CN106674073B - 多孔二烷基二硫代氨基甲酸铋可见光催化剂的制备方法 - Google Patents
多孔二烷基二硫代氨基甲酸铋可见光催化剂的制备方法 Download PDFInfo
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- CN106674073B CN106674073B CN201611141039.0A CN201611141039A CN106674073B CN 106674073 B CN106674073 B CN 106674073B CN 201611141039 A CN201611141039 A CN 201611141039A CN 106674073 B CN106674073 B CN 106674073B
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- bismuth
- porous
- dibutyldithiocarbamate
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- WVBGHELXKIMZDI-UHFFFAOYSA-K bis(dibutylcarbamothioylsulfanyl)bismuthanyl n,n-dibutylcarbamodithioate Chemical compound [Bi+3].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC WVBGHELXKIMZDI-UHFFFAOYSA-K 0.000 title claims abstract description 20
- 239000003054 catalyst Substances 0.000 title claims abstract description 12
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 46
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 150000001621 bismuth Chemical class 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 30
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012990 dithiocarbamate Substances 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 238000011160 research Methods 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000009837 dry grinding Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 23
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 20
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 19
- -1 polyethylene Polymers 0.000 claims description 17
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 16
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 14
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 8
- 239000012046 mixed solvent Substances 0.000 claims description 8
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 claims description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 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 5
- 239000005639 Lauric acid Substances 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 4
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical group Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
- 229920000428 triblock copolymer Polymers 0.000 claims description 4
- KKMOSYLWYLMHAL-UHFFFAOYSA-N 2-bromo-6-nitroaniline Chemical compound NC1=C(Br)C=CC=C1[N+]([O-])=O KKMOSYLWYLMHAL-UHFFFAOYSA-N 0.000 claims description 3
- HWSISDHAHRVNMT-UHFFFAOYSA-N Bismuth subnitrate Chemical compound O[NH+]([O-])O[Bi](O[N+]([O-])=O)O[N+]([O-])=O HWSISDHAHRVNMT-UHFFFAOYSA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 229960001482 bismuth subnitrate Drugs 0.000 claims description 3
- ZREIPSZUJIFJNP-UHFFFAOYSA-K bismuth subsalicylate Chemical compound C1=CC=C2O[Bi](O)OC(=O)C2=C1 ZREIPSZUJIFJNP-UHFFFAOYSA-K 0.000 claims description 3
- 229960000782 bismuth subsalicylate Drugs 0.000 claims description 3
- TXKAQZRUJUNDHI-UHFFFAOYSA-K bismuth tribromide Chemical compound Br[Bi](Br)Br TXKAQZRUJUNDHI-UHFFFAOYSA-K 0.000 claims description 3
- CEJZHMCGESPUGN-UHFFFAOYSA-N bismuth;oxalic acid Chemical compound [Bi].OC(=O)C(O)=O CEJZHMCGESPUGN-UHFFFAOYSA-N 0.000 claims description 3
- 229920001400 block copolymer Polymers 0.000 claims description 3
- 238000003682 fluorination reaction Methods 0.000 claims description 3
- 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 claims description 3
- KOECRLKKXSXCPB-UHFFFAOYSA-K triiodobismuthane Chemical compound I[Bi](I)I KOECRLKKXSXCPB-UHFFFAOYSA-K 0.000 claims description 3
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-O diethylammonium Chemical compound CC[NH2+]CC HPNMFZURTQLUMO-UHFFFAOYSA-O 0.000 claims description 2
- 150000002019 disulfides Chemical class 0.000 claims description 2
- 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 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- YOWAEZWWQFSEJD-UHFFFAOYSA-N quinoxalin-2-amine Chemical compound C1=CC=CC2=NC(N)=CN=C21 YOWAEZWWQFSEJD-UHFFFAOYSA-N 0.000 claims 1
- 239000012266 salt solution Substances 0.000 abstract description 20
- 239000000243 solution Substances 0.000 abstract description 20
- 229910000474 mercury oxide Inorganic materials 0.000 abstract description 14
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 abstract description 14
- 239000002904 solvent Substances 0.000 abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 239000012071 phase Substances 0.000 abstract description 8
- 238000000354 decomposition reaction Methods 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 238000000975 co-precipitation Methods 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000356 contaminant Substances 0.000 abstract description 4
- 238000004500 asepsis Methods 0.000 abstract description 3
- 238000003746 solid phase reaction Methods 0.000 abstract description 3
- SZRLKIKBPASKQH-UHFFFAOYSA-M dibutyldithiocarbamate Chemical compound CCCCN(C([S-])=S)CCCC SZRLKIKBPASKQH-UHFFFAOYSA-M 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 description 33
- 239000002245 particle Substances 0.000 description 13
- 229910001451 bismuth ion Inorganic materials 0.000 description 12
- 230000003301 hydrolyzing effect Effects 0.000 description 9
- 239000013078 crystal Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- IWUXOURWOCRGST-UHFFFAOYSA-N C(N)(S)=S.[Bi] Chemical compound C(N)(S)=S.[Bi] IWUXOURWOCRGST-UHFFFAOYSA-N 0.000 description 6
- GUUVPOWQJOLRAS-UHFFFAOYSA-N Diphenyl disulfide Chemical compound C=1C=CC=CC=1SSC1=CC=CC=C1 GUUVPOWQJOLRAS-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- WWGXHTXOZKVJDN-UHFFFAOYSA-M sodium;n,n-diethylcarbamodithioate;trihydrate Chemical compound O.O.O.[Na+].CCN(CC)C([S-])=S WWGXHTXOZKVJDN-UHFFFAOYSA-M 0.000 description 5
- 239000004094 surface-active agent Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000008139 complexing agent Substances 0.000 description 4
- WKLWZEWIYUTZNJ-UHFFFAOYSA-K diacetyloxybismuthanyl acetate Chemical class [Bi+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WKLWZEWIYUTZNJ-UHFFFAOYSA-K 0.000 description 4
- 229940116901 diethyldithiocarbamate Drugs 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 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 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 229950004394 ditiocarb Drugs 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000003235 pyrrolidines Chemical class 0.000 description 3
- WZRRRFSJFQTGGB-UHFFFAOYSA-N 1,3,5-triazinane-2,4,6-trithione Chemical compound S=C1NC(=S)NC(=S)N1 WZRRRFSJFQTGGB-UHFFFAOYSA-N 0.000 description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical group [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- VSWDORGPIHIGNW-UHFFFAOYSA-N Pyrrolidine dithiocarbamic acid Chemical compound SC(=S)N1CCCC1 VSWDORGPIHIGNW-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004847 absorption spectroscopy Methods 0.000 description 2
- YNNGZCVDIREDDK-UHFFFAOYSA-N aminocarbamodithioic acid Chemical compound NNC(S)=S YNNGZCVDIREDDK-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- AYSTWLLPTAGSJQ-UHFFFAOYSA-N bismuth;formic acid Chemical compound [Bi].OC=O AYSTWLLPTAGSJQ-UHFFFAOYSA-N 0.000 description 2
- SFOQXWSZZPWNCL-UHFFFAOYSA-K bismuth;phosphate Chemical compound [Bi+3].[O-]P([O-])([O-])=O SFOQXWSZZPWNCL-UHFFFAOYSA-K 0.000 description 2
- CXZIVLHEAFSOQK-UHFFFAOYSA-K bismuth;tricarbamodithioate Chemical compound [Bi+3].NC([S-])=S.NC([S-])=S.NC([S-])=S CXZIVLHEAFSOQK-UHFFFAOYSA-K 0.000 description 2
- HIZCIEIDIFGZSS-UHFFFAOYSA-N carbonotrithioic acid Chemical compound SC(S)=S HIZCIEIDIFGZSS-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- YKVABMCSVUSETE-UHFFFAOYSA-N dibenzylcarbamodithioic acid;sodium Chemical compound [Na].C=1C=CC=CC=1CN(C(=S)S)CC1=CC=CC=C1 YKVABMCSVUSETE-UHFFFAOYSA-N 0.000 description 2
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- UQJQVUOTMVCFHX-UHFFFAOYSA-L nabam Chemical compound [Na+].[Na+].[S-]C(=S)NCCNC([S-])=S UQJQVUOTMVCFHX-UHFFFAOYSA-L 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- GSFSVEDCYBDIGW-UHFFFAOYSA-N 2-(1,3-benzothiazol-2-yl)-6-chlorophenol Chemical compound OC1=C(Cl)C=CC=C1C1=NC2=CC=CC=C2S1 GSFSVEDCYBDIGW-UHFFFAOYSA-N 0.000 description 1
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 description 1
- BCFGABRSRXBITB-UHFFFAOYSA-N 4-carbamothioylsulfanylbutyl carbamodithioate Chemical compound NC(=S)SCCCCSC(N)=S BCFGABRSRXBITB-UHFFFAOYSA-N 0.000 description 1
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 1
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- JOSRLCGKZSOTRF-UHFFFAOYSA-K C(=O)N.C(C)(=O)[O-].[Bi+3].C(C)(=O)[O-].C(C)(=O)[O-] Chemical compound C(=O)N.C(C)(=O)[O-].[Bi+3].C(C)(=O)[O-].C(C)(=O)[O-] JOSRLCGKZSOTRF-UHFFFAOYSA-K 0.000 description 1
- OUUTUVQWDPRVOO-UHFFFAOYSA-M C(=O)N.C(C)N(C([S-])=S)CC.[Na+] Chemical compound C(=O)N.C(C)N(C([S-])=S)CC.[Na+] OUUTUVQWDPRVOO-UHFFFAOYSA-M 0.000 description 1
- HHPACOCNTVXYRY-UHFFFAOYSA-N CN(C([O-])=S)C.C(C)[NH2+]CC Chemical compound CN(C([O-])=S)C.C(C)[NH2+]CC HHPACOCNTVXYRY-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004280 Sodium formate Substances 0.000 description 1
- VJMAITQRABEEKP-UHFFFAOYSA-N [6-(phenylmethoxymethyl)-1,4-dioxan-2-yl]methyl acetate Chemical compound O1C(COC(=O)C)COCC1COCC1=CC=CC=C1 VJMAITQRABEEKP-UHFFFAOYSA-N 0.000 description 1
- MEFQFHUBDHENRF-UHFFFAOYSA-N [Bi].C(CCC)N(C(S)=S)CCCC Chemical compound [Bi].C(CCC)N(C(S)=S)CCCC MEFQFHUBDHENRF-UHFFFAOYSA-N 0.000 description 1
- AHGZDXRDCNHGJE-UHFFFAOYSA-N [Bi].C(CCC)NC(=S)S Chemical compound [Bi].C(CCC)NC(=S)S AHGZDXRDCNHGJE-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- HRHBQGBPZWNGHV-UHFFFAOYSA-N azane;bromomethane Chemical compound N.BrC HRHBQGBPZWNGHV-UHFFFAOYSA-N 0.000 description 1
- ZXVOCOLRQJZVBW-UHFFFAOYSA-N azane;ethanol Chemical compound N.CCO ZXVOCOLRQJZVBW-UHFFFAOYSA-N 0.000 description 1
- PTYONPWKVPLXDZ-UHFFFAOYSA-N azanium;carbamothioate Chemical compound [NH4+].NC([O-])=S PTYONPWKVPLXDZ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- SKTYDTKJPZZALZ-UHFFFAOYSA-N bismuth;carbamic acid Chemical compound [Bi].NC(O)=O SKTYDTKJPZZALZ-UHFFFAOYSA-N 0.000 description 1
- LNRIVDIAMXQVIZ-UHFFFAOYSA-N bismuth;ethanol Chemical compound [Bi].CCO LNRIVDIAMXQVIZ-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- PCERBVBQNKZCFS-UHFFFAOYSA-N dibenzylcarbamodithioic acid Chemical class C=1C=CC=CC=1CN(C(=S)S)CC1=CC=CC=C1 PCERBVBQNKZCFS-UHFFFAOYSA-N 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical class CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- MJXOOPBZYCWYIF-UHFFFAOYSA-N dimethylcarbamodithioic acid;sodium Chemical compound [Na].CN(C)C(S)=S MJXOOPBZYCWYIF-UHFFFAOYSA-N 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
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Abstract
一种多孔二烷基二硫代氨基甲酸铋可见光催化剂的制备方法,将铋盐和二烷基二硫代氨基甲酸盐分别溶于溶剂中,将二烷基二硫代氨基甲酸盐溶液逐滴加入到铋盐溶液中,产生黄色沉淀;或直接将铋盐和二烷基二硫代氨基甲酸盐粉末混合,干磨或加入助研剂研磨,得到黄色粉末;过滤、洗涤、干燥,得到多孔二烷基二硫代氨基甲酸铋;本发明通过可溶性铋盐和二烷基二硫代氨基甲酸盐的化学共沉淀反应或低温固相反应,得到尺寸均匀、比表面积大的二烷基二硫代氨基甲酸铋;本发明制备的二烷基二硫代氨基甲酸铋为单斜相结构,结晶度高,相态纯净,形貌和尺寸均一,分散性好,无毒环保,在空气水和绝大多数溶剂中稳定,耐酸碱,具有优异的光催化污染物降解和水分解制氢活性。
Description
技术领域
本发明属于材料化学和光催化技术领域,具体涉及一种多孔二烷基二硫代氨基甲酸铋可见光催化剂的制备方法。
背景技术
由于铋的特殊性质,且无毒、廉价,铋基无机半导体光催化材料,如Bi2O3、BiOCl、BiOBr、BiOI、Bi2O2CO3、Bi2S3、BiPO4、BiVO4、Bi2WO6、Bi2MoO6、Bi2Sn2O7等,具有优异的可见光催化活性,受到广泛的关注。近年来,一些有机铋配合物,成本低廉、合成简便、安全环保、便于大规模合成,并且同样具有优异的光催化活性,成为非常有潜力进入实际光催化污染物降解和水分解制氢制氧、抗菌等应用领域的材料,前景非常广阔,是21世纪重要新材料。
二烷基二硫代氨基甲酸盐(铜试剂)等具有硫配位功能的化合物,作为最为广泛应用的螯合剂之一,成本低廉、安全环保,是水体重金属移除应用领域中极为重要的材料。
二烷基二硫代氨基甲酸铋成本低廉、合成简便、安全环保、便于大规模合成,一般通过简单的化学共沉淀法合成。1976年,Allan H.White等报道了二乙基二硫代氨基甲酸铋的晶体结构。随后其他二硫代氨基甲酸铋的晶体结构相继被报道,并作为单源前驱体应用于单分散Bi2S3纳米结构的合成。2007年,Edward R.T.Tiekink等报道了一系列二烷基二硫代氨基甲酸铋的晶体结构,并研究了晶体中Bi和S原子的相互作用,更加深刻地揭示了二烷基二硫代氨基甲酸铋晶体结构的形成。一直以来,对二烷基二硫代氨基甲酸铋的研究较少,主要集中在单晶的培养与结构的测定,但其形貌调控、纳米化合成、光学特性和相关应用并没有得到相应的研究。由于二烷基二硫代氨基甲酸铋的合成反应速率快,因此很难通过简单的液相共沉淀反应控制其形貌,合成颗粒尺寸均一、分散性好的纳米尺寸功能材料,并且对于铋基配合物在介观尺度下的物理和化学性质的研究更是困难。
发明内容
本发明的目的是提供一种具有单斜相结构,结晶度高,相态纯净,形貌和尺寸均一,比表面积大,分散性好,无毒环保,在空气水和绝大多数溶剂中稳定,耐酸碱,适合大规模廉价合成,具有优异的光催化污染物降解和水分解制氢活性的多孔二烷基二硫代氨基甲酸铋可见光催化剂的制备方法。
为达到上述目的,本发明采用的技术方案是:
1)按物质的量比为1:(3-6)取铋盐和二烷基二硫代氨基甲酸盐分别溶于溶剂中得到铋盐溶液和二烷基二硫代氨基甲酸盐溶液,调节铋盐溶液的pH值小于2或加入络合剂防止铋离子水解,在0-90℃将二烷基二硫代氨基甲酸盐溶液逐滴加入到铋盐溶液中,产生黄色沉淀;
或按物质的量比为1:(3-6)直接将铋盐和二烷基二硫代氨基甲酸盐粉末混合,干磨或加入助研剂研磨,得到黄色粉末;
2)过滤、洗涤、干燥,得到多孔二烷基二硫代氨基甲酸铋。
所述铋盐为可溶性的氯化铋、溴化铋、碘化铋、氟化铋、硝酸铋、次硝酸铋、磷酸铋、乙酸铋、柠檬酸铋、柠檬酸铋铵、新十二酸铋、二乙酸三苯铋或次水杨酸铋。
所述二烷基二硫代氨基甲酸盐为可溶性二硫代氨基甲酸盐、二甲基二硫代氨基甲酸盐、二乙基二硫代氨基甲酸盐、二丁基二硫代氨基甲酸盐、二苄基二硫代氨基甲酸盐、吡咯烷二硫代氨基甲酸盐、三聚硫氰酸盐、三硫代碳酸盐或对苯二硫代甲酸盐。
所述二烷基二硫代氨基甲酸盐为可溶性二烷基二硫代氨基甲酸钠、二烷基二硫代氨基甲酸铵或二烷基二硫代氨基甲酸二乙铵。
所述溶剂为水、甲醇、乙醇、异丙醇、正丁醇、乙二醇、一缩二乙二醇、丙三醇、聚乙二醇、丙酮、甲酰胺、N,N-二甲基甲酰胺、二甲基亚砜或水与醇的混合溶剂。
所述水与醇的混合溶剂中水与醇的物质的量比为1:(0.1-10)。
所述溶剂还包括溶剂与表面活性剂的混合溶剂,其中溶剂与表面活性剂的物质的量比为1:(0.1-1),所述的表面活性剂为十六烷基三甲基溴化铵、聚乙烯吡咯烷酮、六亚甲基四胺、柠檬酸三钠、聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物或聚氧乙烯聚氧丙烯醚嵌段共聚物。
所述助研剂为水、甲醇、乙醇、异丙醇、正丁醇、乙二醇、一缩二乙二醇、丙三醇、聚乙二醇、丙酮、甲酰胺、N,N-二甲基甲酰胺、二甲基亚砜、水与醇的混合溶剂、乙醚、油胺、油酸、乙腈、三氯甲烷、环己烷、聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物或聚氧乙烯聚氧丙烯醚嵌段共聚物。
所述的水与醇的混合溶剂中水与醇的物质的量比为1:(0.1-10)。
所述的络合剂为乙二胺四乙酸二钠,其与铋离子的物质的量比为(1-5):1。
与现有技术相比,本发明具有的有益效果:
1、本发明通过可溶性铋盐和二烷基二硫代氨基甲酸盐的简单的化学共沉淀反应或低温固相反应,得到形貌和尺寸均一,比表面积大的多孔二烷基二硫代氨基甲酸铋颗粒。此外,本发明制得的二烷基二硫代氨基甲酸铋具有结晶度高、相态纯净、分散性好、无毒环保、在空气水和绝大多数溶剂中稳定、耐酸碱的特点。本发明克服了传统有机铋配合物的合成产物无形貌的缺点。
2、本发明采用的前驱体在常温常压下进行反应,无需复杂设备、操作简便、成本低廉、节能环保、适合大规模工业量产。克服了传统有机铋配合物合成过程需要高温、长时间水热的缺点。本发明还可以通过简单的替换反应前驱体,直接拓展到其他金属二烷基二硫代氨基甲酸盐功能纳米结构的制备。
3、本发明制得的二烷基二硫代氨基甲酸铋表面干净,无需任何表面修饰和改性,在水中分散性良好,具有可见光吸收性能,在可见光照射下具有优异的光催化污染物降解和水分解制氢活性。
附图说明
图1为实施例1制得的多孔二乙基二硫代氨基甲酸铋颗粒的X射线衍射图谱。
图2为实施例1制得的2μm的多孔二乙基二硫代氨基甲酸铋颗粒的扫描电镜照片。
图3为实施例2制得的20μm的多孔二乙基二硫代氨基甲酸铋颗粒的扫描电镜照片。
图4为实施例4制得的二乙基二硫代氨基甲酸铋纳米片的透射电镜照片。
图5为实施例1制得的多孔二乙基二硫代氨基甲酸铋颗粒的紫外-可见光吸收光谱图。
图6为实施例1制得的多孔二乙基二硫代氨基甲酸铋可见光催化剂在大于400nm可见光照射下降解罗丹明B的紫外-可见光吸收光谱图。
图7为实施例1制得的多孔二乙基二硫代氨基甲酸铋可见光催化剂在大于400nm可见光照射下分解水制氢的产量图。
具体实施方式
本发明根据反应前驱物在不同溶剂中的共沉淀行为和对晶体的成核和生长过程的控制,以二乙基二硫代氨基甲酸盐为例实施例1-7,得到多孔二乙基二硫代氨基甲酸铋。
多孔二乙基二硫代氨基甲酸铋的制备方法为:将铋盐和二乙基二硫代氨基甲酸盐分别溶于溶剂中,调节pH值或加入络合剂防止铋离子水解,在0-90℃下将二乙基二硫代氨基甲酸盐溶液逐滴加入到铋盐溶液中,产生黄色沉淀;或直接将铋盐和二乙基二硫代氨基甲酸盐粉末混合,干磨或加入助研剂研磨,得到黄色粉末。过滤、洗涤、干燥,得到多孔二乙基二硫代氨基甲酸铋;其中,铋盐和二乙基二硫代氨基甲酸盐的物质的量比为1:(3-6);液相合成过程中使用盐酸调节pH小于2或乙二胺四乙酸二钠(与铋离子的物质的量比为(1-5):1为络合剂防止铋离子水解。各实施例的光催化测试方法为:采用300W氙灯(PLS-SXE300UV,北京泊菲莱科技有限公司)结合400nm截止滤光片作为可见光源,光源距离反应体系20cm,不断搅拌测试体系。罗丹明B降解测试中,50mg样品超声分散于100mL罗丹明B水溶液(5mg/L)中,在黑暗中吸附2小时,待达到吸附-脱附平衡后开始光照,间隔一定时间取样,离心分离粉末样品,测试上清液的吸光度,采用比尔-朗伯定律计算降解率;光解水制氢在泊菲莱光解水测试系统中进行,100mg样品超声分散于100mL含20%的甲醇水溶液中,间隔一定时间采集生成气体进行分析,并计算氢气产量。
下面通过具体实施例进行详细说明。
实施例1:
多孔二乙基二硫代氨基甲酸铋的制备方法为:在室温下,将1mmol乙酸铋和3mmol二乙基二硫代氨基甲酸钠三水合物分别溶于20mL乙二胺四乙酸二钠水溶液(0.15mol/L)和纯水中,将二乙基二硫代氨基甲酸钠水溶液逐滴加入乙酸铋水溶液中,逐渐产生黄色沉淀,滴加结束后,过滤,加入40mL水,过滤、洗涤和干燥,得到尺寸大小为2μm的黄色粉末,即为多孔二乙基二硫代氨基甲酸铋颗粒。
对制备的多孔二乙基二硫代氨基甲酸铋颗粒经粉末X射线衍射鉴定为单斜相,具有高的结晶度(见图1);用扫描电镜观察到该产品为表面具有纳米多孔结构的方块,尺寸大小为2μm(见图2);用紫外-可见光分光光度计检测,该产品具有可见光吸收性能,吸收波长到500nm(见图5);该产品具有优异的可见光催化罗丹明B降解和水分解制氢活性(见图6和7)。
实施例2:
多孔二乙基二硫代氨基甲酸铋的制备方法为:在60℃下,将1mmol新十二酸铋和3mmol二乙基二硫代氨基甲酸铵分别溶于20mL乙醇(用盐酸调节pH小于2)和纯乙醇中,将二乙基二硫代氨基甲酸铵乙醇溶液逐滴加入新十二酸铋乙醇溶液中,逐渐产生黄色沉淀,滴加结束后,过滤,加入40mL水,过滤、洗涤和干燥,得到尺寸大小为20μm的黄色粉末(见图3),即为多孔二乙基二硫代氨基甲酸铋颗粒。
实施例3:
多孔二乙基二硫代氨基甲酸铋的制备方法为:在0℃冰浴下,将1mmol乙酸铋和3mmol二乙基二硫代氨基甲酸钠三水合物分别溶于20mL甲酰胺(用盐酸调节pH小于2)和纯甲酰胺中,将二乙基二硫代氨基甲酸钠甲酰胺溶液逐滴加入乙酸铋甲酰胺溶液中,逐渐产生黄色沉淀,滴加结束后,过滤,加入40mL水,过滤、洗涤和干燥,得到尺寸大小为100μm的黄色粉末,即为多孔二乙基二硫代氨基甲酸铋颗粒。
实施例4:
多孔二乙基二硫代氨基甲酸铋的制备方法为:在室温下,将1mmol乙酸铋和3mmol二乙基二硫代氨基甲酸钠三水合物分别溶于20mL N,N-二甲基甲酰胺(用盐酸调节pH小于2)和纯N,N-二甲基甲酰胺中,将二乙基二硫代氨基甲酸钠N,N-二甲基甲酰胺溶液逐滴加入乙酸铋N,N-二甲基甲酰胺溶液中,逐渐产生黄色沉淀,滴加结束后,过滤,加入40mL水,过滤、洗涤和干燥,得到纳米片状结构(见图4)的黄色粉末,即为二乙基二硫代氨基甲酸铋纳米片。
实施例5:
多孔二乙基二硫代氨基甲酸铋的制备方法为:在室温下,将1mmol乙酸铋和3mmol二乙基二硫代氨基甲酸钠三水合物分别溶于20mL乙醇/丙三醇(体积比为1:1,用盐酸调节pH小于2)和乙醇/丙三醇中,将二乙基二硫代氨基甲酸钠乙醇/丙三醇溶液逐滴加入乙酸铋乙醇/丙三醇溶液中,逐渐产生黄色沉淀,滴加结束后,过滤,加入40mL水,过滤、洗涤和干燥,得到纳米花状结构的黄色粉末,即为二乙基二硫代氨基甲酸铋纳米花。
实施例6:
多孔二乙基二硫代氨基甲酸铋的制备方法为:在室温下,将1mmol氯化铋和3mmol二乙基二硫代氨基甲酸钠三水合物混合于研钵中,加入1mL聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物作为助研剂,研磨30分钟,产生黄色粉末,研磨结束后,加入40mL水,过滤、洗涤和干燥,得到纳米线结构的黄色粉末,即为二乙基二硫代氨基甲酸铋纳米线。
实施例7:
多孔二乙基二硫代氨基甲酸铋的制备方法为:在室温下,将1mmol柠檬酸铋铵和3mmol二乙基二硫代氨基甲酸钠三水合物混合于研钵中,研磨10分钟,产生黄色粉末,研磨结束后,加入40mL水,过滤、洗涤和干燥,得到黄色粉末,即为多孔二乙基二硫代氨基甲酸铋颗粒。
实施例8:
将1mmol的氯化铋和4mmol的二硫代氨基甲酸钠分别溶于20ml甲醇和乙醇中,调节铋盐溶液的pH值小于2防止铋离子水解,60℃将二硫代氨基甲酸钠溶液逐滴加入到铋盐溶液中,产生黄色沉淀;过滤、洗涤、干燥,得到多孔二硫代氨基甲酸铋。
实施例9:
取1mmol的乙酸铋和3mmol的吡咯烷二硫代氨基甲酸铵粉末混合,干磨研磨,得到黄色粉末;过滤、洗涤、干燥,得到多孔吡咯烷二硫代氨基甲酸铋。
实施例10:
将1mmol的溴化铋和5mmol的二甲基二硫代氨基甲酸二乙铵分别溶于20ml的异丙醇和正丁醇中,调节铋盐溶液的pH值小于2防止铋离子水解,在30℃将二甲基二硫代氨基甲酸二乙铵溶液逐滴加入到铋盐溶液中,产生黄色沉淀;过滤、洗涤、干燥,得到多孔二甲基二硫代氨基甲酸铋。
实施例11:
将1mmol的碘化铋和6mmol的二丁基二硫代氨基甲酸铵分别溶于20ml乙二醇和一缩二乙二醇中,调节铋盐溶液的pH值小于2防止铋离子水解,在50℃将二丁基二硫代氨基甲酸铵溶液逐滴加入到铋盐溶液中,产生黄色沉淀;过滤、洗涤、干燥,得到多孔二丁基二硫代氨基甲酸铋。
实施例12:
将1mmol的氟化铋和5mmol的二苄基二硫代氨基甲酸钠分别溶于20ml丙三醇和聚乙二醇中,调节铋盐溶液的pH值小于2防止铋离子水解,在10℃将二苄基二硫代氨基甲酸钠溶液逐滴加入到铋盐溶液中,产生黄色沉淀;过滤、洗涤、干燥,得到多孔二苄基二硫代氨基甲酸铋。
实施例13:
将1mmol的硝酸铋和4.5mmol的二硫代氨基甲酸铵分别溶于20ml丙酮和甲酰胺中,调节铋盐溶液的pH值小于2防止铋离子水解,在50℃将二硫代氨基甲酸铵溶液逐滴加入到铋盐溶液中,产生黄色沉淀;过滤、洗涤、干燥,得到多孔二硫代氨基甲酸铋。
实施例14:
将1mmol的次硝酸铋和3.5mmol的二甲基二硫代氨基甲酸钠分别溶于20ml水与表面活性剂的混合溶剂,其中水与表面活性剂的物质的量比为1:1,表面活性剂为十六烷基三甲基溴化铵,调节铋盐溶液的pH值小于2防止铋离子水解,在70℃将二甲基二硫代氨基甲酸钠溶液逐滴加入到铋盐溶液中,产生黄色沉淀;过滤、洗涤、干燥,得到多孔二甲基二硫代氨基甲酸铋。
实施例15:
将1mmol的磷酸铋和5.5mmol的二丁基二硫代氨基甲酸铵分别溶于20ml N,N-二甲基甲酰胺和二甲基亚砜中,调节铋盐溶液的pH值小于2防止铋离子水解,在0℃将二丁基二硫代氨基甲酸铵溶液逐滴加入到铋盐溶液中,产生黄色沉淀;过滤、洗涤、干燥,得到多孔二丁基二硫代氨基甲酸铋。
实施例16:
取1mmol的柠檬酸铋和3mmol的吡咯烷二硫代氨基甲酸钠粉末混合研磨,得到黄色粉末;过滤、洗涤、干燥,得到多孔吡咯烷二硫代氨基甲酸铋。
实施例17:
取1mmol的柠檬酸铋铵和4mmol的吡咯烷二硫代氨基甲酸铵粉末混合研磨,得到黄色粉末;过滤、洗涤、干燥,得到多孔吡咯烷二硫代氨基甲酸铋。
实施例18:
取1mmol的新十二酸铋和5mmol的三聚硫氰酸钠粉末混合,加入助研剂水研磨,得到黄色粉末;过滤、洗涤、干燥,得到多孔三聚硫氰酸铋。
实施例19:
取1mmol的二乙酸三苯铋和6mmol的对苯二硫代甲酸钠粉末混合研磨,得到黄色粉末;过滤、洗涤、干燥,得到多孔对苯二硫代甲酸铋。
实施例20:
取1mmol的次水杨酸铋和5.5mmol的三硫代碳酸钠粉末混合,研磨,得到黄色粉末;过滤、洗涤、干燥,得到多孔三硫代碳酸铋。
本发明利用简单的化学共沉淀或低温固相反应,通过调节反应前驱体、溶剂或助研剂、温度等参数,实现晶体成核和生长过程的控制,一步可以获得相态纯净、高度晶化、尺寸均匀可调、形貌可控、比表面积大、分散性好、无毒环保、在空气水和绝大多数溶剂中稳定、耐酸碱、具有单斜相结构的多孔二烷基二硫代氨基甲酸铋颗粒。本发明合成的二烷基二硫代氨基甲酸铋颗粒表面干净,无需任何表面修饰和改性,即可在水中良好分散,具有可见光吸收性能,实现了可见光照射下的优异的光催化污染物降解和水分解制氢活性,并且为其在固体磷光、抗菌等方面提供了潜在的应用价值。这种制备二烷基二硫代氨基甲酸铋颗粒的方法可以直接放大反应,适合大规模廉价工业化生产,而且很容易通过简单的替换反应前驱体,直接拓展到其他金属二烷基二硫代氨基甲酸盐功能纳米结构的制备。
Claims (5)
1.一种多孔二烷基二硫代氨基甲酸铋可见光催化剂的制备方法,其特征在于:
1)按物质的量比为1∶(3-6)直接将铋盐和二烷基二硫代氨基甲酸盐粉末混合,干磨或加入助研剂研磨,得到黄色粉末;
2)过滤、洗涤、干燥,得到多孔二烷基二硫代氨基甲酸铋。
2.根据权利要求1所述的多孔二烷基二硫代氨基甲酸铋可见光催化剂的制备方法,其特征在于:所述铋盐为可溶性的氯化铋、溴化铋、碘化铋、氟化铋、硝酸铋、次硝酸铋、磷酸铋、乙酸铋、柠檬酸铋、柠檬酸铋铵、新十二酸铋、二乙酸三苯铋或次水杨酸铋。
3.根据权利要求1所述的多孔二烷基二硫代氨基甲酸铋可见光催化剂的制备方法,其特征在于:所述二烷基二硫代氨基甲酸盐为可溶性二烷基二硫代氨基甲酸钠、二烷基二硫代氨基甲酸铵或二烷基二硫代氨基甲酸二乙铵。
4.根据权利要求1所述的多孔二烷基二硫代氨基甲酸铋可见光催化剂的制备方法,其特征在于:所述助研剂为水、甲醇、乙醇、异丙醇、正丁醇、乙二醇、一缩二乙二醇、丙三醇、聚乙二醇、丙酮、甲酰胺、N,N-二甲基甲酰胺、二甲基亚砜、水与醇的混合溶剂、乙醚、油胺、油酸、乙腈、三氯甲烷、环己烷、聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物或聚氧乙烯聚氧丙烯醚嵌段共聚物。
5.根据权利要求4所述的多孔二烷基二硫代氨基甲酸铋可见光催化剂的制备方法,其特征在于:所述的水与醇的混合溶剂中水与醇的物质的量比为1∶(0.1-10)。
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