CN108298502A - A method of preparing dispersion nano-metal-oxide and Nano metal powder - Google Patents
A method of preparing dispersion nano-metal-oxide and Nano metal powder Download PDFInfo
- Publication number
- CN108298502A CN108298502A CN201810037875.7A CN201810037875A CN108298502A CN 108298502 A CN108298502 A CN 108298502A CN 201810037875 A CN201810037875 A CN 201810037875A CN 108298502 A CN108298502 A CN 108298502A
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- Prior art keywords
- sulfate
- oxide
- metal
- nano
- polyacrylic acid
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- 239000006185 dispersion Substances 0.000 title claims abstract description 52
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 40
- 239000002184 metal Substances 0.000 title claims abstract description 40
- 239000000843 powder Substances 0.000 title claims abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 109
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 103
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 102
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 102
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 88
- 239000004584 polyacrylic acid Substances 0.000 claims abstract description 88
- 239000013049 sediment Substances 0.000 claims abstract description 48
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 136
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 79
- 235000019441 ethanol Nutrition 0.000 claims description 70
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 45
- 238000001816 cooling Methods 0.000 claims description 36
- 238000013019 agitation Methods 0.000 claims description 32
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 27
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 25
- 239000003960 organic solvent Substances 0.000 claims description 21
- 239000007864 aqueous solution Substances 0.000 claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 6
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 238000013459 approach Methods 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 3
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 3
- 229910001940 europium oxide Inorganic materials 0.000 claims description 3
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 3
- 229910003437 indium oxide Inorganic materials 0.000 claims description 3
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 239000005751 Copper oxide Substances 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- GEZAXHSNIQTPMM-UHFFFAOYSA-N dysprosium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Dy+3].[Dy+3] GEZAXHSNIQTPMM-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229910003451 terbium oxide Inorganic materials 0.000 claims description 2
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 claims description 2
- 229910001887 tin oxide Inorganic materials 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 abstract description 36
- 239000002245 particle Substances 0.000 abstract description 23
- 238000002955 isolation Methods 0.000 abstract description 13
- 229910021653 sulphate ion Inorganic materials 0.000 abstract description 7
- 239000002667 nucleating agent Substances 0.000 abstract description 5
- 238000003837 high-temperature calcination Methods 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 239000003495 polar organic solvent Substances 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 39
- 238000001354 calcination Methods 0.000 description 35
- 238000005352 clarification Methods 0.000 description 34
- 239000008367 deionised water Substances 0.000 description 34
- 229910021641 deionized water Inorganic materials 0.000 description 34
- 239000002105 nanoparticle Substances 0.000 description 25
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 24
- 150000003839 salts Chemical class 0.000 description 13
- 229940103272 aluminum potassium sulfate Drugs 0.000 description 12
- 230000008569 process Effects 0.000 description 10
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 8
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 8
- -1 and in the step 1) Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 229910017053 inorganic salt Inorganic materials 0.000 description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 4
- 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 description 4
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 230000005291 magnetic effect Effects 0.000 description 3
- 238000005549 size reduction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 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
- MKNZSAIPAVSJSI-UHFFFAOYSA-N [Tb].S(O)(O)(=O)=O Chemical compound [Tb].S(O)(O)(=O)=O MKNZSAIPAVSJSI-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 2
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 description 2
- 229910000331 cadmium sulfate Inorganic materials 0.000 description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 2
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 2
- 229940044175 cobalt sulfate Drugs 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- 229960004643 cupric oxide Drugs 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- FLWXWKDFOLALOB-UHFFFAOYSA-H dysprosium(3+);trisulfate Chemical compound [Dy+3].[Dy+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FLWXWKDFOLALOB-UHFFFAOYSA-H 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- WLYAEQLCCOGBPV-UHFFFAOYSA-N europium;sulfuric acid Chemical compound [Eu].OS(O)(=O)=O WLYAEQLCCOGBPV-UHFFFAOYSA-N 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 229910000337 indium(III) sulfate Inorganic materials 0.000 description 2
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 description 2
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 2
- 235000019341 magnesium sulphate Nutrition 0.000 description 2
- 230000010534 mechanism of action Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- OJSWEKSDNUORPG-UHFFFAOYSA-H neodymium(3+);trisulfate Chemical compound [Nd+3].[Nd+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OJSWEKSDNUORPG-UHFFFAOYSA-H 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229910000348 titanium sulfate Inorganic materials 0.000 description 2
- 229910000347 yttrium sulfate Inorganic materials 0.000 description 2
- RTAYJOCWVUTQHB-UHFFFAOYSA-H yttrium(3+);trisulfate Chemical compound [Y+3].[Y+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RTAYJOCWVUTQHB-UHFFFAOYSA-H 0.000 description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 2
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012702 metal oxide precursor Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- HIRWGWMTAVZIPF-UHFFFAOYSA-N nickel;sulfuric acid Chemical compound [Ni].OS(O)(=O)=O HIRWGWMTAVZIPF-UHFFFAOYSA-N 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- UBBSASFKEJHWOE-UHFFFAOYSA-M potassium hydrogen sulfate sulfuric acid Chemical compound [K+].OS(O)(=O)=O.OS([O-])(=O)=O UBBSASFKEJHWOE-UHFFFAOYSA-M 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- 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
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- 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
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
-
- 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
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
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Abstract
The invention discloses a kind of methods preparing dispersion nano-metal-oxide and Nano metal powder, metal sulfate and potassium sulfate mixed solution are precipitated in weakly polar organic solvent, it uses polyacrylic acid as nucleating agent simultaneously, forms the state of nanometer granular potassium sulfate dispersion isolation nanometer sulphate particle in sediment.High-temperature calcination decomposition is carried out after sediment is dried, which resolves into metal oxide, and granular potassium sulfate plays buffer action always.The nano-metal-oxide that can be disperseed after washing.By calcined product secondary clacining in a reducing atmosphere, the Nano metal powder that can must disperse after washing.The present invention can be prepared good dispersion with rapid batch, crystallize perfect nano-metal-oxide or Nano metal powder.
Description
Technical field
The present invention relates to a kind of technologies preparing dispersion nano-metal-oxide and Nano metal powder, belong to nano powder system
Standby field.
Background technology
Nano-metal-oxide has skin effect, quantum size effect, bulk effect and macro quanta tunnel effect, because
And there is unique calorifics, optics, electricity, magnetics and chemical property, it is answered in fields such as electronics, chemical industry, machinery, biomedicines
With extensive.
But nano-metal-oxide is easy to happen reunion and sintering in preparation process, leads to the nanometer for being difficult to prepare dispersion
Particle.The industrial at present and widely used liquid phase method in laboratory prepares nano-metal-oxide, synthesizes receive in the solution first
Rice metal oxide precursor, such as hydroxide, oxalates, carbonate, presoma then decomposed to obtain in high-temperature calcination
Nano-metal-oxide.The temperature of calcining and decomposing is often relatively high, needs 350 DEG C as magnesium carbonate decomposes, iron hydroxide turns completely
Become iron oxide and need 500 DEG C, and to obtain the aluminium oxide of α phases, it is necessary to pass through 1000 DEG C of high temperature.At such high temperatures,
Metal oxide nanoparticles, which are difficult to avoid that, can occur to reunite and be sintered.So far, only iron oxide and zinc oxide can make
Mono-dispersed nano particle is prepared with hydro-thermal method or forced hydrolysis method, and less efficient.And height is had to pass through for others
The metal oxide of temperature calcining, the prior art are difficult to prepare the nano-powder of polymolecularity on a large scale.
Solving the problems, such as a kind of this possible method is：High-melting-point water-soluble inorganic salt is used mutually to prevent metal oxygen for isolation
The reunion and sintering of compound nano particle make nano particle be disperseed to be isolated by solid salt always in the high temperature process, are used after calcining
Water washes off inorganic salts, you can the metal oxide nanoparticles disperseed.But the critical issue of the method is how to obtain
Presoma nano particle is simultaneously effectively isolated and is disperseed with nanometer salt particle by the water soluble salt particle of Nano grade.Commercial water
Dissolubility such as NaCl (801 DEG C of fusing point), K2SO4Particles such as (1067 DEG C of fusing points) are generally in tens microns, with so coarse
The granular precursor of nanoscale can not be isolated for grain.And it is also difficult to by the methods of ball milling by the size reduction of salt particle to receiving
Meter level is other.This seminar early period wraps up one using saliferous microemulsion method (Chinese patent 201610365324.4) nano grain surface
Layer salt crust, and finally prepare mono-dispersed nano oxide particle.But the method cost of raw material is higher, and process is more numerous
It is trivial, it is not suitable for mass producing.
Reunite in conclusion metal oxide nanoparticles are difficult to avoid that in preparation process in high-temperature calcination decomposable process
And sintering, and the prior art is difficult to solve the problems, such as this.Using high-melting-point water-soluble inorganic salt come be isolated granular precursor be solve
One possible approaches of this problem, but on condition that must realize dispersion and isolation of the soluble-salt to presoma nano particle.If
Can be by the size reduction of high-melting-point inorganic salt particle to Nano grade, and use inorganic salts nano particle by presoma nano particle
It scatter, will effectively avoid reunion and Sintering Problem of the metal oxide nanoparticles in high-temperature burning process, and prepare
Go out the metal oxide nanoparticles of polymolecularity.
Invention content
Technical problem：The present invention provides the sides that a kind of rapid batch prepares nano-metal-oxide and Nano metal powder
Method can be stablized and prepare the nano particle that grain size is less than 100nm, and prepared nano-metal-oxide crystallinity is good, prepares
Nano metal powder crystallize perfect, electric conductivity and magnetic property it is good.
Technical solution：The method of the preparation dispersion nano-metal-oxide of the present invention, includes the following steps：
1) sulfate corresponding to metal oxide is configured to mixed aqueous solution with potassium sulfate；
2) polyacrylic acid is added in the mixed aqueous solution of the step 1) configuration；
3) mixed aqueous solution containing polyacrylic acid under agitation, is instilled into organic solvent, obtains sediment；
4) by sediment organic solvent washing 1-2 times, a nanometer sulfate mixture is obtained after dry；
5) the nanometer sulfate mixture is calcined below potassium sulfate fusing point；
6) calcined product of the step 5) is washed with water, dried, obtain nano-metal-oxide.
Further, prepared by the present invention disperses in the method for nano-metal-oxide, in the step 1), metal oxide
For aluminium oxide, titanium oxide, iron oxide, nickel oxide, cobalt oxide, copper oxide, magnesia, zirconium oxide, cadmium oxide, tin oxide, oxidation
Zinc, indium oxide, yttrium oxide, europium oxide, cerium oxide, lanthana, terbium oxide, dysprosia or neodymia.
Further, prepared by the present invention disperses in the method for nano-metal-oxide, in step 1), potassium sulfate and metal sulphur
The molar ratio of hydrochlorate is no less than 1: 1, and in the mixed aqueous solution of preparation, a concentration of 0.01mol/L of potassium sulfate is to being saturated.
Further, prepared by the present invention disperses in the method for nano-metal-oxide, the addition of polyacrylic acid in step 2)
Amount is the 0.5%-100% of sulfate gross mass.
Further, prepared by the present invention disperses in the method for nano-metal-oxide, and the organic solvent in step 3) is first
Alcohol, ethyl alcohol, the tert-butyl alcohol, acetone or dimethylformamide, the organic solvent in the step 4) are methanol, ethyl alcohol, the tert-butyl alcohol, third
Ketone or dimethylformamide.
The method of the preparation dispersion Nano metal powder of the present invention, includes the following steps：
1) sulfate corresponding to metal is configured to mixed aqueous solution with potassium sulfate；
2) polyacrylic acid is added in the mixed aqueous solution of the step 1) configuration；
3) mixed aqueous solution containing polyacrylic acid under agitation, is instilled into organic solvent, obtains sediment；
4) by sediment organic solvent washing 1-2 times, a nanometer sulfate mixture is obtained after dry；
5) the nanometer sulfate mixture is calcined below potassium sulfate fusing point；
6) calcined product for obtaining step 5) carries out secondary clacining in a reducing atmosphere, is washed with water, dries after cooling,
Obtain Nano metal powder.
Further, prepared by the present invention disperses in the method for Nano metal powder, and in the step 1), metal is iron, nickel, cobalt
Or copper.
Further, prepared by the present invention disperses in the method for Nano metal powder, in step 1), potassium sulfate and metal sulfate
Molar ratio be no less than 1: 1, in the mixed aqueous solution of preparation, a concentration of 0.01mol/L of potassium sulfate is to being saturated.
Further, prepared by the present invention disperses in the method for Nano metal powder, and the addition of polyacrylic acid is in step 2)
The 0.5%-100% of sulfate gross mass.
Further, prepared by the present invention disperses in the method for Nano metal powder, and the organic solvent in step 3) is methanol, second
Alcohol, the tert-butyl alcohol, acetone or dimethylformamide, the organic solvent in the step 4) be methanol, ethyl alcohol, the tert-butyl alcohol, acetone or
Dimethylformamide.
In the present invention, certain metal sulfate is configured to mixed sulfate aqueous solution with potassium sulfate, and in mixed sulfate water
The polyacrylic acid of 0.5% or more sulfuric acid salt quality is added in solution.When mixed sulfate aqueous solution instills organic solvent, can analyse
Go out the mixed sediment of the sulfate nano particle and potassium sulfate nano particle, and forms potassium sulfate nano particle to the sulfate
The isolation of nano particle.The metal sulfate resolves into metal oxide in subsequent calcination process, and potassium sulfate is not
Become and plays buffer action always.
Advantageous effect：Compared with prior art, the present invention haing the following advantages：
The existing method for preparing nano-metal-oxide, such as chemical precipitation method, sol-gal process, usually make first
For presoma, such as metal carbonate or hydroxide is gone out, then calcines at high temperature, resolve into metal oxide.But particle
Size is smaller, and surface energy is bigger, easier reunion.Either in dehydration and drying process still in high-temperature burning process, metal
Oxide particle can inevitably reunite, and at high temperature between particle it also occur that being sintered, so being difficult to
Prepare the metal oxide nano particles of high dispersive.
The reunion and sintering of granular precursor can be mutually prevented using isolation, studying more isolation at present mutually has carbon, water
Soluble inorganic salt etc..The residual carbon of wherein carbon isolation method is difficult to clean off, and has larger impact to nano particle performance.Water-soluble inorganic
Although salt isolation method theoretically has good isolation effect, and is easy washing and removes, simple and easy to do.But water-soluble inorganic salt
Particle size it is often very big, if NaCl particle sizes are often at tens microns or more, with so coarse salt particle be difficult by
The effectively dispersion and isolation of the granular precursor of Nano grade.Therefore, with high-melting-point water soluble salt do isolation phase critical issue be
It prepares the water soluble salt particle of Nano grade and presoma nano particle is effectively isolated and is disperseed with nanometer salt particle.
Solubility declines to a great extent in weakly polar organic solvent characteristic that present invention utilizes sulfate, by sulphate particle
It is precipitated from organic solvent, but the sulphate particle size obtained so under normal conditions is in the micron-scale.The present invention is by polypropylene
Acid can be used as the nucleating agent of sulfate, after polyacrylic acid is added in mixed sulfate solution, can greatly improve nucleation rate simultaneously
Reduce sulphate particle size.It, can be effectively by sulphate particle when the polyacrylic acid of 0.5% or more sulfuric acid salt quality is added
Size reduction is to 100nm or less.
The mechanism of action of polyacrylic acid it is not immediately clear, nucleating agent is also not present in organic solvent precipitation method technical field
Concept.In metal freezing field, nucleating agent is solid particle, can be used as forming core substrate when metal freezing, to significantly
It improves nucleation rate, reduce crystallite dimension.And polyacrylic acid is dissolved in the high molecular material of water, the mechanism of action in process of setting
Solid nucleating agent obviously have very big difference.It is according to the prior art that polyacrylic acid, which promotes the effect of potassium sulfate forming core, in the present invention
Knowledge is unforeseen.
The sulfate drawn up corresponding to standby metal oxide (or metal powder) is configured to mix by the present invention with potassium sulfate
Sulfate solution, and the polyacrylic acid of 0.5% or more sulfuric acid salt quality is added in mixed sulfate aqueous solution.Work as mix sulphur
When acid salt aqueous solution instills organic solvent, the mixed sediment of the sulfate nano particle and potassium sulfate nano particle can be precipitated,
And form isolation of the potassium sulfate nano particle to the sulfate nano particle.
By taking nickel sulfate and potassium sulfate mixed solution as an example, when the molar ratio of potassium sulfate and nickel sulfate is more than 1: 1, it is added to second
Mixing nanometer sulfate sediment can be obtained in the organic solvents such as alcohol, and a nanometer granular potassium sulfate dispersion can be formed in sediment
The state of nanometer sulfuric acid nickel particle is isolated, as shown in Figure of description 1.In subsequent high-temperature burning process, nanometer nickel sulfate
It decomposes and generates nano-nickel oxide, nanometer potassium sulfate does not decompose.In the generating process of nano-nickel oxide, always by nanometer potassium sulfate
Solid particle dispersions are simultaneously isolated, therefore will not be occurred to reunite and be sintered, and dispersion nano oxygen can be obtained after washing removal potassium sulfate
Change nickel, as shown in Figure of description 2.If to calcined product secondary clacining in a reducing atmosphere, the nanometer that can must disperse after washing
Nickel powder.
If dispersant is added in organic solvent, it will further improve the isolation effect of nanometer potassium sulfate.Dispersant
Including polyethylene glycol, polyvinylpyrrolidone, carboxylic acids surfactant etc..
The present invention can prepare the nano-metal-oxide of favorable dispersibility with rapid batch, solve nano-metal-oxide
Reunion and Sintering Problem, and since calcination temperature is up to 1000 DEG C or more, prepared nano-metal-oxide knot
Crystalline substance is good.Same reason, Nano metal powder prepared by the present invention crystallizes perfect, electric conductivity and magnetic property is good.
Agents useful for same of the present invention is common cheap reagent, and method is easy, is easy to mass produce.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of nanometer nickel sulfate and nanometer potassium sulfate mixture that the present invention obtains.
Fig. 2 is the nano-nickel oxide that the present invention is prepared at 1000 DEG C.
Specific implementation mode
With reference to embodiment and Figure of description, the present invention is further illustrated.
Embodiment 1：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of aluminum sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano aluminium oxide.
Embodiment 2：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.1mol/L, a concentration of 0.1mol/L of aluminum sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano aluminium oxide.
Embodiment 3：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.01mol/L, a concentration of 0.03mol/L of aluminum sulfate.In stirring condition
The lower mixed sulfate solution by containing polyacrylic acid instills in 50 milliliters of ethyl alcohol, and sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano aluminium oxide.
Embodiment 4：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.01mol/L, a concentration of 0.05mol/L of aluminum sulfate.In stirring condition
The lower mixed sulfate solution by containing polyacrylic acid instills in 50 milliliters of ethyl alcohol, and sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano aluminium oxide.
Embodiment 5：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.57mol/L (saturation), a concentration of 0.05mol/L of aluminum sulfate.It is stirring
The mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol under the conditions of mixing, sediment is washed 1 time with ethyl alcohol, is done
It is calcined at 1000 DEG C after dry, is washed with water, dries after cooling, dispersion nano aluminium oxide can be obtained.
Embodiment 6：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 0.5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of aluminum sulfate.In stirring condition
The lower mixed sulfate solution by containing polyacrylic acid instills in 50 milliliters of ethyl alcohol, and sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano aluminium oxide.
Embodiment 7：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 10%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of aluminum sulfate.In stirring condition
The lower mixed sulfate solution by containing polyacrylic acid instills in 50 milliliters of ethyl alcohol, and sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano aluminium oxide.
Embodiment 8：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 100%, dissolved clarification is added in 0.02mol/L, a concentration of 0.01mol/L of aluminum sulfate.In stirring bar
The mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol under part, sediment is washed 1 time with ethyl alcohol, after dry
It is calcined at 1000 DEG C, is washed with water, dries after cooling, dispersion nano aluminium oxide can be obtained.
Embodiment 11：10 milliliters of titanium sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of titanium sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano-titanium oxide.
Embodiment 12：10 milliliters of ferric sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of ferric sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano-sized iron oxide.
Embodiment 13：10 milliliters of nickel sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, concentration of nickel sulfate 0.1mol/L.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano-nickel oxide.
Embodiment 14：10 milliliters of cobaltous sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, cobalt sulfate concentration 0.1mol/L.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nanometer cobalt oxide.
Embodiment 15：10 milliliters of copper sulphate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, concentration of copper sulfate 0.1mol/L.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano cupric oxide.
Embodiment 16：10 milliliters of magnesium sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, magnesium sulfate concentration 0.1mol/L.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano magnesia.
Embodiment 17：10 milliliters of zirconium sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of zirconium sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano zircite.
Embodiment 18：10 milliliters of cadmium sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of cadmium sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano oxygen cadmium.
Embodiment 19：10 milliliters of STANNOUS SULPHATE CRYSTALLINE and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of STANNOUS SULPHATE CRYSTALLINE.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano tin dioxide.
Embodiment 20：10 milliliters of zinc sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of zinc sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano zine oxide.
Embodiment 21：10 milliliters of indium sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of indium sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano indium oxide.
Embodiment 22：10 milliliters of yttrium sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of yttrium sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano yttrium oxide.
Embodiment 23：10 milliliters of europium sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of europium sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano europium oxide.
Embodiment 24：10 milliliters of cerous sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of cerous sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano-cerium oxide.
Embodiment 25：10 milliliters of lanthanum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of lanthanum sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano lanthanum oxide.
Embodiment 26：10 milliliters of sulfuric acid terbium and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of sulfuric acid terbium.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, can obtain disperseing nano oxidized terbium.
Embodiment 27：10 milliliters of dysprosium sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of dysprosium sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, can obtain disperseing nano oxidized dysprosium.
Embodiment 28：10 milliliters of Dineodymium trisulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of Dineodymium trisulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion Nanometer-sized Neodymium Oxide.
Embodiment 29：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of aluminum sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 ml methanols, sediment is washed 1 time with methanol, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano aluminium oxide.
Embodiment 30：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of aluminum sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of tert-butyl alcohols, sediment is washed 1 time with the tert-butyl alcohol, after dry
It is calcined at 1000 DEG C, is washed with water, dries after cooling, dispersion nano aluminium oxide can be obtained.
Embodiment 31：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of aluminum sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of acetone, sediment is washed 1 time with acetone, it is dry after
1000 DEG C of calcinings, are washed with water after cooling, dry, and can obtain dispersion nano aluminium oxide.
Embodiment 32：10 milliliters of aluminum sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of aluminum sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of dimethylformamides, by sediment dimethylformamide
It washes 1 time, is calcined at 1000 DEG C after dry, be washed with water, dry after cooling, dispersion nano aluminium oxide can be obtained.
Embodiment 33：10 milliliters of ferric sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, a concentration of 0.1mol/L of ferric sulfate.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
Calcined product is carried out secondary clacining, is washed with water, dries after cooling, nanometer can be obtained by 1000 DEG C of calcinings in a reducing atmosphere
Metal iron powder.
Embodiment 34：10 milliliters of nickel sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, concentration of nickel sulfate 0.1mol/L.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
Calcined product is carried out secondary clacining, is washed with water, dries after cooling, nanometer can be obtained by 1000 DEG C of calcinings in a reducing atmosphere
Metal nickel powder
Embodiment 35：10 milliliters of cobaltous sulfate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, cobalt sulfate concentration 0.1mol/L.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
Calcined product is carried out secondary clacining, is washed with water, dries after cooling, nanometer can be obtained by 1000 DEG C of calcinings in a reducing atmosphere
Metal cobalt powder
Embodiment 36：10 milliliters of copper sulphate and potassium sulfate mixed solution are prepared with deionized water, wherein potassium sulfate is a concentration of
The polyacrylic acid of sulfate gross mass 5%, dissolved clarification is added in 0.2mol/L, concentration of copper sulfate 0.1mol/L.Under agitation
Mixed sulfate solution containing polyacrylic acid is instilled in 50 milliliters of ethyl alcohol, sediment is washed 1 time with ethyl alcohol, it is dry after
Calcined product is carried out secondary clacining, is washed with water, dries after cooling, nanometer can be obtained by 1000 DEG C of calcinings in a reducing atmosphere
Copper powder.
Claims (10)
1. a kind of method preparing dispersion nano-metal-oxide, which is characterized in that this approach includes the following steps：
1) sulfate corresponding to metal oxide is configured to mixed aqueous solution with potassium sulfate；
2) polyacrylic acid is added in the mixed aqueous solution of the step 1) configuration；
3) mixed aqueous solution containing polyacrylic acid under agitation, is instilled into organic solvent, obtains sediment；
4) by sediment organic solvent washing 1-2 times, a nanometer sulfate mixture is obtained after dry；
5) the nanometer sulfate mixture is calcined below potassium sulfate fusing point；
6) calcined product of the step 5) is washed with water, dried, obtain nano-metal-oxide.
2. a kind of method preparing dispersion nano-metal-oxide according to claim 1, which is characterized in that the step
1) in, metal oxide is aluminium oxide, titanium oxide, iron oxide, nickel oxide, cobalt oxide, copper oxide, magnesia, zirconium oxide, oxidation
Cadmium, tin oxide, zinc oxide, indium oxide, yttrium oxide, europium oxide, cerium oxide, lanthana, terbium oxide, dysprosia or neodymia.
3. a kind of method preparing dispersion nano-metal-oxide according to claim 1, which is characterized in that the step
1) in, the molar ratio of potassium sulfate and metal sulfate is no less than 1: 1, in the mixed aqueous solution of preparation, potassium sulfate it is a concentration of
0.01mol/L is extremely saturated.
4. a kind of method preparing dispersion nano-metal-oxide according to claim 1,2 or 3, which is characterized in that institute
The addition for stating polyacrylic acid in step 2) is the 0.5%-100% of sulfate gross mass.
5. a kind of method preparing dispersion nano-metal-oxide according to claim 1,2 or 3, which is characterized in that institute
It is methanol, ethyl alcohol, the tert-butyl alcohol, acetone or dimethylformamide to state organic solvent in step 3), organic in the step 4)
Solvent is methanol, ethyl alcohol, the tert-butyl alcohol, acetone or dimethylformamide.
6. a kind of method preparing dispersion Nano metal powder, which is characterized in that this approach includes the following steps：
1) sulfate corresponding to metal is configured to mixed aqueous solution with potassium sulfate；
2) polyacrylic acid is added in the mixed aqueous solution of the step 1) configuration；
3) mixed aqueous solution containing polyacrylic acid under agitation, is instilled into organic solvent, obtains sediment；
4) by sediment organic solvent washing 1-2 times, a nanometer sulfate mixture is obtained after dry；
5) the nanometer sulfate mixture is calcined below potassium sulfate fusing point；
6) calcined product for obtaining step 5) carries out secondary clacining in a reducing atmosphere, is washed with water, dries after cooling, obtains
Nano metal powder.
7. a kind of method preparing dispersion Nano metal powder according to claim 6, which is characterized in that the step 1)
In, metal is iron, nickel, cobalt or copper.
8. a kind of method preparing dispersion Nano metal powder according to claim 6, which is characterized in that the step 1)
In, the molar ratio of potassium sulfate and metal sulfate is no less than 1: 1, in the mixed aqueous solution of preparation, potassium sulfate it is a concentration of
0.01mol/L is extremely saturated.
9. a kind of method preparing dispersion Nano metal powder according to claim 6,7 or 8, which is characterized in that the step
It is rapid 2) in polyacrylic acid addition be sulfate gross mass 0.5%-100%.
10. a kind of method preparing dispersion Nano metal powder according to claim 6,7 or 8, which is characterized in that the step
It is rapid 3) in organic solvent be methanol, ethyl alcohol, the tert-butyl alcohol, acetone or dimethylformamide, the organic solvent in the step 4)
For methanol, ethyl alcohol, the tert-butyl alcohol, acetone or dimethylformamide.
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