CN110237811A - A kind of Nanoscale Iron molybdenum-graphene composite material and its preparation method and application - Google Patents
A kind of Nanoscale Iron molybdenum-graphene composite material and its preparation method and application Download PDFInfo
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- CN110237811A CN110237811A CN201910453657.6A CN201910453657A CN110237811A CN 110237811 A CN110237811 A CN 110237811A CN 201910453657 A CN201910453657 A CN 201910453657A CN 110237811 A CN110237811 A CN 110237811A
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- molybdenum
- graphene
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- ion
- composite material
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 87
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000001179 sorption measurement Methods 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 21
- 239000011733 molybdenum Substances 0.000 claims abstract description 21
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 15
- 239000003463 adsorbent Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 11
- 150000002751 molybdenum Chemical class 0.000 claims abstract description 11
- 239000005416 organic matter Substances 0.000 claims abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 24
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 13
- 150000002500 ions Chemical class 0.000 claims description 13
- 229910052700 potassium Inorganic materials 0.000 claims description 13
- 239000011591 potassium Substances 0.000 claims description 13
- -1 Na2Fe04 Chemical compound 0.000 claims description 12
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 claims description 11
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 11
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 10
- 239000011684 sodium molybdate Substances 0.000 claims description 7
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical group [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 7
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 6
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 6
- 229940043237 diethanolamine Drugs 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims description 6
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 5
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 claims description 5
- HAYXDMNJJFVXCI-UHFFFAOYSA-N arsenic(5+) Chemical compound [As+5] HAYXDMNJJFVXCI-UHFFFAOYSA-N 0.000 claims description 5
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 claims description 5
- 229910001430 chromium ion Inorganic materials 0.000 claims description 5
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 5
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 5
- 229910001431 copper ion Inorganic materials 0.000 claims description 5
- 229910001437 manganese ion Inorganic materials 0.000 claims description 5
- 229910001453 nickel ion Inorganic materials 0.000 claims description 5
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-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
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 4
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 claims description 4
- BQPIGGFYSBELGY-UHFFFAOYSA-N mercury(2+) Chemical compound [Hg+2] BQPIGGFYSBELGY-UHFFFAOYSA-N 0.000 claims description 4
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 claims description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 claims description 3
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- RZSYLLSAWYUBPE-UHFFFAOYSA-L Fast green FCF Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC(O)=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 RZSYLLSAWYUBPE-UHFFFAOYSA-L 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- 229910021575 Iron(II) bromide Inorganic materials 0.000 claims description 2
- WUGQZFFCHPXWKQ-UHFFFAOYSA-N Propanolamine Chemical compound NCCCO WUGQZFFCHPXWKQ-UHFFFAOYSA-N 0.000 claims description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- YVBOZGOAVJZITM-UHFFFAOYSA-P ammonium phosphomolybdate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])=O.[O-][Mo]([O-])(=O)=O YVBOZGOAVJZITM-UHFFFAOYSA-P 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229940106691 bisphenol a Drugs 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- YQLZOAVZWJBZSY-UHFFFAOYSA-N decane-1,10-diamine Chemical compound NCCCCCCCCCCN YQLZOAVZWJBZSY-UHFFFAOYSA-N 0.000 claims description 2
- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 claims description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 2
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 2
- 229940046149 ferrous bromide Drugs 0.000 claims description 2
- 229940116007 ferrous phosphate Drugs 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- ATEAWHILRRXHPW-UHFFFAOYSA-J iron(2+);phosphonato phosphate Chemical compound [Fe+2].[Fe+2].[O-]P([O-])(=O)OP([O-])([O-])=O ATEAWHILRRXHPW-UHFFFAOYSA-J 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000155 iron(II) phosphate Inorganic materials 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- GYCHYNMREWYSKH-UHFFFAOYSA-L iron(ii) bromide Chemical compound [Fe+2].[Br-].[Br-] GYCHYNMREWYSKH-UHFFFAOYSA-L 0.000 claims description 2
- FZGIHSNZYGFUGM-UHFFFAOYSA-L iron(ii) fluoride Chemical compound [F-].[F-].[Fe+2] FZGIHSNZYGFUGM-UHFFFAOYSA-L 0.000 claims description 2
- SDEKDNPYZOERBP-UHFFFAOYSA-H iron(ii) phosphate Chemical compound [Fe+2].[Fe+2].[Fe+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SDEKDNPYZOERBP-UHFFFAOYSA-H 0.000 claims description 2
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 claims description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 2
- 229960003742 phenol Drugs 0.000 claims description 2
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims description 2
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 claims description 2
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- HFIYIRIMGZMCPC-YOLJWEMLSA-J remazole black-GR Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]S(=O)(=O)C1=CC2=CC(S([O-])(=O)=O)=C(\N=N\C=3C=CC(=CC=3)S(=O)(=O)CCOS([O-])(=O)=O)C(O)=C2C(N)=C1\N=N\C1=CC=C(S(=O)(=O)CCOS([O-])(=O)=O)C=C1 HFIYIRIMGZMCPC-YOLJWEMLSA-J 0.000 claims description 2
- 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 claims description 2
- 229940043267 rhodamine b Drugs 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 229960004889 salicylic acid Drugs 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 2
- FEONEKOZSGPOFN-UHFFFAOYSA-K tribromoiron Chemical compound Br[Fe](Br)Br FEONEKOZSGPOFN-UHFFFAOYSA-K 0.000 claims description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims 2
- 239000005955 Ferric phosphate Substances 0.000 claims 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims 1
- ZGHDMISTQPRNRG-UHFFFAOYSA-N dimolybdenum Chemical compound [Mo]#[Mo] ZGHDMISTQPRNRG-UHFFFAOYSA-N 0.000 claims 1
- 229940032958 ferric phosphate Drugs 0.000 claims 1
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims 1
- 229910052744 lithium Inorganic materials 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000006365 thiocyanation reaction Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 25
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- 229910004619 Na2MoO4 Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 3
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- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 3
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 238000005342 ion exchange Methods 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- RFGNMWINQUUNKG-UHFFFAOYSA-N iron phosphoric acid Chemical compound [Fe].OP(O)(O)=O RFGNMWINQUUNKG-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- NMHMDUCCVHOJQI-UHFFFAOYSA-N lithium molybdate Chemical compound [Li+].[Li+].[O-][Mo]([O-])(=O)=O NMHMDUCCVHOJQI-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0218—Compounds of Cr, Mo, W
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to a kind of Nanoscale Iron molybdenum-graphene composite materials and its preparation method and application.The preparation method includes the following steps: molysite and molybdenum salt will to be added after graphene oxide Yu Shuizhong ultrasonic disperse, then adds reducing agent and react up to the Nanoscale Iron molybdenum-graphene composite material.The present invention selects one kettle way to prepare, molysite, molybdenum salt and graphene oxide are reduced to Nanoscale Iron, nanometer molybdenum and graphene respectively by reducing agent, the load of Nanoscale Iron and nanometer molybdenum on graphene is realized simultaneously, the iron and molybdenum of load can improve the adsorption capacity of graphene with useless Organic substance in water and heavy metal ion chelating, and iron can be improved the duty factor of molybdenum, obtained composite material has the characteristics that adsorption capacity is big, all has preferable suction-operated to heavy metal ion in solution system or organic matter adsorbent.Preparation method raw material of the invention is easy to get, and process is simple, and reaction efficiency is high, and product separating treatment is easy, and use cost is low, is conducive to industrial applications.
Description
Technical field
The invention belongs to adsorbent material technical fields, and in particular to a kind of Nanoscale Iron molybdenum-graphene composite material and its system
Preparation Method and application.
Background technique
Have in the waste water of the industries such as intermetallic composite coating, hard brittle material processing, printing and dyeing, mineral processing, chemical industry containing a large amount of
Organic pollutant and heavy metal ion, common includes methylene blue, methylene orange, ethamine, aniline, monoethyl amine, dimethylamine, two
Ethamine, trimethylamine, a propylamine, di-n-propylamine, isopropylamine, ethylenediamine, monoethanolamine, diethanol amine, triethanolamine easily make water body rich
Nutrient laden, and a large amount of oxygen are consumed in decomposable process, influence the growth of aquatic organism.Heavy metal wastewater thereby and organic wastewater enter ring
It retains, accumulate and migrates behind border or the ecosystem, seriously threaten ecological environment and human health.
Heavy metal wastewater thereby and method for processing organic wastewater include chemical precipitation, UF membrane, ion exchange and absorption, photocatalysis
Degradation, Fenton oxidation method etc. are considered as a kind of cost-effective method in the treatment of waste water.But conventional adsorbent has suction
The disadvantages of attached capacity is low, difficult separation.Carbon nanomaterial adsorbent material has high-specific surface area, easily preparation, physicalchemical structure steady
The features such as determining has become research hotspot in recent years.Graphene is a kind of Novel Carbon Nanomaterials, is widely used in electronics, biology
The fields such as sensor, drug delivery, ambient water quality purification, show huge application potential in ambient water quality field of purification.
108854162 A of CN discloses one kind, and graphene oxide is firmly attached to sponge surface using dopamine,
Then it with hydrazine hydrate reduction at graphene, then is dipped into γ-methacryloxypropyl trimethoxy silane solution and stone is made
Black alkene composite material, adsorption capacity is strong, and oil-water separation is good.108905973 A of CN disclosed a kind of three-dimensional grapheme/
Fe3O4Fe is added by the way that graphene oxide is carried out ultrasonication in magnetic nano adsorption material, the material3+With L-Cys in alkalinity
Under the conditions of one kettle way be co-precipitated to obtain, for adsorbing dyeing waste water.CN109012598A discloses a kind of based on manganese dioxide/oxygen
The Ciprofloxacin absorption purifier of graphite alkene nanocomposite.A kind of L-arginine of CN108816187A disclosure of the invention changes
Property graphene oxide sponge preparation method.CN108620028A disclose it is a kind of by graphene using stearic acid activation, then will
Precipitated calcium carbonate is distributed in amide solution, is blended with activated graphene, obtains the compound grapheme material of calcium carbonate, and have
Good absorption property.
Grapheme material is modified to improve its adsorption effect and become the research hotspot in adsorbent material field, exploitation one
Kind has important research significance and application value for organic matter and the high modified graphene material of heavy metal ion adsorbed capacity.
Summary of the invention
The purpose of the present invention is to overcome the defects in the prior art and insufficient, and it is multiple to provide a kind of Nanoscale Iron molybdenum-graphene
The preparation method of condensation material.The present invention, for carrier loaded Nanoscale Iron and nanometer molybdenum, obtains the compound suction of stable structure with graphene
Enclosure material has the characteristics that adsorption capacity is big, all has absorption to heavy metal ion in solution system or organic matter adsorbent and makees
With especially for organic matters such as methylene blue, methylene orange, monoethanolamine, diethanol amine, triethanolamines in solution system
And the metals such as manganese ion, copper ion, lead ion, zinc ion, chromium ion, cadmium ion, mercury ion, arsenic ion, cobalt ions, nickel ion
Ion has good adsorption effect；Preparation method raw material provided by the invention is easy to get, and preparation process is simple, and reaction efficiency is high,
Product separating treatment is easy, and use cost is low, is conducive to industrial applications.
Another object of the present invention is to provide a kind of Nanoscale Iron molybdenum-graphene composite materials.
Another object of the present invention is to provide above-mentioned Nanoscale Iron molybdenum-graphene composite materials to adsorb as adsorbent material
The application in organic matter or heavy metal ion in water solution system.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of preparation method of Nanoscale Iron molybdenum-graphene composite material, includes the following steps: graphene oxide Yu Shuizhong
Molysite and molybdenum salt are added after ultrasonic disperse, then adds reducing agent and reacts up to the Nanoscale Iron molybdenum-graphene composite material；
The mass ratio of ferro element and graphene oxide is 0.1~5:1 in the molysite；Molybdenum element and graphene oxide in the molybdenum salt
Mass ratio is 0.1~5:1.
The present invention attempts the absorption property that graphene is improved by supported nano-gold category, receives the study found that ought only load
When rice iron, to the absorption property of graphene substantially without promoting effect；And when loading nanometer molybdenum, a nanometer molybdenum can not be implemented separately in discovery
Load.When loading Nanoscale Iron and nanometer molybdenum simultaneously, absorption property has obtained biggish promotion.
Specifically, the present invention selects one kettle way to prepare Nanoscale Iron molybdenum-graphene composite material, by reducing agent by iron
Salt, molybdenum salt and graphene oxide are reduced to Nanoscale Iron, nanometer molybdenum and graphene respectively, while realizing Nanoscale Iron and nanometer molybdenum in stone
Load on black alkene, graphene can be improved with useless Organic substance in water and heavy metal ion chelating by being supported on iron and molybdenum on graphene
Adsorption capacity, and iron can be improved the duty factor of molybdenum, and obtained Nanoscale Iron molybdenum-graphene composite material has adsorption capacity
Big feature all has suction-operated to heavy metal ion in solution system or organic matter adsorbent, especially for solution body
Organic matters and manganese ion, copper ion, the lead such as methylene blue, methylene orange, monoethanolamine, diethanol amine, triethanolamine in system
The metal ions such as ion, zinc ion, chromium ion, cadmium ion, mercury ion, arsenic ion, cobalt ions, nickel ion have good absorption
Effect.
Preparation method raw material provided by the invention is easy to get, and preparation process is simple, and reaction efficiency is high, product separating treatment letter
Just, use cost is low, is conducive to industrial applications.
Graphene oxide in the present invention both can also refer to conventional method preparation in the prior art by being commercially available
It obtains.
The present invention also provides a kind of preparation method of graphene oxide herein.
Preferably, the graphene oxide is prepared via a method which to obtain: graphite powder, sodium nitrate and the concentrated sulfuric acid are mixed
It is stirred under ice bath, potassium permanganate is added, stirring, then temperature rising reflux stirs, and H is added after cooling2O2Reaction is filtered up to described
Graphene oxide.
Preferably, the molysite is ferric sulfate, ferrous sulfate, iron chloride, frerrous chloride, ferrous nitrate, ferric nitrate, phosphoric acid
Iron, ferrous phosphate, ferrous pyrophosphate, Na2Fe04, potassium ferrate, ferric bromide, ferrous bromide, ferric flouride, ferrous fluoride or sulphur
Ferricyanide and its hydrate it is one or more.
Preferably, the molybdenum salt be sodium molybdate, potassium molybdate, ammonium molybdate, lithium molybdate, bismuth molybdate, phosphomolybdic acid, ammonium phosphomolybdate or
Ammonium tetramolybdate and its hydrate it is one or more.
Preferably, the reducing agent is one of potassium borohydride, sodium borohydride, hydrazine hydrate or sodium hypophosphite or a variety of.
Preferably, the temperature of the reaction is 5~40 DEG C, and the time is 0.5~4h.
Preferably, the mass ratio of ferro element and graphene oxide is 1~3:1 in the molysite；Molybdenum element in the molybdenum salt
Mass ratio with graphene oxide is 1~3:1.
A kind of Nanoscale Iron molybdenum-graphene composite material, is prepared by above-mentioned preparation method.
Above-mentioned Nanoscale Iron molybdenum-graphene composite material is as organic matter of the adsorbent material in adsorption aqueous solution system or again
Application in metal ion is also within the scope of the present invention.
Preferably, the organic matter is methylene blue, methylene orange, methyl red, fast green, rhodamine B, ethamine, aniline, one
Methylamine, monoethyl amine, dimethylamine, diethylamine, trimethylamine, triethylamine, a propylamine, di-n-propylamine, tripropyl amine (TPA), isopropylamine, ethylenediamine, 1,
2- propane diamine, butylamine, octylame, 1,4- butanediamine, 1,10- decamethylene diamine, monoethanolamine, diethanol amine, triethanolamine, diphenylamines,
It is one or more of in Propanolamine, reactive black 5, reddish black, phenol, bisphenol-A, salicylic acid or p-methyl benzenesulfonic acid.
Preferably, the heavy metal ion be manganese ion, copper ion, lead ion, zinc ion, chromium ion, cadmium ion, mercury from
It is one or more of in son, arsenic ion, cobalt ions or nickel ion.
Compared with prior art, the invention has the following beneficial effects:
The present invention selects one kettle way to prepare Nanoscale Iron molybdenum-graphene composite material, by reducing agent by molysite, molybdenum salt and
Graphene oxide is reduced to Nanoscale Iron, nanometer molybdenum and graphene respectively, while realizing Nanoscale Iron and nanometer molybdenum on graphene
Load, the adsorption energy of graphene can be improved with useless Organic substance in water and heavy metal ion chelating by being supported on iron and molybdenum on graphene
Power, and iron can be improved the duty factor of molybdenum, the spy that obtained Nanoscale Iron molybdenum-graphene composite material has adsorption capacity big
Point all has suction-operated to heavy metal ion in solution system or organic matter adsorbent, especially in solution system
Organic matters and manganese ion, copper ion, lead ion, the zinc such as methylene blue, methylene orange, monoethanolamine, diethanol amine, triethanolamine
The metal ions such as ion, chromium ion, cadmium ion, mercury ion, arsenic ion, cobalt ions, nickel ion have good adsorption effect.
Preparation method raw material provided by the invention is easy to get, and preparation process is simple, and reaction efficiency is high, product separating treatment letter
Just, use cost is low, is conducive to industrial applications.
Detailed description of the invention
Fig. 1 is Nanoscale Iron molybdenum-graphene composite material infrared spectrogram that embodiment 1 is prepared.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.These embodiments are merely to illustrate the present invention rather than limitation
The scope of the present invention.Test method without specific conditions in lower example embodiment usually according to this field normal condition or is pressed
The condition suggested according to manufacturer；Used raw material, reagent etc., unless otherwise specified, being can be from the business such as conventional market
The raw materials and reagents that approach obtains.The variation for any unsubstantiality that those skilled in the art is done on the basis of the present invention
And replacement belongs to scope of the present invention.
Graphene oxide in each embodiment obtains by the following method: 1.0g graphite powder is weighed in the 60mL concentrated sulfuric acid,
0.75g sodium nitrate is added, is slowly added to 4g potassium permanganate in ice bath, ice bath 1h is placed in room temperature after ice bath and reacts 1h, after
It is slowly added to 100mL water, is warming up to 98 DEG C, flow back 1h, after heating.55 DEG C are cooled to, 6mL H is added dropwise2O2React half an hour
Afterwards then filtering is added hydrochloric acid with distilled water flushing three times and rinses, and is being rinsed with water to filtrate as neutrality, obtained solid is
Graphene oxide.
Embodiment 1
The present embodiment provides a kind of Nanoscale Iron molybdenum-graphene composite material, Fe:Mo:C=3:1:1 (quality in composite material
Than), preparation method is as follows.
Graphene oxide (1g) is put into reaction flask, 200mL water is added, 14gFeSO is added in ultrasonic half an hour4·6H2O and
2.5g Na2MoO4·2H2Continue ultrasonic half an hour after O, Fe:Mo:C=3 be obtained by filtration after the potassium borohydride reaction 1h of 6g is added dropwise:
The composite material of 1:1.
Such as Fig. 1, for Nanoscale Iron molybdenum-graphene composite material infrared spectrogram.From figure it is found that prepared graphite
Alkene, carbonyl are reduced substantially, and there are also certain C-O to exist.
Embodiment 2
The present embodiment provides a kind of Nanoscale Iron molybdenum-graphene composite material, Fe:Mo:C=2:1:1 (quality in composite material
Than), preparation method is as follows.
Graphene oxide (1g) is put into reaction flask, 200mL water is added, 4.65g FeSO is added in ultrasonic half an hour4·
6H2O and 2.5g Na2MoO4·2H2Continue ultrasonic half an hour after O, Fe be obtained by filtration after the potassium borohydride reaction 1h of 6g is added dropwise:
The composite material of Mo:C=2:1:1.
Embodiment 3
The present embodiment provides a kind of Nanoscale Iron molybdenum-graphene composite material, Fe:Mo:C=2:2:1 (quality in composite material
Than), preparation method is as follows.
Obtained solid is put into addition 200mL water in reaction flask, 4.65gFeSO is added in ultrasonic half an hour4·6H2O and 5g
Na2MoO4·2H2Continue ultrasonic half an hour after O, is obtained by filtration Fe:Mo:C=2:2:1's after the potassium borohydride reaction 1h of 6g is added dropwise
Composite material.
Embodiment 4
The present embodiment provides a kind of Nanoscale Iron molybdenum-graphene composite material, Fe:Mo:C=1:3:1 (quality in composite material
Than), preparation method is as follows.
Graphene oxide (1g) is put into reaction flask, 200mL water is added, 2.33gFeSO is added in ultrasonic half an hour4·6H2O
With 7.5g Na2MoO4·2H2Continue ultrasonic half an hour after O, Fe:Mo:C=is obtained by filtration after the potassium borohydride reaction 1h of 6g is added dropwise
The composite material of 1:3:1.
Embodiment 5
The present embodiment provides a kind of Nanoscale Iron molybdenum-graphene composite material, Fe:Mo:C=1:2:1 (quality in composite material
Than), preparation method is as follows.
Graphene oxide (1g) is put into reaction flask, 200mL water is added, 2.33gFeSO is added in ultrasonic half an hour4·6H2O
With 5g Na2MoO4·2H2Continue ultrasonic half an hour after O, Fe:Mo:C=1 be obtained by filtration after the potassium borohydride reaction 1h of 6g is added dropwise:
The composite material of 2:1.
Embodiment 6
The present embodiment provides a kind of Nanoscale Iron molybdenum-graphene composite material, Fe:Mo:C=0.5:5:1 (matter in composite material
Measure ratio), preparation method is as follows.
Graphene oxide (1g) is put into reaction flask, 200mL water is added, 0.90g FeCl is added in ultrasonic half an hour2·
4H2O and 11.88g (NH4)2Mo4O13·2H2Continue ultrasonic half an hour after O, the hydrazine hydrate of 100mL is added dropwise, after 5 DEG C of reaction 4h
The composite material of Fe:Mo:C=0.5:5:1 is obtained by filtration.
Embodiment 7
The present embodiment provides a kind of Nanoscale Iron molybdenum-graphene composite material, Fe:Mo:C=5:0.5:1 (matter in composite material
Measure ratio), preparation method is as follows.
Graphene oxide (1g) is put into reaction flask, 200mL water is added, 36.08g Fe is added in ultrasonic half an hour
(NO3)3·9H2O and 0.79gH3PO4·12MoO3·H2Continue ultrasonic half an hour after O, the potassium borohydride of 8g is added dropwise, at 40 DEG C
The composite material of Fe:Mo:C=5:0.5:1 is obtained by filtration after reaction 0.5h.
Comparative example 1
This comparative example provides a kind of graphene, is prepared via a method which to obtain.
Graphene oxide (1g) is put into reaction flask, 200mL water is added, the potassium borohydride that 6g is added dropwise in ultrasonic half an hour is anti-
Grapheme material is obtained by filtration after answering 1h.
Comparative example 2
This comparative example provides a kind of graphene, is prepared via a method which to obtain.
Graphene oxide (1g) is put into reaction flask, 200mL water is added, 7.5g Na is added in ultrasonic half an hour2MoO4·
2H2Continue ultrasonic half an hour after O, is added dropwise after the potassium borohydride reaction 1h of 6g after filtering and obtains adsorbent material, the absorption after measured
Material is graphene, and above process molybdenum is loaded there is no complete.
Comparative example 3
This comparative example provides a kind of Nano Iron-graphite alkene composite material, Fe:C=1:1 (mass ratio) in composite material,
Preparation method is as follows.
Graphene oxide (1g) is put into reaction flask, 200mL water is added, 2.33gFeSO is added in ultrasonic half an hour4·6H2O
Continue ultrasonic half an hour afterwards, the composite material that Fe:C=1:1 is obtained by filtration after the potassium borohydride reaction 1h of 6g is added dropwise.
Performance test
By taking Nanoscale Iron molybdenum-graphene composite material that embodiment 1 and embodiment 4 provide as an example, what comparative example 1~2 provided
The Nano Iron-graphite alkene composite material that graphene and comparative example 3 provide as a comparison, is tested its absorption property.
(1) compound concentration is the methylene blue solution of 150mg/L, takes solution 50mL, is added prepared by 0.01g embodiment 1
Adsorbent material, control adsorption temp be 35 DEG C, adsorption time 1h, measure material adsorption capacity be 90.32mg/g.
(2) compound concentration is the methylene blue solution of 150mg/L, takes solution 50mL, is added prepared by 0.01g embodiment 4
Adsorbent material, control adsorption temp be 35 DEG C, adsorption time 1h, measure material adsorption capacity be 116.54mg/g.
(3) compound concentration is the methylene blue solution of 150mg/L, takes solution 50mL, is added prepared by 0.01g comparative example 1
Graphene, control adsorption temp be 35 DEG C, adsorption time 1h, measure material adsorption capacity be 32.79mg/g.
(4) compound concentration is the methylene blue solution of 150mg/L, takes solution 50mL, is added prepared by 0.01g comparative example 2
Graphene, control adsorption temp be 35 DEG C, adsorption time 1h, measure material adsorption capacity be 36.15mg/g.
(5) compound concentration is the methylene blue solution of 150mg/L, takes solution 50mL, is added prepared by 0.01g comparative example 2
Nano Iron-graphite alkene composite material, control adsorption temp is 35 DEG C, adsorption time 1h, and the adsorption capacity for measuring material is
30.56mg/g。
To sum up, Nanoscale Iron molybdenum-graphene composite material provided by the invention is mentioned significantly by load Nanoscale Iron and nanometer molybdenum
The high adsorption capacity of composite material, with more excellent adsorptivity with pure graphene and the only graphene of load iron compared with
Energy；In addition, the load of iron will affect the duty factor of molybdenum, and then influence absorption property.
Above-described specific embodiment has carried out further the purpose of the present invention, technical scheme and beneficial effects
It is described in detail, it should be understood that being not intended to limit the present invention the foregoing is merely a specific embodiment of the invention
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of Nanoscale Iron molybdenum-graphene composite material, which comprises the steps of: stone will be aoxidized
Molysite and molybdenum salt are added after black alkene Yu Shuizhong ultrasonic disperse, then adds reducing agent and reacts up to the Nanoscale Iron molybdenum-graphite
Alkene composite material；The mass ratio of ferro element and graphene oxide is 0.1~5:1 in the molysite；In the molybdenum salt molybdenum element and
The mass ratio of graphene oxide is 0.1~5:1.
2. preparation method according to claim 1, which is characterized in that the graphene oxide is prepared via a method which
To: it will be stirred under graphite powder, sodium nitrate and concentrated sulfuric acid mixing ice bath, potassium permanganate be added, stirring, then temperature rising reflux stirs,
H is added after cooling2O2Reaction is filtered up to the graphene oxide.
3. preparation method according to claim 1, which is characterized in that the molysite be ferric sulfate, ferrous sulfate, iron chloride,
Frerrous chloride, ferrous nitrate, ferric nitrate, ferric phosphate, ferrous phosphate, ferrous pyrophosphate, Na2Fe04, potassium ferrate, ferric bromide,
Ferrous bromide, ferric flouride, ferrous fluoride or thiocyanation iron and its hydrate it is one or more.
4. preparation method according to claim 1, which is characterized in that the molybdenum salt is sodium molybdate, potassium molybdate, ammonium molybdate, molybdenum
Sour lithium, bismuth molybdate, phosphomolybdic acid, ammonium phosphomolybdate or ammonium tetramolybdate and its hydrate it is one or more.
5. preparation method according to claim 1, which is characterized in that the reducing agent is potassium borohydride, sodium borohydride, hydration
One of hydrazine or sodium hypophosphite are a variety of.
6. preparation method according to claim 1, which is characterized in that the temperature of the reaction is 5~40 DEG C, the time 0.5
~4h.
7. preparation method according to claim 1, which is characterized in that the quality of ferro element and graphene oxide in the molysite
Than for 1~3:1；The mass ratio of molybdenum element and graphene oxide is 1~3:1 in the molybdenum salt.
8. a kind of Nanoscale Iron molybdenum-graphene composite material, which is characterized in that pass through any preparation method of claim 1~7
It is prepared.
9. the molybdenum of Nanoscale Iron described in claim 8-graphene composite material having in adsorption aqueous solution system as adsorbent material
Application in machine object or heavy metal ion.
10. applying according to claim 9, which is characterized in that the organic matter be methylene blue, methylene orange, methyl red,
Fast green, rhodamine B, ethamine, aniline, monomethyl amine, monoethyl amine, dimethylamine, diethylamine, trimethylamine, triethylamine, a propylamine, dipropyl
Amine, tripropyl amine (TPA), isopropylamine, ethylenediamine, 1,2- propane diamine, butylamine, octylame, 1,4- butanediamine, 1,10- decamethylene diamine, monoethanolamine,
In diethanol amine, triethanolamine, diphenylamines, Propanolamine, reactive black 5, reddish black, phenol, bisphenol-A, salicylic acid or p-methyl benzenesulfonic acid
It is one or more of；The heavy metal ion be manganese ion, copper ion, lead ion, zinc ion, chromium ion, cadmium ion, mercury ion,
It is one or more of in arsenic ion, cobalt ions or nickel ion.
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