CN108483495A - 一种BiOF材料的制备方法及其应用 - Google Patents
一种BiOF材料的制备方法及其应用 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 46
- 229910016295 BiOF Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 8
- 239000011737 fluorine Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000003814 drug Substances 0.000 claims abstract description 4
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 4
- 239000000049 pigment Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical group [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 5
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 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 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical group [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- 239000010431 corundum Substances 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- -1 fluoride ion Compound Chemical class 0.000 claims description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229920002866 paraformaldehyde Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 235000013024 sodium fluoride Nutrition 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 235000000346 sugar Nutrition 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 239000003570 air Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 claims description 2
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- KVBCYCWRDBDGBG-UHFFFAOYSA-N azane;dihydrofluoride Chemical compound [NH4+].F.[F-] KVBCYCWRDBDGBG-UHFFFAOYSA-N 0.000 claims 1
- 229940031098 ethanolamine Drugs 0.000 claims 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical group [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims 1
- 239000004094 surface-active agent Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000003682 fluorination reaction Methods 0.000 abstract description 2
- 238000000713 high-energy ball milling Methods 0.000 abstract description 2
- 238000006479 redox reaction Methods 0.000 abstract description 2
- 230000001360 synchronised effect Effects 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 9
- 238000001914 filtration Methods 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- 229940073609 bismuth oxychloride Drugs 0.000 description 2
- IPNGSXQUQIUWKO-UHFFFAOYSA-N bismuth;fluoro hypofluorite Chemical compound [Bi].FOF IPNGSXQUQIUWKO-UHFFFAOYSA-N 0.000 description 2
- 230000031709 bromination Effects 0.000 description 2
- 238000005893 bromination reaction Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 2
- 125000000913 palmityl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 235000003270 potassium fluoride Nutrition 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical class [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000010303 mechanochemical reaction Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 150000003385 sodium Chemical class 0.000 description 1
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical class [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- ZSDSQXJSNMTJDA-UHFFFAOYSA-N trifluralin Chemical compound CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O ZSDSQXJSNMTJDA-UHFFFAOYSA-N 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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Abstract
本发明涉及一种BiOF材料的制备方法及其应用。本发明以铋酸盐、还原剂、氟源、助剂为原料，将高能球磨的机械力同步作用于氧化还原与氟化反应，再经过热处理、洗涤除杂、固液分离、干燥制备出BiOF材料。所制备的BiOF材料由2～500nm纳米片或纳米颗粒构成，比表面积为3～300m2/g。本发明具有工艺简单、易于工业化生产、制造工艺成本低、环境友好等优势；所制备的BiOF材料在超级电容器、碱性二次电池、锂离子电池、光催化剂、珠光颜料、医药等领域具有广泛应用。
Description
技术领域
本发明涉及一种BiOF材料的制备方法及其应用，属于新型功能材料领域。
背景技术
氟氧化铋是一种重要的功能材料，由于其独特的微观结构及物理化学性质，并且无毒、成本低，将广泛应用在电极活性材料、催化剂、颜料、化妆品、气体传感器、电子材料、医药材料等领域。
材料的结构与性能与制备工艺方法密切相关。目前合成超细功能粉体的方法根据合成原理可分为物理法和化学法。物理法可制得粒径易控的超细粒子，但所需设备昂贵；化学法成本低，易于通过过程控制调整粒子大小，但工艺流程复杂、并有可能带来环境污染。机械化学法是将物理法与化学法相结合，其基本原理是反应物质通过研磨过程提供的能量，提高反应物的化学活性，使得通常需要在高温下进行的反应能在较低温度下快速进行。机械化学合成方法是一种价格低廉、环境友好、高效率和可控性高的合成方法，这一制备方法使得材料的结构与性能具有更多的设计可能性、且易于工业化生产。
Su等[Scripta Materialia 62(2010)345-348]以硝酸铋、氟化铵为原料，乙二醇为溶剂，采用液相沉淀及后续的热处理方法制备出BiOF材料并在紫外光下研究了它的光催化性能。Matar等[Solid State Ionics11(1983)77-81]以Bi2O3和BiF3为原料，通过600℃的高温固相法制备出BiOF材料。Teng等[RSC Adv.5(2015)88936-88942]以硝酸铋、氟化铵为原料，乙醇为溶剂，通过溶剂热法制备出(002)晶面暴露的BiOF纳米材料，并研究了在紫外光下降解罗丹明B的光催化性能。
发明专利[申请公布号CN104148094A]公开了“一种氟氧化铋/石墨烯复合可见光催化剂的制备方法”，该发明用乙二醇分别溶解硝酸铋和氟化钠，采用水解沉淀法制备出氟氧化铋。发明专利[申请公布号CN104891444A]公开了“一种制备BiOF光催化剂的方法及催化剂作用”，该发明以四氢呋喃水溶液为溶剂，以硝酸铋和氢氟酸为原料，通过水热法合成了BiOF光催化剂。
目前只有少量关于BiOF材料的制备研究，主要有水热法，溶剂热法等。但是这些方法普遍存在合成过程复杂，成本高，生产过程中会产生有害副产物，不适合大量生产等问题。
发明内容
本发明的目的在于提供一种BiOF材料的制备方法及其应用。将高能球磨的机械力同步作用于氧化还原与氟化反应，再经过热处理、洗涤除杂、固液分离、干燥制备出BiOF材料。
本发明通过以下技术方案实现：
一种BiOF材料的制备方法，包括如下步骤：
(1)将铋酸盐、还原剂、氟源和助剂按1:(0.25～2):(1～2):(0.001～0.3)的摩尔比(物质的量之比)混合均匀，得到原料混合物；
(2)将步骤(1)所得原料混合物和磨球按1:(1～100)的质量比放入球磨机中，在保护气氛下球磨0.2h～20h；
(3)将步骤(2)得到的球磨混合物置于高温炉中在100～600℃下热处理0.5～10h，将热处理后的产物分别用蒸馏水和无水乙醇进行洗涤除杂，然后进行固液分离、干燥，即得BiOF材料。
进一步地，所述的铋酸盐为铋酸钠、铋酸锂、铋酸钾、铋酸镁中的一种或两种以上。
进一步地，所述的氟源为含氟离子的化合物，优选氟化钠、氟化钾、氟化铵、氟化氢铵、氟化氢中的一种或两种以上。
进一步地，所述的还原剂为金属铋粉、碳粉、亚硫酸盐、甲醛(或多聚甲醛)、甲酸、还原糖、苯酚中的一种或两种以上。
进一步地，所述助剂为十二烷基磺酸钠、十二烷基苯磺酸钠、十六烷基三甲基溴化铵、聚乙烯吡咯烷酮、聚乙二醇、聚乙烯醇、三乙醇胺、乙二醇、丙三醇、非离子型表面活性剂、糖类物质、可溶性淀粉中的一种或两种以上。
进一步地，所述的保护气氛为氮气、氩气、二氧化碳、空气中的一种或两种以上。
进一步地，球磨机的转速为30～3000rpm。
进一步地，所述的球磨机选自市场上的各种机型；所述的磨球为玛瑙球、刚玉球、氧化锆球、瓷球、不锈钢球中的一种或两种以上。
上述制备方法所得到的BiOF材料在超级电容器、碱性二次电池、锂离子电池、光催化剂、医药等领域中的应用。
本发明的有益效果在于：
(1)本发明方法制备工艺简单、工艺条件较温和、易于工业化生产、生产过程环境友好，产品纯度高、产品微观形貌结构及大小易于控制。
(2)本发明所制备的氯氧化铋材料应用广泛，能够应用的领域包括但不限于在超级电容器、碱性二次电池、锂离子电池、光催化剂、珠光颜料、医药等领域。
附图说明
图1为实施例1所制备的BiOF材料的扫描电子显微镜图。
图2为实施例2所制备的BiOF材料的X射线衍射图。
图3为实施例3中BiOF/炭超级电容电池在不同电流密度下的恒电流充放电
测试图。
图4为实施例4所制备的BiOF材料的氮吸脱附等温线图。
具体实施方式
下面以具体实施例进一步说明本发明的技术方案，但本发明并不局限于实施例。
实施例1
(1)将2mmol铋酸钠，1mmol金属铋粉，2mmol氟化钾，0.15mmol聚乙烯吡咯烷酮混合均匀，得到原料混合物；将原料混合物和刚玉磨球按1:50的质量比加到球磨机中，通入空气，在转速为1000rpm条件下进行球磨8h，将球磨后的混合物在300℃下恒温热处理5h，再将热处理产物用去离子水和无水乙醇洗涤除杂、采用过滤进行固液分离，最后将过滤所得的固体产物在110℃下干燥12h制备出BiOF材料。
(2)采用JEOLJEM-3010型扫描电子显微镜对实施例1所得BiOF材料进行表征，如图1所示，BiOF材料由10～20nm的纳米片状堆积组成。
实施例2
(1)将2mmol铋酸钾，2mmol亚硫酸钠，2mmol氟化铵，0.1mmol聚乙二醇混合均匀，得到原料混合物；将原料混合物和瓷质磨球按1:100的质量比加到球磨机中，通入氮气，在转速为1500rpm条件下进行球磨4h，将球磨后的混合物在450℃下恒温热处理4h，再将热处理产物用去离子水和无水乙醇洗涤除杂、采用过滤进行固液分离，最后将过滤所得的固体产物在100℃下真空干燥8h制备出BiOF材料。
(2)采用XRD-6000型X-射线衍射仪对实施例2所制备的BiOF材料进行测试，如图2所示，所得BiOF产品晶相纯净，无其它杂质峰，结晶度好。
实施例3
(1)将2mmol铋酸镁，2mmol多聚甲醛，2mmol氟化钠，0.05mmol十六烷基三甲基溴化铵混合均匀，得到原料混合物；将原料混合物和氧化锆磨球按1:60的质量比加到球磨机中，通入氩气，在转速为1200rpm条件下进行球磨6h，将球磨后的混合物在300℃下恒温热处理3h，再将热处理产物用去离子水和无水乙醇洗涤除杂、采用过滤进行固液分离，最后将过滤所得的固体产物在100℃下干燥8h制备出BiOF材料。
(2)采用上海辰华公司生产的CHI660A电化学工作站，将实施例3所制备的BiOF样品及活性炭分别制成电极片，采用6mol/L KOH溶液为电解质，组装成BiOF/炭超级电容电池，对所构造的电容电池在室温下进行恒流充放电测试。由图3可知，BiOF/炭超级电容电池在0.5A/g的电流密度下比容量达到138mAh/g，在电流密度为1、2、5A/g时的比容量分别为131、127、100mAh/g。
实施例4
(1)将2mmol铋酸钠，1mmol还原糖，2mmol氟化氢铵混合均匀得到原料混合物；将原料混合物和不锈钢磨球按1:50的质量比加到球磨机中，通入空气，在转速为800rpm条件下进行球磨10h，将球磨后的混合物在400℃下恒温热处理3h，再将热处理产物用去离子水和无水乙醇洗涤除杂、采用过滤进行固液分离，最后将过滤所得的固体产物在110℃下干燥9h制备出BiOF材料。
(2)采用TriStar II 3020型比表面积和孔径分布仪对实施例4所得样品材料进行测试，如图4所示，氯氧化铋材料的比表面积为20.4m2/g。
Claims (10)
1.一种BiOF材料的制备方法，其特征在于，所述的BiOF材料由2～500nm纳米片或纳米颗粒构成，比表面积为3～300m2/g；其制备方法包括如下步骤：
(1)将铋酸盐、还原剂、氟源和助剂按1:(0.25～2):(1～2):(0.001～0.3)的摩尔比混合均匀，得到原料混合物；
(2)将步骤(1)所得原料混合物和磨球按1:(0.5～100)的质量比放入球磨机中，在保护气氛下球磨0.2h～20h；
(3)将步骤(2)得到的球磨混合物置于高温炉中在100～600℃下热处理0.5～10h，将热处理后的产物分别用蒸馏水和无水乙醇进行洗涤除杂，然后进行固液分离、干燥，即得BiOF材料。
2.根据权利要求1所述的BiOF材料的制备方法，其特征在于，所述的铋酸盐为铋酸钠、铋酸锂、铋酸钾、铋酸镁中的一种或两种以上。
3.根据权利要求1所述的BiOF材料的制备方法，其特征在于，所述的氟源为含氟离子的化合物。
4.根据权利要求1所述的BiOF材料的制备方法，其特征在于，所述的氟源为氟化钠、氟化钾、氟化铵、氟化氢铵、氟化氢中的一种或两种以上。
5.根据权利要求1所述的BiOF材料的制备方法，其特征在于，所述的还原剂为金属铋粉、碳粉、亚硫酸盐、甲醛、多聚甲醛、甲酸、还原糖、苯酚中的一种或两种以上。
6.根据权利要求1所述的BiOF材料的制备方法，其特征在于，所述助剂为十二烷基磺酸钠、十二烷基苯磺酸钠、十六烷基三甲基溴化铵、聚乙烯吡咯烷酮、聚乙二醇、聚乙烯醇、三乙醇胺、乙二醇、丙三醇、非离子型表面活性剂、糖类物质、可溶性淀粉中的一种或两种以上。
7.根据权利要求1所述的BiOF材料的制备方法，其特征在于，所述的保护气氛为氮气、氩气、二氧化碳、空气中的一种或两种以上。
8.根据权利要求1所述的BiOF材料的制备方法，其特征在于，球磨机的转速为30～3000rpm。
9.根据权利要求1所述的BiOF材料的制备方法，其特征在于，所述的球磨机选自市场上的各种机型；所述的磨球为玛瑙球、刚玉球、氧化锆球、瓷球、不锈钢球中的一种或两种以上。
10.权利要求1至9任一项所述的制备方法得到的BiOF材料在超级电容器、碱性二次电池、锂离子电池、光催化剂、珠光颜料或医药领域中的应用。
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