CN106283099A - A kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the method for manganese dioxide nano-composite material and application thereof - Google Patents
A kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the method for manganese dioxide nano-composite material and application thereof Download PDFInfo
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- CN106283099A CN106283099A CN201610721311.6A CN201610721311A CN106283099A CN 106283099 A CN106283099 A CN 106283099A CN 201610721311 A CN201610721311 A CN 201610721311A CN 106283099 A CN106283099 A CN 106283099A
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- surfactant
- manganese
- composite material
- electrodeposition
- titanium dioxide
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 94
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000000463 material Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 31
- 239000004094 surface-active agent Substances 0.000 title claims abstract description 29
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 28
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 25
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 20
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 32
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000010936 titanium Substances 0.000 claims abstract description 25
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 25
- 150000002696 manganese Chemical class 0.000 claims abstract description 9
- 239000004064 cosurfactant Substances 0.000 claims abstract description 8
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 7
- 239000003921 oil Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 31
- 239000011259 mixed solution Substances 0.000 claims description 15
- 238000005352 clarification Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 230000036647 reaction Effects 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 235000007079 manganese sulphate Nutrition 0.000 claims description 8
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical group [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 6
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000003945 anionic surfactant Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000003093 cationic surfactant Substances 0.000 claims description 4
- 239000002736 nonionic surfactant Substances 0.000 claims description 4
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical group S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 229940099596 manganese sulfate Drugs 0.000 claims description 3
- 239000011702 manganese sulphate Substances 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- PBLNBZIONSLZBU-UHFFFAOYSA-N 1-bromododecane Chemical compound CCCCCCCCCCCCBr PBLNBZIONSLZBU-UHFFFAOYSA-N 0.000 claims description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 claims description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 2
- 239000013504 Triton X-100 Substances 0.000 claims description 2
- 229920004890 Triton X-100 Polymers 0.000 claims description 2
- PYPCLUOPAQYZSY-UHFFFAOYSA-N [Na].C(CCCCCCCCCCCCCCC)(=O)OC Chemical compound [Na].C(CCCCCCCCCCCCCCC)(=O)OC PYPCLUOPAQYZSY-UHFFFAOYSA-N 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 150000001924 cycloalkanes Chemical class 0.000 claims description 2
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- PMOIAJVKYNVHQE-UHFFFAOYSA-N phosphanium;bromide Chemical compound [PH4+].[Br-] PMOIAJVKYNVHQE-UHFFFAOYSA-N 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 150000003222 pyridines Chemical class 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims 1
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 claims 1
- 239000003599 detergent Substances 0.000 claims 1
- 150000004702 methyl esters Chemical class 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 17
- 238000002360 preparation method Methods 0.000 abstract description 11
- 239000003792 electrolyte Substances 0.000 abstract description 9
- 238000005868 electrolysis reaction Methods 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 5
- 239000012071 phase Substances 0.000 abstract description 5
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 238000012983 electrochemical energy storage Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract description 3
- 229910001437 manganese ion Inorganic materials 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 239000008346 aqueous phase Substances 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 238000006303 photolysis reaction Methods 0.000 abstract description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000012153 distilled water Substances 0.000 description 13
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 11
- 239000007795 chemical reaction product Substances 0.000 description 11
- 239000010949 copper Substances 0.000 description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 230000001105 regulatory effect Effects 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 229960000935 dehydrated alcohol Drugs 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical class [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000000593 microemulsion method Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- JHJUUEHSAZXEEO-UHFFFAOYSA-M sodium;4-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=C(S([O-])(=O)=O)C=C1 JHJUUEHSAZXEEO-UHFFFAOYSA-M 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- ZVZFHCZCIBYFMZ-UHFFFAOYSA-N 6-methylheptoxybenzene Chemical compound CC(C)CCCCCOC1=CC=CC=C1 ZVZFHCZCIBYFMZ-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 206010011376 Crepitations Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- ICBUGLMSHZDVLP-UHFFFAOYSA-N [Si]=O.[Mn] Chemical compound [Si]=O.[Mn] ICBUGLMSHZDVLP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- -1 n-octyl alcohols Chemical class 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 230000010349 pulsation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 1
- 238000005199 ultracentrifugation Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/21—Manganese oxides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Metallurgy (AREA)
- Electrochemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the method for manganese dioxide nano-composite material, with manganese salt solution as aqueous phase, microemulsion is formed as electrolyte solution with surfactant, cosurfactant, oil phase, utilize potentiostatic electrodeposition method, prepare for titanium source with titanium sheet;By changing the composition of microemulsion, manganese ion and the concentration of fluorion, decomposition voltage size, the pattern of electrolysis time regulation composite, size, the method selects cheap reagent as raw material, under room temperature microemulsion electrolyte environment, reaction prepares composite, solve the high-temperature process pattern to product and the problem of stability influence, there is preparation technology simple, with low cost, quickly, energy-conservation, the advantage that efficiency is high, obtained composite is expected at photolysis water hydrogen, degradable organic pollutant, electrochemical energy storage, environmental energy is catalyzed, the fields such as battery material obtain and are widely applied.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, more particularly, to a kind of surfactant assist in electrodeposition
Synthesizing anatase type titanium dioxide and the method for manganese dioxide nano-composite material and application.
Background technology
Manganese dioxide is cheap and easy to get, rich reserves, environmental friendliness, is widely used as the electrode material of ultracapacitor, but
MnO2Relatively big as internal resistance during electrode material for super capacitor, crystal grain is relatively big, and in electrode process, utilization rate is on the low side.As
What overcomes electrode material self-defect, improves the utilization rate in electrode process, plays it at electrode of super capacitor material
Advantage in material, is the key issue in studying about electrode material at present.
TiO2Photocatalyst is owing to having good chemical stability, higher photocatalytic activity, low cost, chemical property
Stable, chemically-resistant and photochemical corrosion and nontoxic feature, in recent years, become a kind of environmental type favored by people
Photocatalyst.But TiO2Greater band gap (Eg=3.0~3.2 eV), only <ultraviolet light of 387 nm just can make it to wavelength X
Excite, and sunlight medium ultraviolet luminous energy proportion is less than 5%, thus the utilization rate of solar energy is low;Further, since light excites product
Raw light induced electron and hole are easily combined, and cause photocatalysis efficiency low.TiO2Reaction is had important by character and the structure on surface
Impact, catalyst surface exist lattice defect be necessary for light-catalyzed reaction.
Semiconductors coupling is to improve TiO2One of effective means of photocatalysis efficiency, it is substantially another kind of granule pair
TiO2Modification.Composite semiconductor not only extends the photoresponse scope of wide band gap semiconducter, and have adjusted photo-generated carrier
The flow direction.The semiconductors coupling that quasiconductor that band-gap energy is big is little with band-gap energy, not only extend to visible region by photoresponse, and
And by electronics and void coalescence at different granules by separation of charge, restrained effectively the compound of photo-generated carrier, improve
The electrostatic charge transfer efficiency at quasiconductor-electrolyte solution interface, thus extend the absorption region to spectrum.So, compound
Quasiconductor nearly all shows the photocatalytic activity higher than single quasiconductor.Manganese dioxide and the system of composite titania material
Standby, it is expected to apply at photocatalysis, electro-catalysis, photoelectrocatalysis, energy environment, sensor, ultracapacitor and lithium ion battery etc.
Field plays an increasingly important role.
The preparation method of composite is common to be had: sol-gel process, solid phase method, electrochemical deposition method, microemulsion method, hydro-thermal
Method, template etc.;Electrochemical deposition method refers to that metal or metallic compound, at substrate deposit, by controlling deposition velocity, obtain
Thin film silicon oxide manganese or the method for its compound to different consistency.The method a direct step can make electrode, but electric
Deposition process is not readily susceptible to control, and causes the film thickness of manganese dioxide and pattern uniform not, compares after Overheating Treatment
A large amount of crackles etc. easily occur.Want to obtain preferable manganese dioxide, can be by regulating solution concentration and electric current density one
Determine to solve in degree the problems referred to above, and obtain or the fine and close or thin film of porous;Microemulsion method is first by precipitant and metal salinity
Be not dissolved in identical microemulsion, mix under certain condition, by control in the reaction zone of microemulsion system micelle nucleation,
Growth, obtains the emulsion of nanoparticle, then by product ultracentrifugation, separates nanometer powder and microemulsion.Finally remove and be attached to
Oil on nanometer powder surface and surfactant, be dried and process the solid sample that i.e. can get nanoparticle.Microemulsion method
Feature be prepared nanopowder particles particle diameter little and uniform, stability is high, good dispersion, it is easy to accomplish High Purity.
Reaction temperature height, length reaction time, products therefrom shape is there is in prior art in composite titania material preparation
The defect that looks heterogeneity, stability are the best, photocatalytic is low.
Summary of the invention
The technical problem to be solved be overcome in prior art composite preparation exist reaction temperature high,
Reaction time length, products therefrom pattern heterogeneity, the defect such as stability is the best, photocatalytic is low, it is provided that a kind of surfactant
Assist in electrodeposition synthesizing anatase type titanium dioxide and the method for manganese dioxide nano-composite material.
Second object of the present invention is to provide titanium dioxide that said method prepares and manganese dioxide nano is combined
Material.
Third object of the present invention is to provide the application of above-mentioned titanium dioxide and manganese dioxide nano-composite material.
It is an object of the invention to be achieved by the following technical programs:
A kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the method for manganese dioxide nano-composite material,
It is characterized in that, comprise the following steps:
(1) surfactant, cosurfactant, oil phase are formed solution A with continuous stirring;
(2) manganese salt, villiaumite and disodiumedetate are formed solution B with continuous stirring, solution B is added dropwise to solution A
In, the mixed solution formed during second time clarification is microemulsion C;
(3) with titanium sheet as anode, using microemulsion C as electrolyte solution, voltage range is 0.5~10V to carry out cell reaction extremely
Electrolyte solution becomes cloudy;Titanium sheet after collection cell reaction is complete, cleaned, drying to obtain product;
Step (1) described surfactant, cosurfactant, the mass ratio of oil phase are 1:0.5~20:0.5~40;Step
(2) concentration of described manganese salt is 0.01~0.9 mol/L;The concentration of villiaumite is 0.05~2.0 mol/L;Described ethylenediamine tetrem
The addition of acid disodium is the amount dissolved so that manganese salt.
When the present invention is by changing the composition of microemulsion, manganese ion and the concentration of fluorion, the size of decomposition voltage, electrolysis
Between regulate the pattern of composite to be obtained, size and size, final to obtain pattern homogeneous, the composite wood of good stability
Material.
Specifically, described step (2) forms mixed solution after solution B instills solution A, and this mixed solution first passes through muddiness
To clarification more muddy, clarifying process again, the mixed solution formed during second time clarification is microemulsion C;Microemulsion now is water
Oil-in, could be used for the electrolyte as electrochemical deposition.
Preferably, described surfactant is selected from cationic surfactant, anion surfactant or nonionic
Surfactant.
Preferably, described cationic surfactant is selected from cetyl trimethylammonium bromide (CTAB), tetramethyl chlorination
Ammonium, bromododecane yl pyridines, dodecyl tributyl bromide phosphine etc..
Preferably, described anion surfactant selected from sodium lauryl sulphate (SDS), dodecylbenzene sodium sulfonate,
Fatty alcohol-ether sodium sulfate, methyl hexadecanoate sodium sulfonate etc..
Preferably, described nonionic surfactant is selected from Triton X-100, Span 60, Tween 80, cocinic acid first
Ester polyoxyethylene ether etc..
Preferably, step (1) described cosurfactant be carbon number be the alcohol of 3~24.
Preferably, step (1) described oil phase be carbon number be alkane or the cycloalkane of 3~24.
Preferably, step (2) described manganese salt is manganese sulfate or manganese chloride or other salt containing manganese, and villiaumite is ammonium fluoride or fluorine
Change sodium or other fluorine-containing salt.
Preferably, the purity of described titanium sheet is more than 95%.
The present invention also provides for titanium dioxide and the manganese dioxide nano-composite material that said method obtains.
The present invention also provides for the application of described titanium dioxide and manganese dioxide nano-composite material, specifically, can be light
Solve the application in terms of the fields such as water hydrogen manufacturing, degradable organic pollutant, electrochemical energy storage, environmental energy catalysis, battery material.
Compared with prior art, the method have the advantages that
The invention provides a kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and manganese dioxide nano is multiple
The method of condensation material, is with the aqueous solution of manganese containing salt as aqueous phase, and surfactant, cosurfactant, oil phase form microemulsion
Liquid, as electrolyte solution, utilizes potentiostatic electrodeposition method, with titanium sheet for titanium source, prepares the nanometer of titanium dioxide and manganese dioxide
Composite;Come by the change composition of microemulsion, manganese ion and the concentration of fluorion, the size of decomposition voltage, electrolysis time
Regulate the pattern of composite to be obtained, size and size, the method select cheap reagent as raw material, micro-in room temperature
React under emulsion electrolyte environment, prepare anatase titanium dioxide and manganese dioxide nano-composite material, solve at high temperature
Manage the pattern of product and the problem of stability influence, have that preparation technology is simple, with low cost, quick, energy-conservation, efficiency is high
Advantage, obtained composite be expected to photolysis water hydrogen, degradable organic pollutant, electrochemical energy storage, environmental energy catalysis,
The fields such as battery material obtain and are widely applied.
Accompanying drawing explanation
Fig. 1 is embodiment 1 prepared anatase titanium dioxide and the X-ray powder of manganese dioxide nano-composite material
Diffraction (XRD) figure.
Fig. 2 is embodiment 2 prepared anatase titanium dioxide and the X-ray powder of manganese dioxide nano-composite material
Diffraction (XRD) figure.
Fig. 3 is that the scanning electron of the prepared anatase titanium dioxide of embodiment 1 and manganese dioxide nano-composite material shows
Micro mirror (SEM) figure.
Fig. 4 is that the scanning electron of the prepared anatase titanium dioxide of embodiment 2 and manganese dioxide nano-composite material shows
Micro mirror (SEM) figure.
Fig. 5 is embodiment 1 prepared anatase titanium dioxide and the energy dispersion light of manganese dioxide nano-composite material
Spectrum (EDS) figure.
Fig. 6 is embodiment 2 prepared anatase titanium dioxide and the energy dispersion light of manganese dioxide nano-composite material
Spectrum (EDS) figure.
Detailed description of the invention
Below by Figure of description and specific embodiment specific descriptions further to the present invention.The design philosophy of the present invention
Or simple replacement of allied substances belongs to protection scope of the present invention.If following used experimental technique is without specified otherwise, all
For the method for the existing routine of the art, the dispensing used or material, if no special instructions, being can by commercial sources
The dispensing obtained or material, all reagent are analytical pure.
Embodiment 1
A kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the preparation of manganese dioxide nano-composite material
Method, comprises the steps:
(1) in a beaker, add 7.5 g sodium lauryl sulphates (SDS), 37.5 g glycerol, normal hexane 10 mL, stir
Mix uniformly, obtain solution A;
(2) in another beaker, 2.5 g manganese sulfates, 5 g ammonium fluorides, 3 g disodiumedetate (EDTA bis-are added
Sodium), appropriate distilled water, stir, be settled in 500 mL volumetric flasks, obtain solution B;
(3) solution B being added dropwise in solution A, the mixed solution of formation first passes through muddy to clarification, more muddy, clarifying process again,
The mixed solution formed during second time clarification is microemulsion C.Regulated power supply is adjusted to 2.5 V, and the titanium sheet of 2 × 3 cm is anode, 2
The copper sheet of × 3 cm is negative electrode, and microemulsion C is electrolyte, starts cell reaction, and the time is 2 hours.After reaction terminates, collect titanium
Sheet, cleans each three times with dehydrated alcohol and distilled water, at room temperature natural drying, obtains end product.
To product use Germany Bruker company produce D8 ADVANCE type X-ray powder diffractometer (XRD) (λ Cu=
0.15418 nm) carry out Crystalline form analysis (such as Fig. 1), result shows: products therefrom is anatase titanium dioxide.
Embodiment 2
A kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the preparation of manganese dioxide nano-composite material
Method, comprises the steps:
(1) in a beaker, 20 g cetyl trimethylammonium bromide (CTAB), 100 g glycerol, normal hexane 50 are added
ML, stirs, and obtains solution A;
(2) in another beaker, 2.5 g manganese sulfates, 5 g ammonium fluorides, 3 g disodiumedetate (EDTA bis-are added
Sodium), appropriate distilled water, stir, be settled in 500 mL volumetric flasks, obtain solution B;
(3) B solution being added dropwise in solution A, the mixed solution of formation first passes through muddy to clarification, more muddy, clarifying process again,
The mixed solution formed during second time clarification is microemulsion C.Regulated power supply is adjusted to 2.5 V, and the titanium sheet of 2 × 3 cm is anode, 2
The copper sheet of × 3 cm is negative electrode, and microemulsion C is electrolyte, starts cell reaction, and the time is 2 hours.After reaction terminates, collect titanium
Sheet, cleans each three times with dehydrated alcohol and distilled water, at room temperature natural drying, obtains end product.
To product use Germany Bruker company produce D8 ADVANCE type X-ray powder diffractometer (XRD) (λ Cu=
0.15418 nm) carry out Crystalline form analysis (such as Fig. 2), result shows: products therefrom is anatase titanium dioxide.
Embodiment 3
A kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the preparation of manganese dioxide nano-composite material
Method, comprises the steps:
(1) in a beaker, adding 10 g dodecylbenzene sodium sulfonate, 30 g n-butyl alcohol, normal heptane 40 mL, stirring is all
Even, obtain solution A;
(2) in another beaker, 2.5 g manganese sulfates, 5 g ammonium fluorides, 3 g disodiumedetate (EDTA bis-are added
Sodium), appropriate distilled water, stir, be settled in 500 mL volumetric flasks, obtain solution B;
(3) B solution being added dropwise in solution A, the mixed solution of formation first passes through muddy to clarification, more muddy, clarifying process again,
The mixed solution formed during second time clarification is microemulsion C.Regulated power supply is adjusted to 5 V, and the titanium sheet of 2 × 3 cm is anode, 2 ×
The copper sheet of 3 cm is negative electrode, and microemulsion C is electrolyte, starts cell reaction, and the time is 1 hour.After reaction terminates, collect titanium
Sheet, cleans each three times with dehydrated alcohol and distilled water, at room temperature natural drying, obtains end product.
Embodiment 4
A kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the preparation of manganese dioxide nano-composite material
Method, comprises the steps:
(1) in a beaker, add 15 g Tween 80s, 30 g n-octyl alcohols, hexamethylene 40 mL, stir, obtain solution A;
(2) in another beaker, 2.5 g manganese sulfates, 5 g ammonium fluorides, 3 g disodiumedetate (EDTA bis-are added
Sodium), appropriate distilled water, stir, be settled in 500 mL volumetric flasks, obtain solution B;
(3) B solution being added dropwise in solution A, the mixed solution of formation first passes through muddy to clarification, more muddy, clarifying process again,
The mixed solution formed during second time clarification is microemulsion C.Regulated power supply is adjusted to 5 V, and the titanium sheet of 2 × 3 cm is anode, 2 ×
The copper sheet of 3 cm is negative electrode, and microemulsion C is electrolyte, starts cell reaction, and the time is 1 hour.After reaction terminates, collect titanium
Sheet, cleans each three times with dehydrated alcohol and distilled water, at room temperature natural drying, obtains end product.
Embodiment 5
A kind of surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the preparation of manganese dioxide nano-composite material
Method, comprises the steps:
(1) in a beaker, add 10 g Polyethylene Glycol to isooctyl phenyl ether (triton x-100), 35 g hexanol,
Normal octane 30 mL, stirs, obtains solution A;
(2) in another beaker, 2.5 g manganese sulfates, 5 g ammonium fluorides, 3 g disodiumedetate (EDTA bis-are added
Sodium), appropriate distilled water, stir, be settled in 500 mL volumetric flasks, obtain solution B;
(3) B solution being added dropwise in solution A, the mixed solution of formation first passes through muddy to clarification, more muddy, clarifying process again,
The mixed solution formed during second time clarification is microemulsion C.Regulated power supply is adjusted to 2.5 V, and the titanium sheet of 2 × 3 cm is anode, 2
The copper sheet of × 3 cm is negative electrode, and microemulsion C is electrolyte, starts cell reaction, and the time is 2 hours.After reaction terminates, collect titanium
Sheet, cleans each three times with dehydrated alcohol and distilled water, at room temperature natural drying, obtains end product.
Comparative example 1
Experimental technique with embodiment 1, unique unlike, the consumption of manganese sulfate is 85 g, with the prepared microemulsion of this comparative example
C, is adjusted to 2.5 V by regulated power supply, and the titanium sheet of 2 × 3 cm is anode, and the copper sheet of 2 × 3 cm is negative electrode, and microemulsion C is electrolysis
Liquid, starts cell reaction, and the time is 2 hours.After reaction terminates, collect titanium sheet, clean each three times with dehydrated alcohol and distilled water,
At room temperature natural drying, obtains end product.
The result of end product: characterize the composite obtained with SEM, finds composite material surface thickness relatively
, there is crackle and caking in thickness, affects the overall performance of composite.
Comparative example 2
Experimental technique with embodiment 1, unique unlike, the consumption of ammonium fluoride is 50 g, with the prepared microemulsion of this comparative example
C, is adjusted to 2.5 V by regulated power supply, and the titanium sheet of 2 × 3 cm is anode, and the copper sheet of 2 × 3 cm is negative electrode, and microemulsion C is electrolysis
Liquid, starts cell reaction, and the time is 2 hours.After reaction terminates, collect titanium sheet, clean each three times with dehydrated alcohol and distilled water,
At room temperature natural drying, obtains end product.
The result of end product: characterize the composite obtained with SEM, finds that composite material surface corrosion is tight
Weight, its microstructure is destroyed, affects the overall performance of composite.
Comparative example 3
Experimental technique with embodiment 1, unique unlike, the consumption of SDS is 1 g, and the consumption of glycerol is 30 g, normal hexane
Consumption is 60 g, the microemulsion C prepared by this comparative example, and regulated power supply is adjusted to 2.5 V, and the titanium sheet of 2 × 3 cm is anode, 2
The copper sheet of × 3 cm is negative electrode, and microemulsion C is electrolyte, starts cell reaction, and the time is 2 hours.After reaction terminates, collect titanium
Sheet, cleans each three times with dehydrated alcohol and distilled water, at room temperature natural drying, obtains end product.
The result of end product: cannot obtain stable microemulsion, during electrolysis, voltage pulsation is relatively big, SEM and EDS characterizes knot
Fruit display, the most successfully upper manganese dioxide of load.
Claims (10)
1. a surfactant assist in electrodeposition synthesizing anatase type titanium dioxide and the side of manganese dioxide nano-composite material
Method, it is characterised in that comprise the following steps:
(1) surfactant, cosurfactant, oil phase are formed solution A with continuous stirring;
(2) manganese salt, villiaumite and disodiumedetate are formed solution B with continuous stirring, solution B is added dropwise to solution A
In, the mixed solution formed during second time clarification is microemulsion C;
(3) with titanium sheet as anode, using microemulsion C as electrolyte solution, voltage range is 0.5~10V to carry out cell reaction extremely
Electrolyte solution becomes cloudy;Titanium sheet after collection cell reaction is complete, cleaned, drying to obtain product;
Step (1) described surfactant, cosurfactant, the mass ratio of oil phase are 1:0.5~20:0.5~40;Step
(2) concentration of described manganese salt is 0.01~0.9 mol/L;The concentration of villiaumite is 0.05~2.0 mol/L;Described ethylenediamine tetrem
The addition of acid disodium is the amount dissolved so that manganese salt.
Surfactant assist in electrodeposition synthesizing anatase type titanium dioxide the most according to claim 1 and manganese dioxide are received
The method of nano composite material, it is characterised in that step (1) described surfactant is selected from cationic surfactant, anion
Surfactant or nonionic surfactant.
Surfactant assist in electrodeposition synthesizing anatase type titanium dioxide the most according to claim 2 and manganese dioxide are received
The method of nano composite material, it is characterised in that described cationic surfactant is selected from cetyl trimethylammonium bromide, tetramethyl
Ammonium chloride, bromododecane yl pyridines or dodecyl tributyl bromide phosphine.
Surfactant assist in electrodeposition synthesizing anatase type titanium dioxide the most according to claim 2 and manganese dioxide are received
The method of nano composite material, it is characterised in that described anion surfactant is selected from sodium lauryl sulphate, detergent alkylate
Sodium sulfonate, fatty alcohol-ether sodium sulfate or methyl hexadecanoate sodium sulfonate.
Surfactant assist in electrodeposition synthesizing anatase type titanium dioxide the most according to claim 2 and manganese dioxide
The method of nano composite material, it is characterised in that described nonionic surfactant is selected from Triton X-100, Span 60, tells
Temperature 80 or cocinic acid methyl ester polyoxyethylene ether.
Surfactant assist in electrodeposition synthesizing anatase type titanium dioxide the most according to claim 1 and manganese dioxide are received
The method of nano composite material, it is characterised in that step (1) described cosurfactant be carbon number be the alcohol of 3~24.
Surfactant assist in electrodeposition synthesizing anatase type titanium dioxide the most according to claim 1 and manganese dioxide are received
The method of nano composite material, it is characterised in that step (1) described oil phase be carbon number be alkane or the cycloalkane of 3~24.
Surfactant assist in electrodeposition synthesizing anatase type titanium dioxide the most according to claim 1 and manganese dioxide are received
The method of nano composite material, it is characterised in that step (2) described manganese salt is manganese sulfate or manganese chloride, and villiaumite is ammonium fluoride or fluorine
Change sodium.
9. described in any one of claim 1 to 8 method obtain titanium dioxide and manganese dioxide nano-composite material.
10. titanium dioxide described in claim 9 and the application of manganese dioxide nano-composite material.
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