CN113526469A - 一种具有二维多孔结构的水溶性稀土纳米材料、制备方法及用途 - Google Patents
一种具有二维多孔结构的水溶性稀土纳米材料、制备方法及用途 Download PDFInfo
- Publication number
- CN113526469A CN113526469A CN202110804072.1A CN202110804072A CN113526469A CN 113526469 A CN113526469 A CN 113526469A CN 202110804072 A CN202110804072 A CN 202110804072A CN 113526469 A CN113526469 A CN 113526469A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- water
- mixed solution
- soluble
- nano material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 99
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 60
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title abstract description 14
- -1 rare earth compound Chemical class 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000003513 alkali Substances 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims description 36
- 239000011148 porous material Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002105 nanoparticle Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- 229910017544 NdCl3 Inorganic materials 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- 239000011777 magnesium Substances 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910001868 water Inorganic materials 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical class OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 3
- 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
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052790 beryllium Inorganic materials 0.000 claims description 3
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- 229910052793 cadmium Inorganic materials 0.000 claims description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052741 iridium Inorganic materials 0.000 claims description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 239000010955 niobium Substances 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052762 osmium Inorganic materials 0.000 claims description 3
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052702 rhenium Inorganic materials 0.000 claims description 3
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052703 rhodium Inorganic materials 0.000 claims description 3
- 239000010948 rhodium Substances 0.000 claims description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052701 rubidium Inorganic materials 0.000 claims description 3
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052713 technetium Inorganic materials 0.000 claims description 3
- GKLVYJBZJHMRIY-UHFFFAOYSA-N technetium atom Chemical compound [Tc] GKLVYJBZJHMRIY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052714 tellurium Inorganic materials 0.000 claims description 3
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 3
- CKLHRQNQYIJFFX-UHFFFAOYSA-K ytterbium(III) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Yb+3] CKLHRQNQYIJFFX-UHFFFAOYSA-K 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052773 Promethium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 2
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims description 2
- 238000003384 imaging method Methods 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 2
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 claims description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 claims 2
- 239000011133 lead Substances 0.000 claims 1
- 238000002560 therapeutic procedure Methods 0.000 claims 1
- 238000004065 wastewater treatment Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 4
- 239000012467 final product Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 229910001629 magnesium chloride Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052716 thallium Inorganic materials 0.000 description 2
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- PVBRXXAAPNGWGE-LGVAUZIVSA-L disodium 5'-guanylate Chemical compound [Na+].[Na+].C1=2NC(N)=NC(=O)C=2N=CN1[C@@H]1O[C@H](COP([O-])([O-])=O)[C@@H](O)[C@H]1O PVBRXXAAPNGWGE-LGVAUZIVSA-L 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- KUBYTSCYMRPPAG-UHFFFAOYSA-N ytterbium(3+);trinitrate Chemical compound [Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUBYTSCYMRPPAG-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0013—Luminescence
- A61K49/0015—Phosphorescence
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/20—Two-dimensional structures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Geology (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Analytical Chemistry (AREA)
- Biomedical Technology (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Physics & Mathematics (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Toxicology (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
本发明提供一种具有二维多孔结构的水溶性稀土纳米材料及相应的制备方法。所述水溶性稀土纳米材料是通过将选择广泛的稀土化合物、非稀土金属盐和碱溶液按一定次序混合得到的溶液进行水热反应、干燥、煅烧后得到的。本发明的方法操作简单,可根据最终产品所需的孔径、粒径、比表面积等理化参数调控工艺制备中的实验条件,从而制备尺寸可控、比表面积较大的具有二维多孔结构的水溶性稀土纳米材料。
Description
技术领域
本发明涉及纳米材料领域,具体涉及一种具有二维多孔结构的水溶性稀土纳米材料及其 制备方法。
背景技术
稀土纳米材料是在许多领域有广泛的应用的一种特殊材料,具有独特的光学、催化和磁 学性质,可以应用于高质量磷光体、催化剂和生物医药等方面。由于稀土多孔纳米材料具有 良好的生物相容性、稳定性,尤其是其具有高比表面积的多孔结构,就可以负载一些催化剂、 药物和气溶胶等物质,成为新一代动植物细胞或组织的载体,扩展了稀土纳米材料的应用领 域。
目前,制备具有多孔结构的稀土纳米材料已有报道,我国学者在这个方面做出了重要贡 献。例如,利用典型的水热法(Qu XG,Nanoscale 2014,6,1445;Small 2013,24,4262)制备得 到了多孔的稀土纳米材料。
例如,Li Zhou等人(“Li Zhou;Zhenhua Li;Zhen Liu;Meili Yin;Jinsong Ren;Xiaogang Qu, One-step nucleotide-programmed growth of porous upconversionnanoparticles:application to cell labeling and drug delivery.Nanoscale 2014,1445-1452”)利用水热法制备得到了一种多孔 NaYF4:Yb,Er纳米颗粒。该文献中,将Y(NO3)3、Yb(NO3)3、Er(NO3)3在搅拌下混合以形成均 匀溶液。然后在磁力搅拌下将GMP二钠盐水溶液滴加到上述溶液中,1小时后,快速加入 NaF水溶液,将混合物搅拌约10分钟,然后转移到高压釜中,并在140℃下水热处理24小 时。但是该文献的方法得到的稀土纳米材料的比表面积较小(15.76m2g-1)。
Zhenhe Xu等人(“Zhenhe Xu,Ping’an Ma,Chunxia Li,Zhiyao Hou,XuefengZhai,Shanshan Huang,Jun Lin,Monodisperse core-shell structured up-conversionYb(OH)CO3@YbPO4:Er3+ hollow spheres as drug carriers.Biomaterials 2011,4161-4173”)利用水热法制备得到了一种多孔 NaLuF4:Yb,Er纳米材料。该文献中,Yb(OH)CO3的单分散胶体球是通过基于尿素的均相沉 淀工艺制备的。将Yb(NO3)3和尿素[CO(NH2)2]溶解在去离子水中,溶液的总体积约为50mL。 将上述溶液首先在室温磁力搅拌2小时,然后将所得溶液在油浴中在90℃下反应2小时,得 到的悬浮液通过离心分离并用去离子水洗涤数次后收集。将得到的Yb(OH)CO3沉淀物通过超 声分散到去离子水中。然后,将0.1g NH4H2PO4加入上述溶液中,再搅拌60分钟后,将获得 的混合溶液转移到高压釜中密封并在180℃下保持24小时。随着高压釜自然冷却至室温,离 心分离沉淀物,依次用去离子水和乙醇洗涤,然后在80℃空气中干燥12小时。但是该文献 的方法得到稀土纳米材料的比表面积较小(14.87m2g-1),平均尺寸较大(300nm)。
因此,亟需开发一种工艺操作简单、实验条件可控、能够制备出尺寸可控、比表面积较 大的具有二维多孔结构的水溶性稀土纳米材料。
发明内容
为了解决上述问题,本发明提供一种具有二维多孔结构的水溶性稀土纳米材料及相应的 制备方法。所述水溶性稀土纳米材料是通过将选择广泛的稀土化合物、非稀土金属盐和碱溶 液按一定次序混合得到的溶液进行水热反应、干燥、煅烧后得到的。本发明的方法操作简单, 可根据最终产品所需的孔径、粒径、比表面积等理化参数调控工艺制备中的实验条件,从而 制备尺寸可控、比表面积较大的具有二维多孔结构的水溶性稀土纳米材料。
本发明提供一种具有二维多孔结构的水溶性稀土纳米材料,所述水溶性稀土纳米材料以 重量百分比计,包括0.01-99.99%的稀土元素和0.01-99.99%的非稀土元素,其中,所述稀土 元素选自镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、钪和钇中的至少一种,所述非稀土元素选自锂、铍、钠、镁、铝、钾、钙、钛、钒、铬、锰、铁、钴、镍、 铜、锌、镓、锗、铷、锶、锆、铌、钼、锝、钌、铑、钯、银、镉、铟、锡、锑、碲、铯、 钡、铪、钽、钨、铼、锇、铱、铂、金、铊、铅、铋中的至少一种;所述水溶性稀土纳米材 料的直径为20nm-4μm,BET比表面积为30-500m2/g,总孔体积为0.1-1.5cm3/g,平均孔径为 8-30nm。
进一步地,所述水溶性稀土纳米材料为MgAlNd-LDO纳米颗粒,以重量百分比计,包括 2%的稀土元素Nd和98%的非稀土元素Mg和Al,直径为50-70nm,BET比表面积、总孔体积和平均孔径大小分别约为125.1071m2/g、0.466425cm3/g、14.9128nm。这里,LDO是指层 状双金属氧化物的英文缩写。
本发明还提供一种前述具有二维多孔结构的水溶性稀土纳米材料的制备方法,所述方法 包括以下步骤:
S1:将稀土化合物、非稀土金属盐溶解于水中,得到混合溶液1;将碱的水溶液与所述 混合溶液1混合得到混合溶液2;将所述混合溶液2于25℃-250℃的温度下,在2MPa-32MPa 的压力下,进行2h-40h的水热反应,得到混合溶液3;
S2:将所述混合溶液3经干燥后的粉末在350-800℃的温度下煅烧0.5-10小时,获得所 述水溶性稀土纳米材料。
进一步地,S1步骤中,所述稀土化合物选自下述至少一种稀土元素形成的盐:镧、铈、 镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、钪和钇。
进一步地,S1步骤中,所述稀土化合物具体可为NdCl3或YbCl3、ErCl3的混合物。
进一步地,所述稀土化合物的水溶液的摩尔浓度为0.0001-0.1mol/L,具体可为0.0005 mol/L或0.005mol/L。这里的“摩尔浓度”指的是所述混合溶液1中,所述稀土化合物本身的 摩尔浓度。
进一步地,S1步骤中,所述非稀土金属盐选自下述至少一种金属元素形成的金属盐:
锂、铍、钠、镁、铝、钾、钙、钛、钒、铬、锰、铁、钴、镍、铜、锌、镓、锗、铷、 锶、锆、铌、钼、锝、钌、铑、钯、银、镉、铟、锡、锑、碲、铯、钡、铪、钽、钨、铼、 锇、铱、铂、金、铊、铅、铋。
进一步地,S1步骤中,所述稀土化合物具体可为NdCl3或YbCl3、ErCl3的混合物。
进一步地,所述非稀土金属盐的溶液的摩尔浓度为0.0001-1mol/L,具体可为0.005mol/L 或0.05mol/L。这里的“摩尔浓度”指的是所述混合溶液1中,所述非稀土金属盐本身的摩尔 浓度。
进一步地,S1步骤中,所述碱选自下述中的至少一种:碱金属氢氧化物、氨水、碳酸盐、 碳酸氢盐、尿素;所述碱溶液的摩尔浓度为0.001-15mol/L。
进一步地,所述碱金属氢氧化物可选自氢氧化钠、氢氧化钾;所述碳酸氢盐可选自碳酸 氢钠、碳酸氢钾。
进一步地,所述碱具体可为NaOH或NH3·H2O;摩尔浓度具体可为0.1mol/L或0.5mol/L。
进一步地,S1步骤中,所述稀土化合物与所述非稀土金属盐的混合溶液1与所述碱溶液 的体积为50mL:1-500mL。
进一步地,S1步骤中,所述水热反应的温度为优选为120-180℃,具体可为140℃、160℃ 或180℃,反应时间优选为12-24h,具体可为10h、12h或24h。
进一步地,S1步骤中,在所述混合溶液1与所述碱溶液混合后,还包括对所得到的所述 混合溶液2搅拌的步骤,所述搅拌的温度为0-80℃,时间为1-60分钟。
进一步地,所述方法还包括在S2步骤前,将所述混合溶液3进行离心处理和洗涤,所 述离心处理的转速为5000-20000rpm,所述离心处理的时间为2分钟-40分钟。
本发明还提供一种前述的具有二维多孔结构的水溶性稀土纳米材料用于生物医学成像和 治疗、光电催化污水处理等的用途。
本发明的方法具有以下有益的技术效果:
1、本发明通过选择合适的稀土化合物、非稀土金属盐,碱及其浓度,以及所述稀土化 合物、非稀土金属盐的混合溶液与碱溶液的配比,控制水热反应温度和时间,从而控制稀土 纳米材料的尺寸,再通过高温煅烧制备具有二维多孔结构的稀土纳米材料。本发明通过水热- 高温煅烧制备得到了尺寸可控的、比表面积较大的具有二维多孔结构的水溶性的稀土纳米材 料。
2、本发明的制备方法成本低、简便、通用,制备得到的二维稀土纳米材料具有良好的 水溶性及多孔结构。
附图说明
图1为实施例1制备得到的二维多孔、水溶性MgAlNd-LDO纳米颗粒的多晶粉末衍射图。
图2为实施例1制备得到的二维多孔、水溶性MgAlNd-LDO纳米颗粒的透射电子显微镜照片。
图3为实施例1制备得到的二维多孔、水溶性MgAlNd-LDO纳米颗粒的N2吸附曲线测试结果。
图4为实施例2制备得到的二维多孔、水溶性MgAlNd-LDO纳米颗粒的多晶粉末衍射图。
图5为实施例2制备得到的二维多孔、水溶性MgAlNd-LDO纳米颗粒的透射电子显微镜照片。
图6为实施例2制备得到的二维多孔、水溶性MgAlNd-LDO纳米颗粒的N2吸附曲线测试结果。
具体实施方式
下述实施例中所使用的实验方法如无特殊说明,均为常规方法;下述实施例中所用的试 剂、材料等,如无特殊说明,均可从商业途径得到。
实施例
以下结合实施例对发明做详细的说明:
实施例1、一种具有二维多孔结构的水溶性稀土纳米材料MgAlNd-LDO,以重量百分比 计,包括2%的稀土元素Nd和98%的非稀土元素Mg和Al,直径为50-70nm,BET比表面 积、总孔体积和平均孔径大小分别约为125.1071m2/g、0.466425cm3/g、14.9128nm。
制备方法如下:
S1:将稀土化合物NdCl3·6H2O、非稀土金属盐MgCl2·6H2O、AlCl3·9H2O溶解于水中,得到50mL混合溶液1,摩尔浓度为0.3mol/L,其中,原料的摩尔比w =[MgCl2·6H2O]/[AlCl3·9H2O]/[NdCl3·6H2O]=2:0.95:0.05;
制备100mLNaOH、Na2CO3的水溶液,摩尔浓度为0.15mol/L,其中,两种碱的摩尔比 w=[NaOH]/[Na2CO3]=1:1;
将100mL两种碱的水溶液与50mL混合溶液1混合,在25℃搅拌大约10分钟,得到混合溶液2;
将混合溶液2放入高压反应釜中于120℃的温度下、在24MPa的压力下进行水热反应, 12小时后取出,降温至室温,得到混合溶液3;
S2:将混合溶液3在10000rpm的转速下高速离心8分钟,用去离子水依次清洗沉淀、再高速离心以除去吸附的离子,干燥沉淀得到粉末1;
将粉末1在500℃下高温煅烧4小时,得到所需的水溶性稀土纳米材料样品。
将所得的水溶性稀土纳米材料样品在120℃下活化6h。氮气吸附解吸曲线及比表面积均 在低压范围内(P/P0=0.01)使用BET模型测量,孔径大小使用BJH方法测量。
如图1所示,可看出水溶性多孔MgAlNd-LDO稀土纳米材料的XRD数据的110、200、220的衍射峰与MgO标准卡片(JCPDS Card No.45-0946)很好的匹配,证明了MgAlNd-LDO 纳米材料的成功合成。
如图2所示,该图为水溶性多孔MgAlNd-LDO稀土纳米材料样品的形貌和粒径采用透射 电子显微镜测定的结果,MgAlNd-LDO主要为二维片状纳米颗粒,直径约为50-70nm,尺寸 较小,且由图可得到通过该发明的方法更加简单的制备孔状结构的稀土纳米材料。
如图3所示,BET比表面积、总孔体积和平均孔径大小分别约为125.1071m2/g、0.466425 cm3/g、14.9128nm,证明由该方法合成的稀土纳米材料为多孔且比表面积较大,孔径也相对 较大,可增强材料的应用性能。
实施例2
一种具有二维多孔结构的水溶性稀土纳米材料MgAlNd-LDO,以重量百分比计,包括 2%的稀土元素Nd和98%的非稀土元素Mg和Al,直径为100-120nm,BET比表面积、总孔体积和平均孔径大小分别约为87.8129m2/g、0.201601cm3/g、9.1832nm。
制备方法如下:
S1:将稀土化合物NdCl3·6H2O、非稀土金属盐MgCl2·6H2O、AlCl3·9H2O溶解于水中,得到50mL混合溶液1,摩尔浓度为0.3mol/L,其中,原料的摩尔比w =[MgCl2·6H2O]/[AlCl3·9H2O]/[NdCl3·6H2O]=2:0.95:0.05;
制备100mLNaOH、Na2CO3的水溶液,摩尔浓度为0.15mol/L,其中,两种碱的摩尔比 w=[NaOH]/[Na2CO3]=1:1;
将100mL两种碱的水溶液与50mL混合溶液1混合,在25℃搅拌大约10分钟,得到混合溶液2;
将混合溶液2放入高压反应釜中于160℃的温度下、在24MPa的压力下进行水热反应, 12小时后取出,降温至室温,得到混合溶液3;
S2:将混合溶液3在10000rpm的转速下高速离心8分钟,用去离子水依次清洗沉淀、再高速离心以除去吸附的离子,干燥沉淀得到粉末1;
将粉末1在500℃下高温煅烧4小时,得到所需的水溶性稀土纳米材料样品。
将所得的水溶性稀土纳米材料样品在120℃下活化6h。氮气吸附解吸曲线及比表面积均 在低压范围内(P/P0=0.01)使用BET模型测量,孔径大小使用BJH方法测量。
如图4所示,可看出水溶性多孔MgAlNd-LDO稀土纳米材料的110、200、220的衍射峰与MgO标准卡片(JCPDS Card No.45-0946)很好的匹配,证明了MgAlNd-LDO纳米材料的 成功合成。
如图5所示,为水溶性多孔MgAlNd-LDO稀土纳米材料样品的形貌和粒径采用透射电子 显微镜测定的结果,MgAlNd-LDO为二维片状纳米颗粒,直径约为100-120nm,由图可得通 过该发明的方法更加简单的制备孔状结构的稀土纳米材料。但是由于改变了实验的温度,所 以合成出来的多孔MgAlNd-LDO稀土纳米材料较实施例1的尺寸较大,孔较小,但形貌没有 改变,同样是二维片状纳米材料。由此也可证明通过改变实验温度可控制由该发明方法合成 出来的稀土纳米材料的尺寸大小。
如图6所示,BET比表面积、总孔体积和平均孔径大小分别约为87.8129m2/g、0.201601cm3/g、9.1832nm。
证明由该方法合成的稀土纳米材料为多孔且比表面积较大,孔径也相对较大,可增强材 料的应用性能。但是由于改变了实验的温度,所以合成出来的多孔MgAlNd-LDO稀土纳米材 料较实施例1的比表面积、总孔体积和平均孔径大小较小,由此也可证明通过改变实验温度 可控制由该发明方法合成出来的稀土纳米材料的比表面积、总孔体积和平均孔径大小。
以上所述,仅是本发明的较佳实施例而已,并非是对本发明作任何其他形式的限制,而 依据本发明的技术实质所作的任何修改或等同变化,仍属于本发明所要求保护的范围。
Claims (10)
1.一种具有二维多孔结构的水溶性稀土纳米材料,其特征在于,以重量百分比计,所述水溶性稀土纳米材料包括0.01-99.99%的稀土元素和0.01-99.99%的非稀土元素,其中,所述稀土元素选自镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、钪和钇中的至少一种,所述非稀土元素选自锂、铍、钠、镁、铝、钾、钙、钛、钒、铬、锰、铁、钴、镍、铜、锌、镓、锗、铷、锶、锆、铌、钼、锝、钌、铑、钯、银、镉、铟、锡、锑、碲、铯、钡、铪、钽、钨、铼、锇、铱、铂、金、铊、铅、铋中的至少一种;
所述水溶性稀土纳米材料的直径为20nm-4μm,BET比表面积为30-500m2/g,总孔体积为0.1-1.5cm3/g,平均孔径为8-30nm。
2.根据权利要求1所述的具有二维多孔结构的水溶性稀土纳米材料,其特征在于,所述水溶性稀土纳米材料为MgAlNd-LDO纳米颗粒,颗粒直径为50-70nm,BET比表面积、总孔体积和平均孔径大小分别为220.5425m2/g、0.782559cm3/g、14.1933nm。
3.一种权利要求1或2所述的具有二维多孔结构的水溶性稀土纳米材料的制备方法,其特征在于,所述方法包括以下步骤:
S1:将稀土化合物、非稀土金属盐溶解于水中,得到混合溶液1;将碱的水溶液与所述混合溶液1混合得到混合溶液2;将所述混合溶液2于25℃-250℃的温度下,在2MPa-32MPa的压力下,进行2h-40h的水热反应,得到混合溶液3;
S2:将所述混合溶液3经干燥后的粉末在350-800℃的温度下煅烧0.5-10小时,获得所述水溶性稀土纳米材料。
4.根据权利要求3所述的方法,其特征在于,S1步骤中,所述稀土化合物为NdCl3或YbCl3、ErCl3的混合物;
所述稀土化合物的水溶液的摩尔浓度为0.0001-0.1mol/L。
5.根据权利要求3所述的方法,其特征在于,S1步骤中,所述非稀土金属盐为Mg(NO3)2·6H2O、Al(NO3)3·9H2O或Ni(NO3)2·6H2O;
所述非稀土金属盐的溶液的摩尔浓度为0.0001-1mol/L。
6.根据权利要求3所述的方法,其特征在于,S1步骤中,所述碱选自下述中的至少一种:
碱金属氢氧化物、氨水、碳酸盐、碳酸氢盐、尿素;
所述碱溶液的摩尔浓度为0.001-15mol/L。
7.根据权利要求6所述的方法,其特征在于,S1步骤中,所述稀土化合物与所述非稀土金属盐的混合溶液1与所述碱溶液的体积为50mL:1-500mL。
8.根据权利要求7所述的方法,其特征在于,S1步骤中,在所述混合溶液1与所述碱溶液混合后,还包括对所得到的所述混合溶液2搅拌的步骤,所述搅拌的温度为0-80℃,时间为1-60分钟。
9.根据权利要求8述的方法,其特征在于,所述方法还包括在S2步骤前,将所述混合溶液3进行离心处理和洗涤,所述离心处理的转速为5000-20000rpm,所述离心处理的时间为2分钟-40分钟。
10.一种根据权利要求1或2所述的具有二维多孔结构的水溶性稀土纳米材料用于生物医学成像和治疗、光电催化、污水处理的用途。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110804072.1A CN113526469A (zh) | 2021-07-16 | 2021-07-16 | 一种具有二维多孔结构的水溶性稀土纳米材料、制备方法及用途 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110804072.1A CN113526469A (zh) | 2021-07-16 | 2021-07-16 | 一种具有二维多孔结构的水溶性稀土纳米材料、制备方法及用途 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN113526469A true CN113526469A (zh) | 2021-10-22 |
Family
ID=78128272
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110804072.1A Pending CN113526469A (zh) | 2021-07-16 | 2021-07-16 | 一种具有二维多孔结构的水溶性稀土纳米材料、制备方法及用途 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113526469A (zh) |
Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2002085787A1 (de) * | 2001-04-19 | 2002-10-31 | Süd-Chemie AG | Verfahren zur herstellung von hydrotalciten |
US6852670B1 (en) * | 1999-04-06 | 2005-02-08 | Japan Science And Technology Agency | Method for manufacturing anion-layered double hydroxide intercalation compounds and compounds produced thereby |
CN101302031A (zh) * | 2007-05-09 | 2008-11-12 | 广东炜林纳功能材料有限公司 | 镁铝稀土三元类水滑石、其制备方法及用途 |
JP2009184869A (ja) * | 2008-02-06 | 2009-08-20 | National Institute For Materials Science | 層状希土類水酸化物を製造する方法 |
CN103487473A (zh) * | 2013-09-26 | 2014-01-01 | 内蒙古科技大学 | 稀土改性的氧化锌气敏传感器及其制备方法 |
CN104087301A (zh) * | 2014-07-03 | 2014-10-08 | 上海交通大学 | 一种通用多孔稀土掺杂上转换纳米材料的制备方法 |
CN108579720A (zh) * | 2018-05-14 | 2018-09-28 | 福州大学 | 一种以稀土元素掺杂的类水滑石为前驱体的硫化氢选择性氧化催化剂及其制备方法 |
JP2018184306A (ja) * | 2017-04-24 | 2018-11-22 | 丸尾カルシウム株式会社 | ハイドロタルサイト類化合物、該ハイドロタルサイト類化合物を配合してなる樹脂組成物及びその成形体 |
CN109279616A (zh) * | 2018-12-03 | 2019-01-29 | 包头稀土研究院 | 改性膨润土的制备方法 |
CN110629288A (zh) * | 2019-10-24 | 2019-12-31 | 营口理工学院 | 一种水热技术制备晶须状铝酸钆粉体材料的方法 |
CN111701609A (zh) * | 2020-07-09 | 2020-09-25 | 中国科学院过程工程研究所 | 一种稀土基水滑石辅助钒磷氧催化剂的方法 |
US20200306725A1 (en) * | 2019-03-25 | 2020-10-01 | King Fahd University Of Petroleum And Minerals | Ca-y-carbonate nanosheets, their use, and synthesis |
US20200325031A1 (en) * | 2017-12-22 | 2020-10-15 | Vito Nv | Lanthanide-doped layered double hydroxides and method of producing same |
-
2021
- 2021-07-16 CN CN202110804072.1A patent/CN113526469A/zh active Pending
Patent Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6852670B1 (en) * | 1999-04-06 | 2005-02-08 | Japan Science And Technology Agency | Method for manufacturing anion-layered double hydroxide intercalation compounds and compounds produced thereby |
WO2002085787A1 (de) * | 2001-04-19 | 2002-10-31 | Süd-Chemie AG | Verfahren zur herstellung von hydrotalciten |
CN101302031A (zh) * | 2007-05-09 | 2008-11-12 | 广东炜林纳功能材料有限公司 | 镁铝稀土三元类水滑石、其制备方法及用途 |
JP2009184869A (ja) * | 2008-02-06 | 2009-08-20 | National Institute For Materials Science | 層状希土類水酸化物を製造する方法 |
CN103487473A (zh) * | 2013-09-26 | 2014-01-01 | 内蒙古科技大学 | 稀土改性的氧化锌气敏传感器及其制备方法 |
CN104087301A (zh) * | 2014-07-03 | 2014-10-08 | 上海交通大学 | 一种通用多孔稀土掺杂上转换纳米材料的制备方法 |
JP2018184306A (ja) * | 2017-04-24 | 2018-11-22 | 丸尾カルシウム株式会社 | ハイドロタルサイト類化合物、該ハイドロタルサイト類化合物を配合してなる樹脂組成物及びその成形体 |
US20200325031A1 (en) * | 2017-12-22 | 2020-10-15 | Vito Nv | Lanthanide-doped layered double hydroxides and method of producing same |
CN108579720A (zh) * | 2018-05-14 | 2018-09-28 | 福州大学 | 一种以稀土元素掺杂的类水滑石为前驱体的硫化氢选择性氧化催化剂及其制备方法 |
CN109279616A (zh) * | 2018-12-03 | 2019-01-29 | 包头稀土研究院 | 改性膨润土的制备方法 |
US20200306725A1 (en) * | 2019-03-25 | 2020-10-01 | King Fahd University Of Petroleum And Minerals | Ca-y-carbonate nanosheets, their use, and synthesis |
CN110629288A (zh) * | 2019-10-24 | 2019-12-31 | 营口理工学院 | 一种水热技术制备晶须状铝酸钆粉体材料的方法 |
CN111701609A (zh) * | 2020-07-09 | 2020-09-25 | 中国科学院过程工程研究所 | 一种稀土基水滑石辅助钒磷氧催化剂的方法 |
Non-Patent Citations (4)
Title |
---|
DENGFENG WANG ET AL.: "La-modified mesoporous Mg–Al mixed oxides:effective and stable base catalysts for the synthesis of dimethyl carbonate from methyl carbamate and methanol", 《CATALYSIS SCIENCE & TECHNOLOGY》 * |
FUHAI WANG: "One-pot synthesis of CeO2/Mg-Al layered double oxide nanosheets for efficient visible-light induced photo-reduction of Cr(VI)", 《COLLOIDS AND SURFACES A》 * |
YI QIAN ET AL.: "Hydrothermal Synthesis of Lanthanum-Doped MgAl-Layered Double Hydroxide/Graphene Oxide Hybrid and Its Application as Flame Retardant for Thermoplastic Polyurethane", 《ADVANCES IN POLYMER TECHNOLOGY》 * |
郑建华等: "规整、均一纳米水滑石晶体的水热合成与表征", 《化学学报》 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Yang et al. | Fine tuning of the dimensionality of zinc silicate nanostructures and their application as highly efficient absorbents for toxic metal ions | |
Zhu et al. | Self-assembled 3D porous flowerlike α-Fe 2 O 3 hierarchical nanostructures: synthesis, growth mechanism, and their application in photocatalysis | |
US11027259B2 (en) | Preparation method for hollow molybdate composite microspheres and method for catalyzing ammonia borane hydrolysis to produce hydrogen | |
Pal et al. | Hierarchically order porous lotus shaped nano-structured MnO 2 through MnCO 3: chelate mediated growth and shape dependent improved catalytic activity | |
JP4478766B2 (ja) | 球状シリカ多孔質粒子及びその製造方法 | |
CN113287635B (zh) | 用于抗菌、防霉的掺杂金属氧化物纳米颗粒、分散体或粉体的制备方法 | |
EP1711259A2 (en) | Nano-structured particles with high thermal stability | |
Fu et al. | Room temperature synthesis of a novel γ-MnO2 hollow structure for aerobic oxidation of benzyl alcohol | |
Pezeshkpour et al. | Synthesis and characterization of nanocrystalline NiO-GDC via sodium alginate-mediated ionic sol-gel method | |
CN108083316A (zh) | 一种纳米稀土氧化物粉体的制备方法 | |
CN112830464A (zh) | 一种锶掺杂羟基磷灰石微米管及其制备方法 | |
CN100453469C (zh) | 一种赤铁矿纳米立方体的制备方法 | |
Tang et al. | Construction of Ce (OH) 4 nanostructures from 1D to 3D by a mechanical force-driven method | |
CN102530976A (zh) | 一种多级结构硼酸镁空心微球的制备方法 | |
CN112125344A (zh) | 一种单分散纳米铁氧化物分散体的制备方法 | |
WO2017068350A1 (en) | Methods of making metal oxide catalysts | |
CN113526469A (zh) | 一种具有二维多孔结构的水溶性稀土纳米材料、制备方法及用途 | |
Chen et al. | Low-temperature preparation of α-Al2O3 with the assistance of seeding a novel hydroxyl aluminum oxalate | |
CN111498880A (zh) | 一种双水相体系温和制备拜尔石微球的方法 | |
CN107587195B (zh) | 一类钽基稀土多酸及其纳米晶的制备方法 | |
CN113680291B (zh) | 一种顺磁性金属氧化物/尖晶石/碳复合微球的制备方法 | |
Jiu et al. | Preparation and luminescent properties of hollow Y2O3: Tb3+ microspheres | |
CN113996802B (zh) | 一种立方体铜纳米粒子的制备方法 | |
JP4484193B2 (ja) | 球状マイクロポアシリカ多孔質粒子及びその製造方法 | |
CN1086206C (zh) | 一种制备金属氧化物超细粉的溶剂萃取反胶团法及其用途 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211022 |