CN110813313B - Silver oxide/layered double-metal hydroxide compound and preparation and application thereof - Google Patents
Silver oxide/layered double-metal hydroxide compound and preparation and application thereof Download PDFInfo
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- CN110813313B CN110813313B CN201911094749.6A CN201911094749A CN110813313B CN 110813313 B CN110813313 B CN 110813313B CN 201911094749 A CN201911094749 A CN 201911094749A CN 110813313 B CN110813313 B CN 110813313B
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- Prior art keywords
- silver oxide
- nickel
- double hydroxide
- layered double
- titanium
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- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 title claims abstract description 399
- 229910001923 silver oxide Inorganic materials 0.000 title claims abstract description 201
- 229910000000 metal hydroxide Inorganic materials 0.000 title claims description 49
- 238000002360 preparation method Methods 0.000 title abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 150
- 239000002131 composite material Substances 0.000 claims abstract description 92
- -1 hydroxide compound Chemical class 0.000 claims abstract description 38
- 230000001699 photocatalysis Effects 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 7
- 230000023556 desulfurization Effects 0.000 claims abstract description 7
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical group [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 claims description 186
- 229910001000 nickel titanium Inorganic materials 0.000 claims description 186
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 150000004692 metal hydroxides Chemical class 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 11
- 238000010992 reflux Methods 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 150000002815 nickel Chemical class 0.000 claims description 4
- 150000003608 titanium Chemical class 0.000 claims description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 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 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- 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 3
- 229940096017 silver fluoride Drugs 0.000 claims description 3
- REYHXKZHIMGNSE-UHFFFAOYSA-M silver monofluoride Chemical compound [F-].[Ag+] REYHXKZHIMGNSE-UHFFFAOYSA-M 0.000 claims description 3
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- INNSZZHSFSFSGS-UHFFFAOYSA-N acetic acid;titanium Chemical compound [Ti].CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O INNSZZHSFSFSGS-UHFFFAOYSA-N 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 claims description 2
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 claims description 2
- UQPSGBZICXWIAG-UHFFFAOYSA-L nickel(2+);dibromide;trihydrate Chemical compound O.O.O.Br[Ni]Br UQPSGBZICXWIAG-UHFFFAOYSA-L 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 37
- 238000000926 separation method Methods 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 239000000969 carrier Substances 0.000 abstract description 4
- 238000013329 compounding Methods 0.000 abstract description 2
- 125000001741 organic sulfur group Chemical group 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 112
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 64
- 238000001179 sorption measurement Methods 0.000 description 35
- 238000001035 drying Methods 0.000 description 17
- 238000012360 testing method Methods 0.000 description 17
- 230000007935 neutral effect Effects 0.000 description 14
- 239000000047 product Substances 0.000 description 13
- 238000005406 washing Methods 0.000 description 11
- 239000010410 layer Substances 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 9
- 239000011521 glass Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 239000012065 filter cake Substances 0.000 description 7
- 238000002329 infrared spectrum Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 239000011229 interlayer Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 5
- 150000004679 hydroxides Chemical class 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000012496 blank sample Substances 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 238000013507 mapping Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000001052 transient effect Effects 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910001453 nickel ion Inorganic materials 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000003459 sulfonic acid esters Chemical class 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 229910021585 Nickel(II) bromide Inorganic materials 0.000 description 1
- 229910018553 Ni—O Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000007707 calorimetry Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000013213 extrapolation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 description 1
- 229940053662 nickel sulfate Drugs 0.000 description 1
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 description 1
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 description 1
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- OTCVAHKKMMUFAY-UHFFFAOYSA-N oxosilver Chemical compound [Ag]=O OTCVAHKKMMUFAY-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000000276 potassium ferrocyanide Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000001055 reflectance spectroscopy Methods 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
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
- 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
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/892—Nickel and noble metals
-
- 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—
-
- B01J35/39—
-
- B01J35/61—
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
Abstract
The invention discloses a silver oxide/layered double hydroxide compound, wherein silver oxide is loaded on a layered double hydroxide. The invention discloses a preparation method of the silver oxide/layered double hydroxide compound, which comprises the following steps: adding silver salt and layered double hydroxide into a solvent, uniformly mixing, and adjusting to be alkaline to obtain the silver oxide/layered double hydroxide compound. The invention discloses application of the silver oxide/layered double hydroxide compound in the field of photocatalytic desulfurization. The invention introduces the object-silver oxide into the layered double hydroxide for compounding, synergistically improves the absorption and utilization rate of photons, improves the separation efficiency of photon-generated carriers and the surface catalytic reaction efficiency, further improves the photocatalytic activity of the composite material, and can be applied to the removal of organic sulfur.
Description
Technical Field
The invention relates to the technical field of photocatalysts, in particular to a silver oxide/layered double hydroxide compound and preparation and application thereof.
Background
With the rapid development of economy, the global fossil energy consumption is continuously increased, and the environmental pollution is increasingly serious. Conversion of sulfur compounds in petroleum products to SO after combustionXIs one of the important causes of acid rain formation and atmospheric pollution. Thus, strict fuel sulfur standards are established throughout the world in various countries. Currently, china has promulgated the national gasoline standard at stage five. From 1 month and 1 day 2018, gasoline in the fifth stage is supplied nationwide, and the sulfur content of the Chinese gasoline is reduced to below 10 ppm. The production of low sulfur fuels has become one of the important tasks in modern refineries today.
In order to produce ultra low sulfur standard fuels, some early hydrodesulfurization processes must meet conditions of higher temperature, higher hydrogen pressure, higher catalyst activity, and longer reaction time. Deep desulfurization results in the production of certain secondary reactions, such as shortened catalyst life and increased hydrogen consumption, with severe yield losses and ultimately high costs.
The nano layered two-dimensional photocatalyst material mostly has larger specific surface area and more catalytic activity centers, which is beneficial to the catalytic reaction, and the method of laminate peeling and the like is used for reducing the layer number of the layered material, which is beneficial to the catalytic reaction, effectively reducing the bulk phase recombination rate of the photocarrier, and enabling the layered material to rapidly migrate to the surface for the catalytic reaction. The Layered Double Hydroxides (LDHs) have the advantages of adjustable chemical components of the laminate, easy exchange of anions between layers, multiple types of intercalation molecules, large specific surface area, topological transformation and the like, and can be used as ideal photocatalysts, catalyst carriers or precursors. Such as Bingwei Chang, Mengmeng Wu, Jie Mi. pyrolosis kinetics of ZnAl LDHs and its catalyzed products for H2S removal[J].Journal of Thermal Analysis&Calorimetry,2018,132(1)581-589.》、《Yu N L,Yang Z,Yu Z B,Cai T F,Li Y,Guo C Y,Qi C Y,Ren T Q.Synthesis of four-angle star-like CoAl-MMOBiVO4 p-n heterojunction and its application in photocatalytic desulfurization[J]RSC Advances,2017,7(41) 25455-25460A and Yingjie Cai, Hongyan Song, ZHE An, Xu Xian, Xin Shua, Jing He]Green chem, 2018,20, 5509-.
However, catalytic activity of the LDHs photocatalytic material is still low, which limits the application of the LDHs photocatalytic material in the field of photocatalytic oxidation desulfurization.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a silver oxide/layered double hydroxide compound and preparation and application thereof.
A silver oxide/layered double hydroxide composite having silver oxide supported on a layered double hydroxide.
Preferably, the silver oxide is supported on the surface of the layered double hydroxide.
Preferably, the layered double hydroxide is a nickel-titanium double hydroxide.
Preferably, the mass ratio of silver oxide to layered double hydroxide is 0.4-0.6: 1, can be 0.4: 1. 0.42: 1. 0.44: 1. 0.46: 1. 0.48: 1. 0.5: 1. 0.51: 1. 0.53: 1. 0.55: 1. 0.57: 1. 0.59: 1. 0.6: 1.
preferably, the forbidden band width of the silver oxide/layered double hydroxide composite is 1.25-1.30 eV.
The invention introduces the object-silver oxide into the layered double hydroxide for compounding, synergistically improves the absorption and utilization rate of photons, improves the separation efficiency of photon-generated carriers and the surface catalytic reaction efficiency, further improves the photocatalytic activity of the composite material, and can be applied to the removal of organic sulfur.
The preparation method of the silver oxide/layered double hydroxide compound comprises the following steps: adding silver salt and layered double hydroxide into a solvent, uniformly mixing, and adjusting to be alkaline to obtain the silver oxide/layered double hydroxide compound.
Preferably, the silver salt is silver nitrate or silver fluoride.
Preferably, the solvent is water.
Preferably, the system is adjusted to be alkaline by using aqueous sodium hydroxide solution, aqueous potassium hydroxide solution, triethylamine, diethylamine, diethanolamine, triethanolamine or urea solution, preferably aqueous sodium hydroxide solution, more preferably aqueous sodium hydroxide solution with the concentration of 0.2 mol/L.
Preferably, the adjustment to alkalinity is an adjustment of the system pH to 13.5-14.5.
Preferably, after being adjusted to be alkaline, the precipitate is washed to be neutral and dried in vacuum to obtain the silver oxide/layered double hydroxide composite.
Preferably, the vacuum drying time is 10-14h, preferably 12 h.
Preferably, if the layered double hydroxide is a nickel-titanium double hydroxide, it is prepared by the following process: mixing nickel salt, titanium salt and triethanolamine, adjusting the pH value of the system to 8-9, heating, condensing and refluxing to obtain the nickel-titanium double metal hydroxide.
Preferably, the molar ratio of nickel ions, titanium ions and triethanolamine is 5: 1: 4-6, the molar ratio of nickel ion to titanium ion is determined by the structure of the product (nickel-titanium double hydroxide), and can be increased or decreased, but only the product yield is affected, and the product generation is not affected, so that the molar ratio is still considered to fall within the protection scope when the molar ratio is inconsistent with the range.
Preferably, the temperature is raised to 95-100 ℃, and the condensation reflux is carried out for 44-52 h; can be heated to 95 deg.C, 95.2 deg.C, 95.4 deg.C, 95.6 deg.C, 95.8 deg.C, 96 deg.C, 96.1 deg.C, 96.3 deg.C, 96.5 deg.C, 96.7 deg.C, 96.9 deg.C, 97 deg.C, 97.2 deg.C, 97.4 deg.C, 97.6 deg.C, 97.8 deg.C, 98.1 deg.C, 98.3 deg.C, 98.5 deg.C, 98.7 deg.C, 98.9 deg.C, 99 deg.2 deg.C, 99.4 deg.C, 99.6 deg.8 deg.C, 100 deg.C; the condensing reflux time can be 44h, 44.5h, 46h, 46.5h, 47h, 47.5h, 48h, 48.5h, 49h, 49.5h, 50h, 50.5h, 51h, 51.5h, 52 h.
Preferably, the nickel salt is at least one of nickel nitrate, nickel sulfate, nickel fluoride, nickel chloride, nickel bromide and nickel acetate, and is preferably nickel nitrate.
Preferably, the titanium salt is at least one of titanium acetate, titanium chloride, titanium fluoride, tetrabutyl titanate and isopropyl titanate, and tetrabutyl titanate is preferred.
Preferably, the pH of the system is adjusted to 8-9 by using aqueous sodium hydroxide solution, aqueous potassium hydroxide solution, triethylamine, diethylamine, diethanolamine, triethanolamine and urea solution, preferably aqueous sodium hydroxide solution, and more preferably aqueous sodium hydroxide solution with the concentration of 1 mol/L.
Preferably, after condensing and refluxing, carrying out suction filtration, washing a filter cake to be neutral, and drying to obtain the nickel-titanium double metal hydroxide.
Preferably, the drying temperature is 55-65 ℃, and the drying time is 20-28 h; more preferably, the drying temperature is 60 ℃ and the drying time is 24 h.
Preferably, the resulting nickel-titanium double hydroxide is a green powder.
The method adopts a precipitation method to prepare the layered double hydroxide, and then obtains the silver oxide/layered double hydroxide compound through the precipitation method, the preparation process is simple, the silver oxide is effectively loaded on the surface of the layered double hydroxide, the forbidden bandwidth is reduced, the wavelength range of the absorbable light is expanded, the separation efficiency of the photon-generated carriers and the surface catalytic reaction efficiency are improved, and the separation efficiency of the photon-generated electron-hole pair is enhanced.
The silver oxide/layered double hydroxide compound is applied to the field of photocatalytic desulfurization.
The LDHs have the advantages of easy adjustment of chemical composition of a coating, easy exchange of anions between layers, various types of embedded molecules, large specific surface area and topological transformation. However, the LDHs has low photocatalytic activity, which limits the application of the LDHs in the field of photocatalysis.
The invention constructs the metal semiconductor material composite LDHs photocatalytic material by introducing the object oxide particles-silver oxide, and obtains the composite material with higher photocatalytic efficiency for removing the organic sulfide ethanethiol.
Drawings
FIG. 1 is an X-ray diffraction pattern of the nickel-titanium double hydroxide obtained in comparative example 1.
FIG. 2 shows comparative X-ray diffraction patterns of the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2, and the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3.
FIG. 3 is an electron microscope scan of the nickel-titanium double hydroxide obtained in comparative example 1.
FIG. 4 is an electron micrograph of the silver oxide obtained in comparative example 2.
FIG. 5 is an electron microscope scan of the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3.
FIG. 6 is a SEM-EDS Mapping elemental map of the silver oxide/nickel-titanium double metal hydroxide composite obtained in comparative example 3.
FIG. 7 is an infrared spectrum of a silver oxide/nickel-titanium double hydroxide composite obtained in example 5, a nickel-titanium double hydroxide obtained in comparative example 1, a silver oxide obtained in comparative example 2, and a silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3, wherein a is the nickel-titanium double hydroxide obtained in comparative example 1, b is the silver oxide obtained in comparative example 2, c is the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3, and d is the silver oxide/nickel-titanium double hydroxide composite obtained in example 5.
FIG. 8 is a UV-visible diffuse reflectance spectrum of the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2, and the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3, wherein a is the nickel-titanium double hydroxide obtained in comparative example 1, b is the silver oxide obtained in comparative example 2, c is the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, and d is the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3.
FIG. 9 is a graph showing the relationship between the photon absorption coefficient and the photon energy of the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2, and the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3; wherein, the curves of the silver oxide/nickel-titanium double metal hydroxide composites obtained in example 5 and comparative example 3 in the region of 200-800nm are enlarged as attached small graphs.
Fig. 10 is a graph showing transient photocurrent responses of the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2, and the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3 under visible light irradiation, wherein a is the nickel-titanium double hydroxide obtained in comparative example 1, b is the silver oxide obtained in comparative example 2, c is the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, and d is the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3.
FIG. 11 is a graph showing electrochemical impedance spectra of the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2, and the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3; wherein, the curves of the silver oxide/nickel-titanium double hydroxide composites obtained in example 5 and comparative example 3, and the silver oxide obtained in comparative example 2 in the region of 0-1000 Ω are enlarged as attached panels.
FIG. 12 is a Mott-Schottky graph of the nickel-titanium double hydroxide obtained in comparative example 1.
FIG. 13 is a Mott-Schottky plot of the silver oxide obtained in comparative example 2.
FIG. 14 is a Mott-Schottky graph of the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3.
FIG. 15 is a Mott-Schottky graph of the silver oxide/nickel-titanium double hydroxide composite obtained in example 5.
FIG. 16 is an infrared spectrum of the adsorbed photocatalytic process of the nickel-titanium double hydroxide obtained in comparative example 1, in which a is a plot of the nickel-titanium double hydroxide as it is, b is a plot of the nickel-titanium double hydroxide after adsorption, and c is a plot of the nickel-titanium double hydroxide after adsorption in visible light.
FIG. 17 is an infrared spectrum of the silver oxide obtained in comparative example 2 in the adsorption and photocatalytic process, wherein a is a curve of the silver oxide as it is, b is a curve of the silver oxide obtained after adsorption, and c is a curve of the silver oxide irradiated with visible light after adsorption.
FIG. 18 is an infrared spectrum of the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3 in the adsorption and photocatalytic process, in which a is a curve of the silver oxide/nickel-titanium double hydroxide composite as it is, b is a curve of the silver oxide/nickel-titanium double hydroxide composite after adsorption, and c is a curve of the silver oxide/nickel-titanium double hydroxide composite after adsorption in visible light.
Fig. 19 is an infrared spectrum of the silver oxide/nickel-titanium double hydroxide composite obtained in example 5 in the adsorption and photocatalytic processes, in which a is the original curve of the silver oxide/nickel-titanium double hydroxide composite, b is the curve of the silver oxide/nickel-titanium double hydroxide composite after adsorption, and c is the curve of the silver oxide/nickel-titanium double hydroxide composite after adsorption and visible light irradiation.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
The main experimental instruments used were as follows:
the main reagents used were as follows:
example 1
A preparation method of a silver oxide/nickel-titanium double metal hydroxide compound comprises the following steps:
5.257g of nickel sulfate hexahydrate, 0.759g of titanium chloride and 2.387g of triethanolamine are mixed, potassium hydroxide aqueous solution is adopted to adjust the pH value of the system to 8, the temperature is raised to 100 ℃, the mixture is condensed and refluxed for 44 hours, the filtration is carried out, the filter cake is washed to be neutral, and the filter cake is dried for 20 hours at 65 ℃ to obtain green powder, namely nickel-titanium double metal hydroxide;
adding 0.088g of silver fluoride and 0.200g of nickel-titanium double hydroxide into water, uniformly mixing, adjusting the pH value of a system to 14.5 by using triethylamine, washing the precipitate to be neutral, and drying in vacuum for 10 hours to obtain a silver oxide/nickel-titanium double hydroxide compound, wherein the mass ratio of the silver oxide to the nickel-titanium double hydroxide is 0.4: 1.
example 2
A preparation method of a silver oxide/nickel-titanium double metal hydroxide compound comprises the following steps:
mixing 47.538g of nickel chloride hexahydrate, 7.587g of titanium chloride and 35.805g of triethanolamine, adjusting the pH of the system to 9 by adopting a urea aqueous solution, heating to 95 ℃, condensing and refluxing for 52 hours, carrying out suction filtration, washing a filter cake to be neutral, and drying for 28 hours at 55 ℃ to obtain green powder, namely nickel-titanium double metal hydroxide;
adding 0.176g of silver nitrate and 0.200g of nickel-titanium double hydroxide into water, uniformly mixing, adjusting the pH value of a system to 13.5 by using diethylamine, washing the precipitate to be neutral, and drying in vacuum for 14 hours to obtain a silver oxide/nickel-titanium double hydroxide compound, wherein the mass ratio of the silver oxide to the nickel-titanium double hydroxide is 0.6: 1.
example 3
A preparation method of a silver oxide/nickel-titanium double metal hydroxide compound comprises the following steps:
mixing 5.933g of nickel nitrate hexahydrate, 1.361g of tetrabutyl titanate and 2.684g of triethanolamine, adjusting the pH of the system to 8.5 by using diethylamine, heating to 98 ℃, condensing and refluxing for 46h, performing suction filtration, washing a filter cake to be neutral, and drying for 26h at 58 ℃ to obtain green powder, namely nickel-titanium double metal hydroxide;
adding 0.132g of silver nitrate and 0.200g of nickel-titanium double hydroxide into water, uniformly mixing, adjusting the pH value of a system to 14 by adopting a potassium hydroxide aqueous solution, washing a precipitate to be neutral, and drying in vacuum for 13 hours to obtain a silver oxide/nickel-titanium double hydroxide compound, wherein the mass ratio of the silver oxide to the nickel-titanium double hydroxide is 0.45: 1.
example 4
A preparation method of a silver oxide/nickel-titanium double metal hydroxide compound comprises the following steps:
3.654g of nickel acetate, 1.137g of isopropyl titanate and 3.282g of triethanolamine are mixed, the pH value of the system is adjusted to 8.5 by using an aqueous solution of sodium hydroxide, the temperature is increased to 99 ℃, the mixture is condensed and refluxed for 50h, filtered, washed to be neutral, and dried for 22h at 62 ℃ to obtain green powder, namely nickel-titanium double metal hydroxide;
adding 0.161g of silver nitrate and 0.200g of nickel-titanium double hydroxide into water, uniformly mixing, adjusting the pH value of a system to 14 by using an aqueous solution of sodium hydroxide, washing a precipitate to be neutral, and drying in vacuum for 11 hours to obtain a silver oxide/nickel-titanium double hydroxide compound, wherein the mass ratio of the silver oxide to the nickel-titanium double hydroxide is 0.55: 1.
example 5
A preparation method of a silver oxide/nickel-titanium double metal hydroxide compound comprises the following steps:
adding 7.5mL of absolute ethyl alcohol and 1.390g of n-butyl titanate into a three-neck flask, mixing at 60 ℃, adding 3.615g of triethanolamine into the three-neck flask, continuously stirring until the mixture is uniform, then adding 5.933g of nickel nitrate hexahydrate and 50.0mL of deionized water, then slowly adding 1mol/L sodium hydroxide aqueous solution, adjusting the pH value of the system to 8-9, heating to 100 ℃, condensing and refluxing for 48 hours, then performing suction filtration, washing a filter cake to be neutral, and drying at 60 ℃ for 24 hours to obtain green powder, namely nickel-titanium double metal hydroxide;
dispersing 0.200g of nickel-titanium double hydroxide in 50.0mL of distilled water, adding 0.146g of silver nitrate, and magnetically stirring for 30 min; dropwise adding a 0.2mol/L sodium hydroxide aqueous solution until the pH value of the system is 14, washing the obtained precipitate to be neutral by using deionized water, and then drying in a vacuum drying oven for 12 hours to obtain a silver oxide/nickel-titanium double hydroxide compound, wherein the mass ratio of the silver oxide to the nickel-titanium double hydroxide is 0.5: 1.
comparative example 1
Adding 7.5mL of absolute ethyl alcohol and 1.390g of n-butyl titanate into a three-neck flask, mixing at 60 ℃, adding 3.615g of triethanolamine into the three-neck flask, continuously stirring until the mixture is uniform, then adding 5.933g of nickel nitrate hexahydrate and 50.0mL of deionized water, then slowly adding 1mol/L sodium hydroxide aqueous solution, adjusting the pH value of the system to 8-9, heating to 100 ℃, condensing and refluxing for 48h, then performing suction filtration, washing a filter cake to be neutral, and drying at 60 ℃ for 24h to obtain green powder, namely the nickel-titanium double metal hydroxide.
Comparative example 2
Dissolving 0.29g of silver nitrate in 50.0mL of distilled water, dropwise adding a 0.2mol/L sodium hydroxide aqueous solution until the pH value of the system is 14, washing the obtained precipitate to be neutral by using deionized water, and then drying the precipitate in a vacuum drying oven for 12 hours to obtain the silver oxide.
Comparative example 3
The difference from example 5 is that silver nitrate is used in an amount of 0.290 g. In the obtained silver oxide/nickel-titanium double metal hydroxide compound, the mass ratio of the silver oxide to the nickel-titanium double metal hydroxide is 1: 1.
first, X-ray diffraction test
The applicant carried out X-ray diffraction on the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2, and the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3; before testing, a sample to be tested is poured into a glass groove and compacted, and the test is carried out on a SmartLab SE model X-ray powder diffractometer of Rigaku company in Japan; a Cu target, a Ka ray source, a Ni filter plate, lambda of 0.15406nm, a tube flow of 40mA, a tube pressure of 50kV, a scanning speed of 10 degrees/min, and a scanning range of 2 theta of 5-70 degrees; the results are shown in FIGS. 1 and 2.
As can be seen from fig. 1: the product obtained in comparative example 1 has typical diffraction peaks characteristic to hydrotalcite (003), (010), (110), indicating that it has a polycrystalline structure and the structure is relatively intact. In the figure, the diffraction peaks corresponding to the 2 theta of 8.08 degrees, 16.08 degrees and 24.67 degrees are more obvious and respectively correspond to the diffraction peaks (003), (006) and (009) of the obtained product, which shows that the obtained product presents a complete layered structure, and the product obtained in the comparative example 1 is proved to be the nickel-titanium double metal hydroxide.
The interlayer distance of the product obtained in comparative example 1 was calculated to be 1.09nm from the XRD spectrum, the diffraction peak at 2 θ of 8.08 °, from the bragg equation (λ of 2dsin θ), and the theoretical interlayer distance was calculated to be 0.83nm from the related literature, which is due to a small amount of triethanolamine remaining between layers, so that the nickel-titanium double metal hydroxide obtained in comparative example 1 was experimentally calculated to have a larger interlayer distance than the theoretical value.
As can be seen from fig. 2: for the XRD pattern of the product obtained in comparative example 2, diffraction peaks at 26.70 °, 32.88 °, 38.22 °, 55.13 °, 65.69 ° and 68.92 ° respectively correspond to the (110), (111), (200), (220), (331) and (222) crystal planes of silver oxide (JCPDS card number: 41-1104); and no additional crystalline phase was observed, indicating that the product obtained in comparative example 2 was silver oxide.
While typical diffraction peaks of silver oxide and nickel-titanium double hydroxide can be clearly observed in the graphs of the products obtained in example 5 and comparative example 3, some peaks related to nickel-titanium double hydroxide are not obvious and weak due to too high content of the supported silver oxide or high intensity of the diffraction peak of the silver oxide. The resulting silver oxide/nickel-titanium double hydroxide composite exhibited an impurity peak at 44.22 ° 2 θ, presumably due to the presence of elemental silver particles during the synthesis.
The above results show that: the silver oxide/nickel-titanium double metal hydroxide compound is obtained by loading silver oxide in nickel-titanium double metal hydroxide.
Second, analysis test of scanning electron microscope
The applicant performs electron microscope scanning on the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2, and the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3; the test is carried out on a FlexSEM-1000 type scanning electron microscope of Hitachi technologies, Inc. of Japan, a small amount of samples to be tested are taken before the test, absolute ethyl alcohol is added, the samples are coated on a copper net after being dispersed uniformly by ultrasound, and the samples are naturally air-dried; the results are shown in FIGS. 3 to 5.
As can be seen from fig. 3: the nickel-titanium double metal hydroxide obtained in the comparative example 1 is of a structure stacked layer by layer, the layers are uniformly dispersed, and the outer surface is smooth; as can be seen from fig. 4: the silver oxide obtained in comparative example 2 was in an irregular particle shape; as can be seen from fig. 5: the silver oxide particles are attached to the surface of the nickel-titanium double hydroxide, which shows that the silver oxide and the nickel-titanium double hydroxide are successfully compounded together.
Thirdly, scanning electron microscopy energy spectrum (SEM-EDS Mapping) analysis
The applicant employed SEM-EDS Mapping technique to reveal the element distribution of the resulting silver oxide/nickel-titanium double metal hydroxide composite, the result of which is shown in fig. 6. Fig. 6 shows an SEM image and a corresponding element mapping image in sequence, as can be seen from fig. 6: the elements of O, Ag, Ni and Ti are uniformly distributed in the obtained silver oxide/nickel-titanium double hydroxide compound, and further shows that the silver oxide is successfully loaded on the surface of the nickel-titanium double hydroxide.
Four, infrared spectroscopy (FT-IR) analysis
The applicant detected the changes in the framework peaks of the obtained silver oxide/nickel-titanium double hydroxide composite obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2, and the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3 by infrared spectroscopy; the test was performed on a fourier transform infrared spectrometer model ls50 from semer flyer, usa, using potassium bromide sheeting, scan range: 4000-400cm-1(ii) a The scanning times are as follows: 32, a first step of removing the first layer; resolution ratio: 4cm-1(ii) a The results are shown in FIG. 7.
As can be seen from fig. 7:
1. comparative example 1 the nickel-titanium double hydroxide obtained at 3438.6cm-1A broad peak, which can be attributed to the association stretching vibration peak of hydroxyl and water, 1634.1cm-1The absorption peak is attributed to the bending stretching vibration peak of hydroxyl and water, which indicates that hydroxyl and water are contained; 1385.6cm-1The absorption peak at (a) is attributed to the stretching vibration peak of nitrate, indicating that the interlayer anion is nitrate; 634.3cm-1The absorption peak at (b) is attributed to the stretching vibration peak of Ti-O, 453.3cm-1The absorption peak belongs to the expansion vibration peak of Ni-O, which shows that the laminate is nickel-titanium double metal hydroxide; and at 1300--1In the range of (1) shows a slight absorption peak of 1214.3cm-1、1115.1cm-1The absorption peak at (b) is assigned to the C-N symmetric stretching vibration peak, 1071.0cm-1、1045.7cm-1The absorption peak at the position is attributed to the stretching vibration peak of C-O, and is 2869.9cm-1A weak absorption peak is attributed to the symmetric stretching vibration peak of methylene and is 911.1cm-1The absorption peaks at (a) were assigned to the out-of-plane bending vibration peaks of the hydroxyl groups, which were characteristic peaks of triethanolamine, indicating that the interlayer was not washed off by a small amount of triethanolamine.
2. The silver oxide/nickel-titanium double hydroxide composites obtained in example 5 and comparative example 3 had both the main characteristic peak of nickel-titanium double hydroxide and the characteristic peak of silver oxide, and after the composite, the silver oxide/nickel-titanium double hydroxide composite was 1385cm-1、1634cm-1The intensity of the absorption peak at (a) becomes weak and the position of the characteristic peak is substantially unchanged.
Fifth, ultraviolet-visible diffuse reflectance spectroscopy (UV-vis DRS) analysis
The applicant adopts a UV-vis DRS map to detect the optical absorption performance of the silver oxide/nickel-titanium double hydroxide compound obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2 and the silver oxide/nickel-titanium double hydroxide compound obtained in comparative example 3; the test was performed on a Lambda 950 model ultraviolet-visible near infrared spectrophotometer, platinum Elmer, Inc. of USA; the results are shown in FIG. 8.
As can be seen from fig. 8: the absorption spectrum of the nickel-titanium double metal hydroxide obtained in the comparative example 1 has two absorption bands which are located in the areas of 200-400nm and 600-800nm and can be respectively attributed to the interlayer charge transfer of octahedral titanium atoms in the nickel-titanium double metal hydroxide structure and the existence of nickel cations of a main layer plate; the silver oxide obtained in comparative example 2 has absorption in the whole visible light region; whereas the absorbance of the silver oxide/nickel-titanium double hydroxide composite obtained in example 5 and comparative example 3 was increased and was greater than that of the nickel-titanium double hydroxide obtained in comparative example 1 and that of the silver oxide obtained in comparative example 2, the absorbance of the silver oxide/nickel-titanium double hydroxide composite was increased with the increase in the silver oxide loading and was absorbed throughout the visible light region, and the silver oxide/nickel-titanium double hydroxide composite showed an enhanced absorption capacity throughout the visible light region.
The applicant processes fig. 8 to obtain a relationship between the absorption coefficient and the photon energy change, and as shown in fig. 9, the forbidden bandwidth of each group of samples can be estimated through the relationship between the photon absorption coefficient and the photon energy change.
Extrapolation from the straight line portion of the graph in FIG. 9 shows that the forbidden bandwidths of the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2, the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, and the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3 are 2.31eV, 1.34eV, 1.27eV, and 1.18eV, respectively.
The results show that the silver oxide/nickel-titanium double metal hydroxide compound obtained by the invention has response under visible light, and the forbidden band width is reduced along with the increase of the silver oxide load, namely, the energy required by photo-generated electron hole pairs generated by visible light excitation is reduced, and the photocatalytic activity is enhanced.
Sixthly, electrochemical test analysis
Taking ITO conductive glass, carrying out ultrasonic treatment in acetone for 30min, then carrying out ultrasonic treatment in ethanol for 30min, finally carrying out ultrasonic treatment with deionized water for 30min, and storing the treated ITO conductive glass in the deionized water for later use. Taking 5mg of a sample to be tested (the silver oxide/nickel-titanium double hydroxide compound obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2 and the silver oxide/nickel-titanium double hydroxide compound obtained in comparative example 3), respectively adding 800 mu L of deionized water, 200 mu L of ethanol and 50 mu L of perfluorosulfonic acid (binder), carrying out ultrasonic treatment for 1h, and standing to obtain an active substance. Drying the ITO conductive glass, placing the dried ITO conductive glass in a watch glass, measuring the conductive surface of the ITO conductive glass by using a digital multimeter, fixing the ITO conductive glass by using an adhesive tape, then transferring 50 mu L of supernatant of active substances by using a liquid transfer gun, and uniformly coating the supernatant on the ITO conductive glass to obtain a working electrode; the test was performed on an electrochemical workstation model CHI-660D of Shanghai Chenghua instruments, Inc.
(1) Photocurrent density (i-t) curve
Photocurrent density is an effective technique for revealing the photoelectron transfer property, and the higher the photocurrent density, the higher the photoelectron separation efficiency. The applicant adopts a three-phase electrode for testing, wherein an Ag/AgCl electrode is used as a reference electrode, a platinum wire electrode is used as a counter electrode, the obtained working electrode is adopted, an electrolyte is 0.2mol/L sodium sulfate solution, and the testing condition is no bias voltage.
The transient photocurrent intensity of the silver oxide/nickel-titanium double hydroxide composite obtained in example 5, the nickel-titanium double hydroxide obtained in comparative example 1, the silver oxide obtained in comparative example 2, and the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3 was measured at on/off cycles, and the results are shown in fig. 10. As can be seen from fig. 10: under visible light illumination, all samples produced photocurrents, indicating that they were able to react to visible light and produce electrons and holes; however, the photocurrent density of the silver oxide/nickel-titanium double hydroxide composite was greater than those of the nickel-titanium double hydroxide and silver oxide, and in contrast, the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3 exhibited the highest photocurrent intensity, indicating that the photoelectron separation efficiency was the highest.
(2) Electrochemical Impedance Spectroscopy (EIS) curve
Electrochemical Impedance Spectroscopy (EIS) studies the charge transfer capability of a sample under visible light illumination. The applicant still adopts a three-phase electrode for testing, wherein an Ag/AgCl electrode is used as a reference electrode, a platinum wire electrode is used as a counter electrode, and the obtained working electrode is adopted; the electrolyte is a mixed solution of potassium ferricyanide, potassium ferrocyanide and potassium chloride; the test conditions were as follows: the initial potential is open circuit potential, and the amplitude is 5 mV; the results are shown in FIG. 11.
Since the arc radius of the ac impedance is smaller, the hindrance of electron-hole transfer is smaller, which means that the charge separation efficiency is higher. As can be seen from fig. 11: the radius sizes are arranged as follows: comparative example 1 resulting nickel-titanium double hydroxide > comparative example 2 resulting silver oxide > silver oxide/nickel-titanium double hydroxide composite obtained in example 5 > silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3.
The above results confirm that: the arc radius of the silver oxide/nickel-titanium double metal hydroxide compound is smaller than that of the nickel-titanium double metal hydroxide and the silver oxide, and the arc radius of the silver oxide/nickel-titanium double metal hydroxide compound obtained in the comparative example 3 is the smallest, which means that the charge transfer resistance of the silver oxide/nickel-titanium double metal hydroxide compound is the smallest and the charge separation efficiency is the highest, corresponding to the result of photocurrent.
(3) Mott-Schottky curve
The applicant used the Mott-Schottky test to confirm the flat band potential and the semiconductor type. The applicant adopts a three-phase electrode for testing, wherein an Ag/AgCl electrode is used as a reference electrode, a platinum wire electrode is used as a counter electrode, the obtained working electrode is adopted, electrolyte is 0.2mol/L sodium sulfate solution, and the testing frequency is 1000 Hz; as shown in fig. 12-15.
As can be seen from fig. 12: the flat band potential of the nickel-titanium double hydroxide obtained in comparative example 1 was about-1.23 eV, while the nickel-titanium double hydroxide obtained in comparative example 1 was considered to be an n-type semiconductor due to the positive slope of the Mott-Schottky curve.
As can be seen from fig. 13: the flat band potential of the silver oxide obtained in comparative example 2 was about 1.32eV, while the Mott-Schottky curve showed a negative slope, indicating that the silver oxide obtained in comparative example 2 was a p-type semiconductor.
As can be seen from fig. 14 and 15: the Mott-Schottky curve of the silver oxide/nickel-titanium double metal hydroxide composite obtained by the invention is in an inverted V shape, and shows that a p-n junction exists in the silver oxide/nickel-titanium double metal hydroxide composite.
Seventhly, degrading ethanethiol by photocatalysis
The applicant adopts a static adsorption-photocatalysis method to adsorb and degrade ethanethiol, and the method specifically comprises the following steps:
drying each group of samples at 80 ℃ for 2h for activation, adsorbing ethanethiol for 1h in a closed space in the dark by each group of activated samples, then turning on a xenon lamp light source (a cut-off filter CEL-UVIRCUT420), carrying out dark treatment for 1h, measuring the framework peaks of each group of adsorbed samples and each group of photocatalytic samples by a Fourier transform infrared spectroscopy (FT-IR), and qualitatively analyzing the photocatalytic degradation performance of the catalyst on ethanethiol.
The test was performed on a Fourier transform infrared spectrometer model ls50 from Saimer fly, USA, using potassium bromide pellets. Scanning range: 4000-400cm-1(ii) a The scanning times are as follows: 32, a first step of removing the first layer; resolution ratio: 4cm-1。
(1) Comparative example 1 analysis of adsorption and photocatalytic Properties of Nickel-titanium double hydroxide on ethanethiol
The change of the skeletal peak after adsorption and photocatalytic oxidation of Ethanethiol (EM) by the nickel-titanium double hydroxide obtained in comparative example 1 was measured by Fourier transform infrared spectroscopy, and the result is shown in FIG. 16, using the corresponding blank sample as a control.
In FIG. 16, a is a graph of the nickel-titanium double hydroxide as it is, b is a graph of the nickel-titanium double hydroxide after adsorption, and c is a graph of the nickel-titanium double hydroxide with visible light after adsorption.
As can be seen from fig. 16: the infrared spectrum of the adsorbed nickel-titanium double metal hydroxide is consistent with the original spectrum of the nickel-titanium double metal hydroxide, which indicates that no organic matter is left on the surface of the adsorbed nickel-titanium double metal hydroxide, and the adsorption of ethanethiol on the surface of the nickel-titanium double metal hydroxide obtained in the comparative example 1 is possibly weak; since no organic matter is attached to the surface of the nickel-titanium double metal hydroxide obtained in comparative example 1, the skeleton peak before and after the catalyst photocatalysis is not observed to be obviously changed in the infrared spectrogram of the nickel-titanium double metal hydroxide obtained in comparative example 1 under the irradiation of visible light.
(2) Comparative example 2 analysis of adsorption and photocatalytic Performance of silver oxide on ethanethiol
The change of the framework peak after the adsorption and photocatalytic oxidation of ethanethiol by silver oxide obtained in comparative example 2 was measured by fourier transform infrared spectroscopy, and the result is shown in fig. 17, using the corresponding blank sample as a control.
In fig. 17, a is a graph of silver oxide as it is, b is a graph of silver oxide obtained after adsorption, and c is a graph of silver oxide irradiated with visible light after adsorption.
As can be seen from fig. 17: the concentrations of the adsorbed ethanethiol and the adsorbed photocatalytic silver oxide were 1258.4cm respectively, as compared with those of the original silver oxide-1、975.6cm-1A new absorption peak appears at the left and right parts and is 1060.8cm-1The intensity of the absorption peak is enhanced. 1258.4cm-1The absorption peak of (A) is attributed to HO-SO2-(CH3CH2-SO2-OH) antisymmetric stretching vibration peak, 975.6cm-1The absorption peak at (A) is attributed to the antisymmetric bending vibration peak of S-O-C, 1060.8cm-1The enhancement of the absorption peak intensity is presumed to be caused by stretching vibration of S ═ O, which indicates that the silver oxide obtained in comparative example 2 is adsorptive to ethanethiol, but weak in adsorption capacity, and that ethanethiol is oxidized to sulfonic acid or sulfonic acid ester or the like under irradiation of visible light.
(3) Comparative example 3 analysis of adsorption and photocatalytic Performance of silver oxide/Nickel-titanium double hydroxide composite on ethanethiol
Changes in the peak of the framework of the silver oxide/nickel-titanium double metal hydroxide composite obtained in comparative example 3 after adsorption of ethanethiol and photocatalytic oxidation were measured by fourier transform infrared spectroscopy, and a corresponding blank sample was used as a control, as shown in fig. 18.
In fig. 18, a is a graph of the silver oxide/nickel-titanium double hydroxide composite as it is, b is a graph of the silver oxide/nickel-titanium double hydroxide composite after adsorption, and c is a graph of the silver oxide/nickel-titanium double hydroxide composite after adsorption in visible light.
As can be seen from fig. 18: with silver oxide/nickel-titanium double hydroxidesCompared with the original composite, the silver oxide/nickel-titanium double metal hydroxide composite after absorbing ethanethiol is respectively 1446.1cm-1、1252.3cm-1、1023.6cm-1、971.2cm-1The new absorption peak appears at the left and right, 1446.1cm-1The absorption peak of (A) belongs to O-SO2-(CH3CH2-SO2-OH) asymmetric stretching vibration peak, 1252.3cm-1The absorption peak of (A) is attributed to HO-SO2-(CH3CH2-SO2-OH) antisymmetric stretching vibration peak, 1023.6cm-1The absorption peak at (A) is assigned to S ═ O (CH)3CH2-SO2OH) stretching vibration peak, 971.2cm-1The absorption peak at (a) is attributed to the peak of S-O-C, which indicates that the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3 can adsorb ethanethiol, and it is presumed that it can oxidize ethanethiol into sulfate, sulfonic acid, sulfonate, etc. under natural light conditions.
The silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3 was 1446.2cm under visible light irradiation-1、1253.1cm-1、1023.5cm-1The new absorption peaks appeared on the left and right, but the intensities of the absorption peaks were decreased, which indicates that the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3 produces a catalytic oxidation reaction on ethanethiol to produce sulfate, sulfonic acid, sulfonate, etc. under the irradiation of visible light, which is consistent with the results under the irradiation of natural light.
(4) Adsorption and photocatalytic Performance analysis of ethanethiol by silver oxide/Nickel-titanium double hydroxide composite obtained in example 5
The changes of the framework peaks after the silver oxide/nickel-titanium double metal hydroxide composite obtained in example 5 was measured by fourier transform infrared spectroscopy for the adsorption of ethanethiol and the photocatalytic oxidation, and the results are shown in fig. 19, using the corresponding blank sample as a control.
In fig. 19, a is a graph of the silver oxide/nickel-titanium double hydroxide composite as it is, b is a graph of the silver oxide/nickel-titanium double hydroxide composite after adsorption, and c is a graph of the silver oxide/nickel-titanium double hydroxide composite after adsorption in visible light.
As can be seen from fig. 19: the concentrations of the silver oxide/nickel-titanium double hydroxide composites after absorbing ethanethiol were 1446.1cm respectively, compared with the silver oxide/nickel-titanium double hydroxide composites as they were-1、1250.6cm-1The new absorption peak appears at the left and right, 1446.1cm-1The absorption peak of (A) belongs to O-SO2-(CH3CH2-SO2-OH) asymmetric stretching vibration peak, 1250.6cm-1The absorption peak of (A) is attributed to HO-SO2-(CH3CH2-SO2-OH), which indicates that the silver oxide/nickel-titanium double hydroxide compound obtained in example 5 can adsorb ethanethiol and oxidize ethanethiol into sulfate, sulfonic acid, sulfonate and the like under natural light conditions.
The silver oxide/nickel-titanium double hydroxide composite obtained in example 5 was also 1449.2cm under visible light irradiation-1、1252.3cm-1New absorption peaks appear at the left and right parts; this shows that under the irradiation of visible light, the silver oxide/nickel-titanium double metal hydroxide composite obtained in example 5 can perform photocatalytic degradation on ethanethiol, and the products after photocatalytic oxidation are sulfates, sulfonic acids, sulfonates, and the like.
In conclusion, the infrared spectrogram of the nickel-titanium double hydroxide obtained in the comparative example 1 does not have a new absorption peak, which indicates that the nickel-titanium double hydroxide does not have adsorption capacity on ethanethiol, so that the nickel-titanium double hydroxide does not have a new absorption peak under the irradiation of visible light; the change of the skeleton peak occurs in the infrared spectrogram of the silver oxide obtained in the comparative example 2, which shows that the silver oxide has the adsorption capacity on ethanethiol, and the ethanethiol is oxidized into sulfonic acid, sulfonic acid ester and the like under the irradiation of visible light; the framework peaks of the infrared spectra of the silver oxide/nickel-titanium double metal hydroxide composites obtained in example 5 and comparative example 3 also change, which indicates that the silver oxide/nickel-titanium double metal hydroxide composites obtained by the invention have adsorption capacity to ethanethiol, the adsorption capacity is stronger than that of silver oxide, and ethanethiol is oxidized into sulfate, sulfonic acid, sulfonate and the like under the irradiation of visible light.
Comparing FIGS. 16-19, it can be seen that: the adsorption and photocatalytic capacities of the four samples on ethanethiol are arranged in sequence as follows: comparative example 3 silver oxide/nickel-titanium double hydroxide composite > silver oxide/nickel-titanium double hydroxide composite obtained in example 5 > silver oxide obtained in comparative example 2 > nickel-titanium double hydroxide obtained in comparative example 1. The above results show that: the silver oxide/nickel-titanium double hydroxide composite obtained in comparative example 3 is best in terms of adsorption and photocatalytic ability to ethanethiol, which is consistent with the results of the transient photocurrent response and alternating current impedance (EIS) measured previously; however, in comparative example 3, the silver oxide ratio is too high, which results in too high cost, and therefore, it is most suitable to select the silver oxide/nickel-titanium double hydroxide composite obtained in example 5.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (11)
1. The silver oxide/layered double hydroxide compound for photocatalytic desulfurization is characterized in that silver oxide is loaded on the surface of layered double hydroxide, the layered double hydroxide is nickel-titanium double hydroxide, the forbidden band width of the silver oxide/layered double hydroxide compound is 1.25-1.30ev, and the mass ratio of the silver oxide to the layered double hydroxide is 0.4-0.6: 1.
2. a method of preparing the silver oxide/layered double hydroxide composite of claim 1, comprising the steps of: mixing nickel salt, titanium salt and triethanolamine, adjusting the pH value of the system to 8-9, heating, condensing and refluxing to obtain nickel-titanium double metal hydroxide; adding silver salt and nickel-titanium double metal hydroxide into a solvent, uniformly mixing, and adjusting to be alkaline to obtain the silver oxide/layered double metal hydroxide compound.
3. The method for preparing a silver oxide/layered double hydroxide complex according to claim 2, wherein the silver salt is silver nitrate or silver fluoride.
4. The method of preparing a silver oxide/layered double hydroxide composite according to claim 2, wherein the solvent is water.
5. The method for preparing a silver oxide/layered double hydroxide composite according to any one of claims 2 to 4, wherein the system is adjusted to be alkaline by using an aqueous solution of sodium hydroxide, an aqueous solution of potassium hydroxide, triethylamine, diethylamine, diethanolamine, triethanolamine or an aqueous solution of urea.
6. The method for preparing a silver oxide/layered double hydroxide composite according to any one of claims 2 to 4, wherein the system is adjusted to be alkaline with an aqueous sodium hydroxide solution.
7. The method for preparing a silver oxide/layered double hydroxide composite according to any one of claims 2 to 4, wherein the adjustment to the basicity is an adjustment of the pH of the system to 13.5 to 14.5.
8. The method for preparing a silver oxide/layered double hydroxide composite according to claim 2, wherein the temperature is raised to 95-100 ℃ and the condensation reflux is carried out for 44-52 hours.
9. The method of claim 2, wherein the nickel salt is at least one of nickel nitrate, nickel sulfate, nickel fluoride, nickel chloride, nickel bromide, and nickel acetate.
10. The method for preparing a silver oxide/layered double hydroxide composite according to claim 2, wherein the titanium salt is at least one of titanium acetate, titanium chloride, titanium fluoride, tetrabutyl titanate, and isopropyl titanate.
11. Use of the silver oxide/layered double hydroxide composite according to claim 1 in the field of photocatalytic desulfurization.
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