/CN113333013A/zh active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105601266A (zh) * | 2015-12-16 | 2016-05-25 | 同济大学 | 气液界面法制备磷酸银二维有序纳米网薄膜及其方法 |
| CN106542509A (zh) * | 2016-10-19 | 2017-03-29 | 张家港市东大工业技术研究院 | 一种高效制备类石墨烯氮化碳的方法 |
| CN111326810A (zh) * | 2018-12-13 | 2020-06-23 | 多氟多化工股份有限公司 | 光催化降解废旧锂离子电池极片中有机物的方法、极片中集流体和活性物质的回收方法 |
| CN111659450A (zh) * | 2020-07-13 | 2020-09-15 | 安徽汇泽通环境技术有限公司 | 一种Ag3PO4/g-C3N4@MoS2复合光催化材料及制备方法和应用 |
Non-Patent Citations (4)
| Title |
|---|
| CHAO-SHENG ZHU ET AL: "Facile synthesis of porous Ag3PO4 particles and its application in MB wastewater degradation under visible light irradiation", ADVANCES IN ENGINEERING RESEARCH, pages 2 * |
| QIUSHI YANG ET AL.: "Engineering graphitic carbon nitride with expanded interlayer distance for boosting photocatalytic hydrogen evolution", CHINESE JOURNAL OF CATALYSIS, pages 2 * |
| 朱鹏飞等: "g-C3N4-Ag3PO4/Fe3O4磁性光催化剂的制备及性能研究", 应用化工, vol. 49, no. 9, pages 2202 - 2203 * |
| 陶虎春等: "磁性CoFe2O4/g-C3N4复合纳米材料对环丙沙星的光催化降解研究", 北京大学学报(自然科学版), vol. 57, no. 3, pages 1 * |
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