CN113786825A - Nano nickel ferrite/zinc titanate modified microporous silicon oxide, preparation method and application thereof - Google Patents
Nano nickel ferrite/zinc titanate modified microporous silicon oxide, preparation method and application thereof Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 115
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 43
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 42
- 239000011701 zinc Substances 0.000 title claims abstract description 42
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 39
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 59
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 48
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 48
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 48
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 48
- 238000003756 stirring Methods 0.000 claims abstract description 45
- 239000002243 precursor Substances 0.000 claims abstract description 44
- 229910003122 ZnTiO3 Inorganic materials 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- 229910003264 NiFe2O4 Inorganic materials 0.000 claims abstract description 25
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 19
- 230000008021 deposition Effects 0.000 claims abstract description 15
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims abstract description 13
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 150000002815 nickel Chemical class 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000001632 sodium acetate Substances 0.000 claims abstract description 10
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 10
- 238000003980 solgel method Methods 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 239000011148 porous material Substances 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 238000009826 distribution Methods 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- UKDYPJBSLOCNRU-UHFFFAOYSA-J ethanol tetrachlorotitanium Chemical compound CCO.Cl[Ti](Cl)(Cl)Cl UKDYPJBSLOCNRU-UHFFFAOYSA-J 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 150000003751 zinc Chemical class 0.000 claims description 10
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- 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 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 229940123317 Sulfonamide antibiotic Drugs 0.000 claims description 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004246 zinc acetate Substances 0.000 claims description 5
- 239000011592 zinc chloride Substances 0.000 claims description 5
- 235000005074 zinc chloride Nutrition 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 4
- 230000000593 degrading effect Effects 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 4
- 229940078494 nickel acetate Drugs 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 4
- 229960001763 zinc sulfate Drugs 0.000 claims description 4
- 150000002505 iron Chemical class 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000001228 spectrum Methods 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 238000000151 deposition Methods 0.000 description 11
- 230000015556 catabolic process Effects 0.000 description 9
- 238000006731 degradation reaction Methods 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000011941 photocatalyst Substances 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- GWIJGCIVKLITQK-UHFFFAOYSA-N sodium;(4-aminophenyl)sulfonyl-(1,3-thiazol-2-yl)azanide Chemical compound [Na+].C1=CC(N)=CC=C1S(=O)(=O)[N-]C1=NC=CS1 GWIJGCIVKLITQK-UHFFFAOYSA-N 0.000 description 3
- 239000004016 soil organic matter Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000003911 water pollution Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229960005476 sulfathiazole sodium Drugs 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- TYMRLRRVMHJFTF-UHFFFAOYSA-N Mafenide Chemical compound NCC1=CC=C(S(N)(=O)=O)C=C1 TYMRLRRVMHJFTF-UHFFFAOYSA-N 0.000 description 1
- WMPXPUYPYQKQCX-UHFFFAOYSA-N Sulfamonomethoxine Chemical compound C1=NC(OC)=CC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 WMPXPUYPYQKQCX-UHFFFAOYSA-N 0.000 description 1
- NHUHCSRWZMLRLA-UHFFFAOYSA-N Sulfisoxazole Chemical compound CC1=NOC(NS(=O)(=O)C=2C=CC(N)=CC=2)=C1C NHUHCSRWZMLRLA-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- TVUBDAUPRIFHFN-UHFFFAOYSA-N dioxosilane;oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4].O=[Si]=O TVUBDAUPRIFHFN-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- SKIVFJLNDNKQPD-UHFFFAOYSA-N sulfacetamide Chemical compound CC(=O)NS(=O)(=O)C1=CC=C(N)C=C1 SKIVFJLNDNKQPD-UHFFFAOYSA-N 0.000 description 1
- 229960002673 sulfacetamide Drugs 0.000 description 1
- SEEPANYCNGTZFQ-UHFFFAOYSA-N sulfadiazine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CC=N1 SEEPANYCNGTZFQ-UHFFFAOYSA-N 0.000 description 1
- 229960004306 sulfadiazine Drugs 0.000 description 1
- 229960002135 sulfadimidine Drugs 0.000 description 1
- 229960000654 sulfafurazole Drugs 0.000 description 1
- ASWVTGNCAZCNNR-UHFFFAOYSA-N sulfamethazine Chemical compound CC1=CC(C)=NC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 ASWVTGNCAZCNNR-UHFFFAOYSA-N 0.000 description 1
- 229960005404 sulfamethoxazole Drugs 0.000 description 1
- 229950003874 sulfamonomethoxine Drugs 0.000 description 1
- 229940091629 sulfamylon Drugs 0.000 description 1
- JNMRHUJNCSQMMB-UHFFFAOYSA-N sulfathiazole Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CS1 JNMRHUJNCSQMMB-UHFFFAOYSA-N 0.000 description 1
- 229960001544 sulfathiazole Drugs 0.000 description 1
- JLKIGFTWXXRPMT-UHFFFAOYSA-N sulphamethoxazole Chemical compound O1C(C)=CC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 JLKIGFTWXXRPMT-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/08—Silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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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
- B01J23/755—Nickel
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Abstract
The invention discloses a nano nickel ferrite/zinc titanate modified microporous silicon oxideThe specific surface area of the microporous silicon oxide is 700-800m2(g) the particle size distribution range is 300-700nm, the average pore diameter is 1.2-1.3nm, and the SiO is spherical microporous2As a core, nano ZnTiO is sequentially grown in situ on the surface of the core3Nano NiFe2O4(ii) a The preparation method comprises the following steps: s1: synthesis of spherical microporous SiO by sol-gel method2(ii) a S2: deposition of ZnTiO3A precursor; s3: deposition of NiFe2O4Precursor: adding soluble ferric salt and soluble nickel salt into deionized water, stirring and dissolving, then adding sodium acetate and ZnTiO3Precursor modified microporous SiO2Stirring and dispersing, carrying out hydrothermal reaction at 130-200 ℃ for 10-18h, filtering and washing to obtain NiFe2O4/ZnTiO3Precursor modified microporous SiO2(ii) a S4: and (4) calcining. The invention utilizes the nano nickel ferrite and the nano zinc titanate to compound into a P-N type heterojunction, effectively improves the photocatalytic efficiency and the catalytic stability, and enlarges the spectrum absorption range.
Description
Technical Field
The invention belongs to the field of nano functional materials, and particularly relates to nano nickel ferrite/zinc titanate modified microporous silicon oxide, a preparation method and application thereof.
Background
Nano SiO2Is one of the new-generation inorganic materials with high utilization value, has small particle size and large specific surface area, and shows specific performance compared with general materials in the aspects of magnetism, catalysis, optical performance, electrical performance and the like, thereby gaining wide attention of people. At present, the preparation method of nano SiO2 comprises a physical method and a chemical method, wherein the physical method mainly comprises a superfine grinding machine and a combustion method, and the chemical method mainly comprises a chemical vapor deposition method, a chemical precipitation method, a microemulsion method and a sol-gel method. Nano SiO2The catalyst can be applied to a plurality of fields, in particular to the fields of catalysis, coating, color ink-jet printing, light, medicine carrying and agricultural production. Wherein, in the field of catalysis, SiO2Can be used as an excellent catalyst carrier, in particular to microporous nano SiO2Because the pore diameter is smaller and the pore wall is thicker, the catalyst carrier can ensure that the framework structure of the catalyst is not easy to collapse, improve the mechanical strength of the catalyst and simultaneously use SiO2The active metal particles are encapsulated as a mesoporous scaffold protective shell, the accessibility of active sites of the active metal particles can be higher, the encapsulation strategy has obvious effect on limiting the growth of the particles,the catalytic performance is greatly improved.
In recent years, in the aspect of pollution degradation and environmental restoration by sunlight, the photocatalyst compounded by the silicon oxide microspheres and the semiconductor material has a good application prospect. At present, the research on materials compounded by silicon oxide, titanium oxide and titanate is the most extensive, for example, patent application No. CN201611243082.8 discloses a nano titanium dioxide-silicon dioxide composite photocatalyst and a preparation method thereof, patent application No. CN201810888339.8 discloses a preparation method of a near-infrared responsive photocatalyst using porous silicon dioxide fiber as a carrier and a photocatalyst, patent application No. CN201810612084.2 discloses silica/titanium dioxide composite aerogel particles, a composition for forming the photocatalyst and the photocatalyst, patent application No. CN201811484282.1 discloses a titanium dioxide/silicon dioxide photocatalyst and a preparation method thereof, but because of ZnTiO3Forbidden band width of 3.65eV, TiO2The forbidden band width is 3.2eV, the catalytic activity is only realized under the ultraviolet radiation, the ultraviolet content in the sunlight is only 5%, the visible light in the sunlight cannot be utilized, and the further application of the catalyst is limited. In addition, when the photocatalytic material is applied to water pollution treatment and soil organic matter degradation, the photocatalytic material is difficult to recycle, so that resource waste is caused, and the excessive accumulation of the photocatalytic material can cause environmental damage and ecological system change. Therefore, how to prepare the composite photocatalytic material which is easy to separate and has high visible light catalytic activity is a technical problem to be solved urgently, and has important significance for popularizing photocatalytic degradation and environmental remediation.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a nano nickel ferrite/zinc titanate modified microporous silicon oxide, a preparation method and application thereof.
The technical scheme of the invention is summarized as follows:
the specific surface area of the nano nickel ferrite/zinc titanate modified microporous silicon oxide is 700-800m2(g) the particle size distribution range is 300-700nm, the average pore diameter is 1.2-1.3nm, and the SiO is spherical microporous2As a core, nano ZnTiO is sequentially grown in situ on the surface of the core3Nano NiFe2O4。
A preparation method of nano nickel ferrite/zinc titanate modified microporous silicon oxide comprises the following steps:
s1: synthesis of spherical microporous SiO by sol-gel method2: adding CTAB into deionized water, dissolving to clarify, adding 1-2mol/LNaOH solution, stirring for 10-30min, heating to 65-85 deg.C, adding ethyl orthosilicate dropwise, stirring at constant temperature for 2-6h to obtain white flocculent precipitate, vacuum filtering, washing with water and ethanol to neutrality, drying at 80-100 deg.C for 12h, grinding, calcining at 550 deg.C for 6h to obtain nanometer microporous SiO2A white powder;
s2: deposition of ZnTiO3Precursor: dissolving soluble zinc salt in deionized water, dripping titanium tetrachloride-ethanol solution, stirring, and adding microporous SiO2Adjusting pH to 1-3 with 1-2mol/L hydrochloric acid solution, stirring for 2-3 hr, transferring to reaction kettle, reacting at 100 deg.C for 12-18 hr, washing the obtained product with ethanol for 2-3 times, and drying to obtain ZnTiO3Precursor modified microporous SiO2；
S3: deposition of NiFe2O4Precursor: adding soluble ferric salt and soluble nickel salt into deionized water, stirring and dissolving, then adding sodium acetate and ZnTiO3Precursor modified microporous SiO2Stirring and dispersing, carrying out hydrothermal reaction at 130-200 ℃ for 10-18h, filtering and washing to obtain NiFe2O4/ZnTiO3Precursor modified microporous SiO2；
S4: and (3) calcining: the obtained NiFe2O4/ZnTiO3Precursor modified microporous SiO2Calcining for 2-3h at the temperature of 550-.
Preferably, the soluble zinc salt is one or more of zinc chloride, zinc sulfate, zinc nitrate and zinc acetate.
Preferably, the soluble iron salt is one or more of ferric chloride, ferric sulfate, ferric nitrate and ferric acetate.
Preferably, the soluble nickel salt is one or more of nickel chloride, nickel sulfate, nickel nitrate and nickel acetate.
Preferably, the dosage ratio of CTAB, deionized water, NaOH solution and tetraethoxysilane is (0.2-0.4) g: (1.5-2) mL: (3.0-4.5) mL: 5 mL.
Preferably, the soluble zinc salt, deionized water, titanium tetrachloride-ethanol solution and microporous SiO2The dosage ratio of (0.0025-0.005) mol: 50mL of: 5mL of: 3g of the total weight.
Preferably, the concentration of the titanium tetrachloride-ethanol solution is 0.5-1mol/L, and the preparation method comprises the following steps: adding 0.25-0.5mol of titanium tetrachloride into 200mL of absolute ethyl alcohol solvent, stirring uniformly, and then using absolute ethyl alcohol to fix the volume to 500mL to obtain the titanium tetrachloride.
Preferably, the soluble iron salt, the soluble nickel salt, the deionized water, the sodium acetate and the ZnTiO are3Precursor modified microporous SiO2The dosage ratio of (0.002-0.004) mol: (0.001-0.002) mol: 50mL of: (0.8-1.4) g: 3g of the total weight.
The application of the nano nickel ferrite/zinc titanate modified microporous silicon oxide in degrading sulfonamide antibiotics.
The invention has the beneficial effects that:
1. the invention takes microporous silicon oxide as a carrier for the first time, loads nano nickel ferrite, further deposits nano zinc titanate in situ, provides a large number of reaction sites by utilizing larger specific surface area of the microporous silicon oxide, improves the dispersibility of nano particles, avoids particle agglomeration, and is beneficial to the improvement of the photocatalytic activities of the nano nickel ferrite and the nano zinc titanate; the nano nickel ferrite and the nano zinc titanate are compounded into a P-N type heterojunction, so that photoproduction electrons and photoproduction holes are transferred to different directions, the effective separation of the photoproduction electrons and the photoproduction holes is realized, compared with single-phase nano zinc titanate, the photocatalysis efficiency and the catalysis stability can be effectively improved, meanwhile, the forbidden bandwidth of the nano copper sulfide is only 1.5eV, the nano copper sulfide can respond to visible light or even near infrared light, the spectrum absorption range is expanded, and the light conversion efficiency and the catalysis performance are further improved.
2. The product of the invention has magnetic separation performance because the outer layer of the product is coated with the nano nickel ferrite which has electromagnetic performance, is easy to recycle and can be recycled when being applied to water pollution treatment and soil organic matter degradation, and avoids the waste of the catalyst and the damage to the environment and the ecological system.
3. The nickel ferrite/zinc titanate modified microporous silicon oxide prepared by the method can be used for degrading sulfonamide antibiotics, and the degradation rate can reach more than 95%.
Drawings
FIG. 1 is a flow chart of a preparation method of nano nickel ferrite/zinc titanate modified microporous silicon oxide according to the invention;
FIG. 2 is an SEM image of the nano nickel ferrite/zinc titanate modified microporous silica prepared in example 1.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
The specific surface area of the nano nickel ferrite/zinc titanate modified microporous silicon oxide is 700-800m2(g) the particle size distribution range is 300-700nm, the average pore diameter is 1.2-1.3nm, and the SiO is spherical microporous2As a core, nano ZnTiO is sequentially grown in situ on the surface of the core3Nano NiFe2O4。
The preparation method of the nano nickel ferrite/zinc titanate modified microporous silicon oxide of the embodiment comprises the following steps:
s1: synthesis of spherical microporous SiO by sol-gel method2: adding CTAB into deionized water, dissolving to clarify, adding 1-2mol/LNaOH solution, stirring for 10-30min, heating to 65-85 deg.C, adding ethyl orthosilicate dropwise, stirring at constant temperature for 2-6h to obtain white flocculent precipitate, vacuum filtering, washing with water and ethanol to neutrality, drying at 80-100 deg.C for 12h, grinding, calcining at 550 deg.C for 6h to obtain nanometer microporous SiO2A white powder; the dosage ratio of CTAB, deionized water, NaOH solution and tetraethoxysilane is (0.2-0.4) g: (1.5-2) mL: (3.0-4.5) mL: 5 mL;
s2: deposition of ZnTiO3Precursor: dissolving soluble zinc salt in deionized water, dripping titanium tetrachloride-ethanol solution, stirring, and adding microporous SiO2Adjusting pH to 1-3 with 1-2mol/L hydrochloric acid solution, stirring for 2-3 hr, transferring to reaction kettle, reacting at 100 deg.C for 12-18 hr, washing the obtained product with ethanol for 2-3 times, and drying to obtain ZnTiO3Precursor modified microporous SiO2(ii) a The soluble zinc salt is one or more of zinc chloride, zinc sulfate, zinc nitrate and zinc acetate; the soluble zinc salt, deionized water, titanium tetrachloride-ethanol solution and microporous SiO2The dosage ratio of (0.0025-0.005) mol: 50mL of: 5mL of: 3g of the total weight of the mixture; the concentration of the titanium tetrachloride-ethanol solution is 0.5-1mol/L, and the preparation method comprises the following steps: adding 0.25-0.5mol of titanium tetrachloride into 200mL of absolute ethyl alcohol solvent, stirring uniformly, and then using absolute ethyl alcohol to fix the volume to 500mL to obtain the titanium tetrachloride;
s3: deposition of NiFe2O4Precursor: adding soluble ferric salt and soluble nickel salt into deionized water, stirring and dissolving, then adding sodium acetate and ZnTiO3Precursor modified microporous SiO2Stirring and dispersing, carrying out hydrothermal reaction at 130-200 ℃ for 10-18h, filtering and washing to obtain NiFe2O4/ZnTiO3Precursor modified microporous SiO2(ii) a The soluble ferric salt is one or more of ferric chloride, ferric sulfate, ferric nitrate and ferric acetate; the soluble nickel salt is one or more of nickel chloride, nickel sulfate, nickel nitrate and nickel acetate; the soluble ferric salt, the soluble nickel salt, the deionized water, the sodium acetate and the ZnTiO3Precursor modified microporous SiO2The dosage ratio of (0.002-0.004) mol: (0.001-0.002) mol: 50mL of: (0.8-1.4) g: 3g of the total weight of the mixture;
s4: and (3) calcining: the obtained NiFe2O4/ZnTiO3Precursor modified microporous SiO2Calcining for 2-3h at the temperature of 550-.
The application of the nano nickel ferrite/zinc titanate modified microporous silicon oxide in the degradation of sulfonamide antibiotics specifically comprises one or more of sulfathiazole and sodium salt, sulfadiazine and sodium salt, sulfisoxazole, sulfadimidine, sulfamethoxazole, sulfamonomethoxine, sulfamylon and sulfacetamide.
Example 1
The preparation method of the nano nickel ferrite/zinc titanate modified microporous silicon oxide comprises the following steps:
s1: synthesis of spherical microporous SiO by sol-gel method2: adding 0.4g CTAB into 3mL of deionized water, dissolving until the solution is clear, adding 6mL of 1mol/L NaOH solution, stirring for 10min, heating to 65 ℃, dropwise adding 10mL of ethyl orthosilicate, stirring at constant temperature for 2h to obtain white flocculent precipitate, performing suction filtration, washing with water and ethanol to neutrality, drying at 80 ℃ for 12h, grinding, calcining at 550 ℃ for 6h to obtain nano microporous SiO2A white powder;
s2: deposition of ZnTiO3Precursor: dissolving 0.0025mol of zinc chloride in 50mL of deionized water, then dropwise adding 5mL of 0.5mol/L titanium tetrachloride-ethanol solution, stirring uniformly, and adding 3g of microporous SiO2Then regulating the pH value to 2 by using 1mol/L hydrochloric acid solution, continuously stirring for 2h, transferring the mixture into a reaction kettle, reacting for 12h at 100 ℃, washing the obtained product for 2 times by using ethanol, and drying to obtain ZnTiO3Precursor modified microporous SiO2(ii) a The preparation method of the titanium tetrachloride-ethanol solution comprises the following steps: adding 0.25mol of titanium tetrachloride into 200mL of absolute ethyl alcohol solvent, stirring uniformly, and then using absolute ethyl alcohol to fix the volume to 500mL to obtain the titanium tetrachloride;
s3: deposition of NiFe2O4Precursor: adding 0.002mol of ferric chloride and 0.001mol of nickel chloride into 50mL of deionized water, stirring and dissolving, and then adding 0.8g of sodium acetate and 3g of ZnTiO3Precursor modified microporous SiO2Stirring, dispersing, hydrothermal reacting at 130 deg.C for 10 hr, filtering, washing to obtain NiFe2O4/ZnTiO3Precursor modified microporous SiO2；
S4: and (3) calcining: the obtained NiFe2O4/ZnTiO3Precursor modified microporous SiO2Calcining for 2h at 550 ℃ to obtain the nano nickel ferrite/zinc titanate modified microporous silicon oxide.
Example 2
The preparation method of the nano nickel ferrite/zinc titanate modified microporous silicon oxide comprises the following steps: s1: synthesis of spherical microporous SiO by sol-gel method2: adding 0.6g CTAB into 3.5mL deionized water, dissolving to be clear, adding 7.5mL 1.5mol/L NaOH solution, stirring for 20min, heating to 75 ℃, dropwise adding 10mL ethyl orthosilicate, stirring at constant temperature for 4h to obtain white flocculent precipitate, performing suction filtration, washing with water and ethanol to be neutral, drying at 100 ℃ for 12h, grinding, and calcining at 550 ℃ for 6h to obtain nano microporous SiO2A white powder;
s2: deposition of ZnTiO3Precursor: 0.00375mol of zinc nitrate is dissolved in 50mL of deionized water, 5mL of 0.75mol/L titanium tetrachloride-ethanol solution is added dropwise, after uniform stirring, 3g of microporous SiO is added2Then regulating the pH value to 2 by using 1.5mol/L hydrochloric acid solution, continuously stirring for 2.5h, transferring the mixture into a reaction kettle, reacting for 15h at 100 ℃, washing the obtained product for 3 times by using ethanol, and drying to obtain ZnTiO3Precursor modified microporous SiO2(ii) a The soluble zinc salt is one or more of zinc chloride, zinc sulfate, zinc nitrate and zinc acetate; the preparation method of the titanium tetrachloride-ethanol solution comprises the following steps: adding 0.375mol of titanium tetrachloride into 200mL of absolute ethyl alcohol solvent, stirring uniformly, and then using absolute ethyl alcohol to fix the volume to 500mL to obtain the titanium tetrachloride;
s3: deposition of NiFe2O4Precursor: adding 0.003mol of ferric nitrate and 0.0015mol of nickel nitrate into 50mL of deionized water, stirring to dissolve, and then adding 1.1g of sodium acetate and 3g of ZnTiO3Precursor modified microporous SiO2Stirring, dispersing, hydrothermal reacting at 160 deg.C for 15 hr, filtering, washing to obtain NiFe2O4/ZnTiO3Precursor modified microporous SiO2；
S4: and (3) calcining: the obtained NiFe2O4/ZnTiO3Precursor modified microporous SiO2Calcining for 2.5h at 600 ℃ to obtain the nano nickel ferrite/zinc titanate modified microporous silicon oxide.
Example 3
The preparation method of the nano nickel ferrite/zinc titanate modified microporous silicon oxide comprises the following steps:
s1: synthesis of spherical microporous SiO by sol-gel method2: adding 0.8g CTAB into 4mL of deionized water, dissolving until the solution is clear, adding 9mL of 2mol/L NaOH solution, stirring for 30min, heating to 85 ℃, dropwise adding 10mL of ethyl orthosilicate, stirring at constant temperature for 6h to obtain white flocculent precipitate, performing suction filtration, washing with water and ethanol to neutrality, drying at 100 ℃ for 12h, grinding, calcining at 550 ℃ for 6h to obtain nano microporous SiO2A white powder;
s2: deposition of ZnTiO3Precursor: dissolving 0.005mol of zinc acetate in 50mL of deionized water, then dropwise adding 5mL of 1mol/L titanium tetrachloride-ethanol solution, stirring uniformly, and adding 3g of microporous SiO2Adjusting the pH value to 3 by using 2mol/L hydrochloric acid solution, continuously stirring for 3h, transferring the mixture into a reaction kettle, reacting for 18h at 100 ℃, washing the obtained product for 3 times by using ethanol, and drying to obtain ZnTiO3Precursor modified microporous SiO2(ii) a The preparation method of the titanium tetrachloride-ethanol solution comprises the following steps: adding 0.5mol of titanium tetrachloride into 200mL of absolute ethyl alcohol solvent, stirring uniformly, and then using absolute ethyl alcohol to fix the volume to 500mL to obtain the titanium tetrachloride;
s3: deposition of NiFe2O4Precursor: adding 0.004mol of iron acetate and 0.002mol of nickel acetate into 50mL of deionized water, stirring and dissolving, and then adding 1.4g of sodium acetate and 3g of ZnTiO3Precursor modified microporous SiO2Stirring, dispersing, hydrothermal reacting at 200 deg.C for 18h, filtering, washing to obtain NiFe2O4/ZnTiO3Precursor modified microporous SiO2；
S4: and (3) calcining: the obtained NiFe2O4/ZnTiO3Precursor modified microporous SiO2Calcining for 3h at 600 ℃ to obtain the nano nickel ferrite/zinc titanate modified microporous silicon oxide.
The nano zinc titanate modified microporous silicon oxide is used as a comparative example: comparative example the procedure was the same as in example 1, except that: comparative example preparation method no S3 deposition of NiFe2O4And (5) precursor step.
And (3) measuring the photocatalytic performance:
50mg of the modified microporous silicon oxide products prepared in the embodiments 1 to 3 and the comparative example are weighed, then respectively added into 4 groups of 100mL 50mg/L sulfathiazole sodium water solution under dark condition, stirred for 5min, then an LED lamp of 40W is turned on, and after stirring treatment for 6h, the degradation rate of the sulfathiazole sodium is measured.
The test results are shown in table 1:
| example 1 | Example 2 | Example 3 | Comparative example | |
| Percent ratio of sodium sulfathiazole degradation | 95.2 | 97.7 | 98.5 | 36.1 |
| Specific surface area/m2/g | 783 | 755 | 739 | 785 |
| Particle size distribution range/nm | 300-650 | 360-700 | 410-700 | 300-600 |
| Average pore diameter/nm | 1.3 | 1.3 | 1.2 | 1.4 |
In the embodiments 1-3, the microporous silicon oxide is used as a carrier for the first time, the nano nickel ferrite is loaded, and the nano zinc titanate is further deposited in situ, so that a large number of reaction sites are provided by utilizing the larger specific surface area of the microporous silicon oxide, the dispersibility of nano particles is improved, the particle agglomeration is avoided, and the improvement of the photocatalytic activity of the nano nickel ferrite and the nano zinc titanate is facilitated; the nano nickel ferrite and the nano zinc titanate are compounded into a P-N type heterojunction, so that photoproduction electrons and photoproduction holes are transferred to different directions, the effective separation of the photoproduction electrons and the photoproduction holes is realized, compared with single-phase nano zinc titanate, the photocatalysis efficiency and the catalysis stability can be effectively improved, meanwhile, the forbidden bandwidth of the nano copper sulfide is only 1.5eV, the nano copper sulfide can respond to visible light or even near infrared light, the spectrum absorption range is expanded, and the light conversion efficiency and the catalysis performance are further improved.
The nano nickel ferrite is coated on the outer layer of the product in the embodiments 1-3, and the nickel ferrite has electromagnetic property, so that the product has magnetic separation property, is easy to recycle and can be recycled when being applied to water pollution treatment and soil organic matter degradation, and avoids waste of the catalyst and damage to the environment and the ecological system.
The nickel ferrite/zinc titanate modified microporous silicon oxide prepared in the embodiments 1 to 3 can be used for degrading sulfonamide antibiotics, and the degradation rate can reach more than 95%.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (10)
1. The nano nickel ferrite/zinc titanate modified microporous silicon oxide is characterized in that the specific surface area of the nano nickel ferrite/zinc titanate modified microporous silicon oxide is 700-800m2(g) the particle size distribution range is 300-700nm, the average pore diameter is 1.2-1.3nm, and the SiO is spherical microporous2As a core, nano ZnTiO is sequentially grown in situ on the surface of the core3Nano NiFe2O4。
2. A preparation method of nano nickel ferrite/zinc titanate modified microporous silicon oxide is characterized by comprising the following steps:
s1: synthesis of spherical microporous SiO by sol-gel method2: adding CTAB into deionized water, dissolving to clarify, adding 1-2mol/LNaOH solution, stirring for 10-30min, heating to 65-85 deg.C, adding ethyl orthosilicate dropwise, stirring at constant temperature for 2-6h to obtain white flocculent precipitate, vacuum filtering, washing with water and ethanol to neutrality, drying at 80-100 deg.C for 12h, grinding, calcining at 550 deg.C for 6h to obtain nanometer microporous SiO2A white powder;
s2: deposition of ZnTiO3Precursor: dissolving soluble zinc salt in deionized water, dripping titanium tetrachloride-ethanol solution, stirring, and adding microporous SiO2Adjusting pH to 1-3 with 1-2mol/L hydrochloric acid solution, stirring for 2-3 hr, transferring to reaction kettle, reacting at 100 deg.C for 12-18 hr, washing the obtained product with ethanol for 2-3 times, and drying to obtain ZnTiO3Precursor modified microporous SiO2；
S3: deposition of NiFe2O4Precursor: adding soluble ferric salt and soluble nickel salt into deionized water, stirring and dissolving, then adding sodium acetate and ZnTiO3Precursor modified microporous SiO2Stirring and dispersing, carrying out hydrothermal reaction at 130-200 ℃ for 10-18h, filtering and washing to obtain NiFe2O4/ZnTiO3Precursor modified microporous SiO2；
S4: and (3) calcining: the obtained NiFe2O4/ZnTiO3Precursor modified microporous SiO2Calcining for 2-3h at the temperature of 550-.
3. The method for preparing nano nickel ferrite/zinc titanate modified microporous silica according to claim 2, wherein the soluble zinc salt is one or more of zinc chloride, zinc sulfate, zinc nitrate and zinc acetate.
4. The method for preparing nano nickel ferrite/zinc titanate modified microporous silica according to claim 2, wherein the soluble ferric salt is one or more of ferric chloride, ferric sulfate, ferric nitrate and ferric acetate.
5. The method for preparing nano nickel ferrite/zinc titanate modified microporous silica according to claim 2, wherein the soluble nickel salt is one or more of nickel chloride, nickel sulfate, nickel nitrate and nickel acetate.
6. The method for preparing nano nickel ferrite/zinc titanate modified microporous silica according to claim 2, wherein the dosage ratio of CTAB, deionized water, NaOH solution and ethyl orthosilicate is (0.2-0.4) g: (1.5-2) mL: (3.0-4.5) mL: 5 mL.
7. The method for preparing nano nickel ferrite/zinc titanate modified microporous silica according to claim 2, wherein the soluble zinc salt, deionized water, titanium tetrachloride-ethanol solution, microporous SiO, and the like are added2The dosage ratio of (0.0025-0.005) mol: 50mL of: 5mL of: 3g of the total weight.
8. The method for preparing nano nickel ferrite/zinc titanate modified microporous silica according to claim 7, wherein the concentration of the titanium tetrachloride-ethanol solution is 0.5-1mol/L, and the preparation method comprises the following steps: adding 0.25-0.5mol of titanium tetrachloride into 200mL of absolute ethyl alcohol solvent, stirring uniformly, and then using absolute ethyl alcohol to fix the volume to 500mL to obtain the titanium tetrachloride.
9. The method for preparing nano nickel ferrite/zinc titanate modified microporous silica according to claim 2, wherein the soluble iron salt, the soluble nickel salt, deionized water, sodium acetate and ZnTiO are used as raw materials3Precursor modified microporous SiO2The dosage ratio of (0.002-0.004) mol: (0.001-0.002) mol: 50mL of: (0.8-1.4) g: 3g of the total weight.
10. The application of the nano nickel ferrite/zinc titanate modified microporous silicon oxide prepared by the preparation method according to any one of claims 2 to 9 in degrading sulfonamide antibiotics.
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