CN103936083A - Nickel magnesium composite oxide and preparation method thereof - Google Patents
Nickel magnesium composite oxide and preparation method thereof Download PDFInfo
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- CN103936083A CN103936083A CN201310023125.1A CN201310023125A CN103936083A CN 103936083 A CN103936083 A CN 103936083A CN 201310023125 A CN201310023125 A CN 201310023125A CN 103936083 A CN103936083 A CN 103936083A
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- nickel
- oxide
- source
- mixed oxide
- magnesia mixed
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title abstract description 11
- ATTFYOXEMHAYAX-UHFFFAOYSA-N magnesium nickel Chemical compound [Mg].[Ni] ATTFYOXEMHAYAX-UHFFFAOYSA-N 0.000 title abstract 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 60
- 239000002245 particle Substances 0.000 claims abstract description 13
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 8
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 7
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 45
- 239000003795 chemical substances by application Substances 0.000 claims description 22
- 229910052759 nickel Inorganic materials 0.000 claims description 22
- 239000002243 precursor Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 14
- 239000011777 magnesium Substances 0.000 claims description 14
- 229910052749 magnesium Inorganic materials 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 10
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- -1 polyethylene Polymers 0.000 claims description 8
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229920001400 block copolymer Polymers 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 239000011572 manganese Substances 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 235000015320 potassium carbonate Nutrition 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 230000029087 digestion Effects 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 235000011147 magnesium chloride Nutrition 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- NIAZXXPEOWDLOF-UHFFFAOYSA-N S(O)(O)(=O)=O.[Ni]=O Chemical compound S(O)(O)(=O)=O.[Ni]=O NIAZXXPEOWDLOF-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 229960004424 carbon dioxide Drugs 0.000 claims description 2
- 229910002090 carbon oxide Inorganic materials 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 2
- 229960004643 cupric oxide Drugs 0.000 claims description 2
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 2
- 230000036571 hydration Effects 0.000 claims description 2
- 238000006703 hydration reaction Methods 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 2
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 2
- 239000011654 magnesium acetate Substances 0.000 claims description 2
- 235000011285 magnesium acetate Nutrition 0.000 claims description 2
- 229940069446 magnesium acetate Drugs 0.000 claims description 2
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 claims description 2
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 2
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- ABEWDFYANWOMJE-UHFFFAOYSA-N oxalic acid;potassium Chemical compound [K].OC(=O)C(O)=O ABEWDFYANWOMJE-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 2
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims description 2
- 229940039790 sodium oxalate Drugs 0.000 claims description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 2
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000005554 pickling Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical group [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000011859 microparticle Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 2
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical group [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical group [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical group [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000005815 base catalysis Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical group [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000005616 pyroelectricity Effects 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 238000006057 reforming reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- Catalysts (AREA)
Abstract
The invention relates to a nickel magnesium composite oxide and a preparation method thereof, mainly solving problems of the low specific surface area, less pore content and nonuniform microcosmic particles of nickel magnesium composite oxides in the prior art. According to a technical scheme, the nickel magnesium composite oxide comprises a) 0.1-30 parts by weight of nickel oxide and b) 100 parts by weight of magnesium oxide, wherein the BET specific surface area of the nickel magnesium composite oxide is larger than 25 m<2>/g, the pore content is higher than 0.12 cm<3>/g, and the microcosmic particle size is between 0.5 [mu]m and 5.0 [mu]m. By adoption of the technical scheme, the problems are solved well. The preparation method thereof can be used for industrial production of the nickel magnesium composite oxide.
Description
Technical field
The present invention relates to a kind of nickel-magnesia mixed oxide and preparation method thereof.
Background technology
Composite oxide of metal, the oxide compound especially with perovskite typed, spinel type or green stone type crystal structure, there is good optics, electricity, magnetic performance, important laserable material, pyroelectricity material, piezoelectric and strong magnetic material, in traditional industry and modern high technology, all there is important purposes, apply very extensive.Wherein, nickel-magnesia mixed oxide because its preparation is simple, excellent property, environmental protection, the advantage such as cheap, can be used as sensor, catalyzer and sorbent material etc.In addition, in gas chemical industry's industry, via methane reforming reaction preparing synthetic gas, then by the process of synthetic gas synthesis of organic chemical product as an important channel of methyl hydride catalyzed conversion and be subject to extensive concern.Loading type nickel-based reforming catalyst has the activity and selectivity suitable with loaded noble metal catalyst, and price is more cheap again, thereby having good application prospect, many investigators have carried out a large amount of research on various carriers, auxiliary agent and preparation condition etc. to the impact of catalyst performance.Existing research points out, MgO is a kind of good base catalysis agent carrier, and the nickel-magnesia mixed oxide that the NiO/ MgO catalyzer of nickel-loaded or single stage method obtain has higher reformation catalytic activity and stability.But still there is shortcomings in above-mentioned nickel-magnesia mixed oxide, low such as specific surface area, voids content is few and microscopic particles is inhomogeneous etc., these drawbacks limit their further application.
For example, in the Chinese patent that is CN95111008.X at application number, through preparing porous oxidation magnesium carrier, preparation steeping fluid, with steeping fluid, flood above-mentioned carrier, in the prepared metal composite of the complex steps such as dry and roasting, nickel enters the surface of magnesium oxide skeleton, but the method for this dipping can not guarantee all nickel and all form sosoloid with magnesium oxide skeleton, and magnesium oxide microscopic particles size is also inhomogeneous, from all having distribution to millimeter rank below 70 microns, therefore this composite oxides anti-caking power at high temperature greatly reduces, work-ing life in catalytic applications is corresponding shortening also.
Chinese patent CN102133529 discloses a kind of method that method of utilizing alkali-titration is prepared Ni-based steam reforming catalyzer, utilize soluble magnesium nitrate, aluminum nitrate to be precipitated thing, after suction filtration, washing, dry and roasting, obtain the carrier of composite oxides, then utilize a certain amount of nickel of pickling process load and obtain finished catalyst after the steps such as dry and roasting again.But the porosity via the method gained catalyzer is lower, also cannot guarantee the homogeneity of microscopic particles.Moreover, in above-described these patents, all used the pickling process of complex steps, so not only improved preparation cost, and made preparation technology more complicated.
Summary of the invention
One of technical problem to be solved by this invention is the problem that nickel-magnesia mixed oxide specific surface area is low, voids content is few and microscopic particles is inhomogeneous existing in prior art, and a kind of new nickel-magnesia mixed oxide is provided.These composite oxides have that specific surface area is high, voids content is high and the uniform feature of microscopic particles.Two of technical problem to be solved by this invention is to provide a kind of preparation method of the nickel-magnesia mixed oxide corresponding with one of technical solution problem.
For one of solving the problems of the technologies described above, the technical solution adopted in the present invention is as follows: a kind of nickel-magnesia mixed oxide, in parts by weight, comprises following component: a) nickel oxide of 0.1 ~ 30 part; B) magnesium oxide of 100 parts; Wherein, described nickel-magnesia mixed oxide BET specific surface area is greater than 25 meters
2/ gram, pore space is greater than 0.12 centimetre
3/ gram, microscopic particles size is between 0.5 ~ 5.0 micron.
Preferably, in parts by weight, in described nickel-magnesia mixed oxide, the content of nickel oxide is 0.5 ~ 20 part.
Preferably, described nickel-magnesia mixed oxide BET specific surface area is more than or equal to 50 meters
2/ gram.
More preferably, described nickel-magnesia mixed oxide BET specific surface area is 50 ~ 150 meters
2/ gram.
Described in described nickel-magnesia mixed oxide BET specific surface area, nickel-magnesia mixed oxide pore space is more than or equal to 0.4 centimetre
3/ gram.
More preferably, described nickel-magnesia mixed oxide pore space is 0.4 ~ 0.7 centimetre
3/ gram.
Preferably, described nickel-magnesia mixed oxide microscopic particles size is between 0.8 ~ 4.0 micron.
Preferably, in parts by weight, in described nickel-magnesia mixed oxide, also comprise 0.1 ~ 10 part at least one in ferric oxide, cobalt oxide, aluminum oxide, cupric oxide, titanium oxide, manganese oxide, sodium oxide, potassium oxide or calcium oxide that be selected from.
For solve the problems of the technologies described above two, the technical solution adopted in the present invention is as follows: a kind of preparation method of nickel-magnesia mixed oxide, comprises the following steps:
A) nickel source, magnesium source, precipitation agent, dispersion agent and water are formed to mixture, the pH value of adjusting mixture is 7～12, under 5 ~ 90 ℃ of conditions of temperature, stirs 5 ~ 40 hours, obtains precursor A; Wherein, in precursor A, the weight ratio of each material is nickel source: magnesium source: precipitation agent: dispersion agent: water=(0.001～0.3): 1:(0.5～5): (0.05～5): (2～20);
B) precursor A, through burin-in process, obtains precursor B;
C) precursor B, through washing, dry, calcining, obtains described nickel-magnesia mixed oxide;
Wherein, described nickel source is selected from least one in nickelous nitrate, nickelous chloride, single nickel salt, nickel acetate, nickelous bromide, sulfuric acid oxygen nickel, six hydration nickel, hexamine nickel or nickle carbonoxide; Magnesium source is selected from least one in magnesium nitrate, magnesium chloride, magnesium sulfate, magnesium acetate, magnesium fluoride or bischofite; Precipitation agent is selected from least one in sodium carbonate, salt of wormwood, sodium bicarbonate, saleratus, carbonic acid, sodium oxalate, oxalic acid or oxalic acid potassium; Dispersion agent is selected from least one in succinate sodium 2-ethylhexyl, cetyl trimethylammonium bromide, polyethylene oxide-propylene oxide block copolymer, polyoxyethylene glycol or polyvinyl alcohol.
Preferably, nickel source is selected from least one in nickelous nitrate, nickelous chloride or single nickel salt; Magnesium source is selected from least one in magnesium nitrate, magnesium chloride or magnesium sulfate; Dispersion agent is selected from least one in succinate sodium 2-ethylhexyl, cetyl trimethylammonium bromide, polyethylene oxide-propylene oxide block copolymer or polyoxyethylene glycol.
Preferably, in step a) precursor A, the weight ratio of each material is nickel source: magnesium source: precipitation agent: dispersion agent: water=(0.005～0.2): 1:(0.3～2): (0.2～3): (3～10), the pH value of adjusting mixture is 8～10, and temperature is 30 ~ 60 ℃.
Preferably, step b) aging temperature is 100 ~ 200 ℃, and aging pressure is 0.1 ~ 5MPa, and digestion time is 4 ~ 40 hours.
More preferably, step b) aging temperature is 120 ~ 160 ℃, and aging pressure is 0.2 ~ 3MPa, and digestion time is 8 ~ 20 hours.
Preferably, step c) drying temperature is 60～150 ℃, and be 1～10 hour time of drying, and calcining temperature is 300～1200 ℃, and calcination time is 3～10 hours.
More preferably, step c) drying temperature is 80～120 ℃, and be 2～8 hours time of drying, and calcining temperature is 500～1000 ℃, and calcination time is 5～10 hours.
Preferably, also comprise at least one being selected from source of iron, cobalt source, aluminium source, Tong Yuan, titanium source, manganese source, sodium source, Huo Gai source, potassium source described in step a) in mixture, the weight ratio in its consumption and magnesium source is (0.001 ~ 0.1): 1.
Preferably, described source of iron is selected from iron nitrate; Described cobalt source is selected from Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES; Described aluminium source is selected from aluminum nitrate; Described copper source is selected from copper sulfate; Described titanium source is selected from Titanium Nitrate; Described manganese source is selected from manganous nitrate; Described sodium source is selected from sodium-chlor; Described potassium source is selected from Repone K; Described calcium source is selected from nitrocalcite.
Preferably, in step a), adding alkali take to adjust the pH value of mixture is 7～12, and alkali is selected from least one in sodium hydroxide, potassium hydroxide, ammoniacal liquor, quadrol, triethylamine or fatty ammonium hydroxide.
More preferably, alkali is selected from least one in sodium hydroxide, potassium hydroxide or ammoniacal liquor.
Preferably, water and alcohol wash respectively for step c) precursor B washing; Wherein, the weight ratio of water and precursor B is (1 ~ 200): 1, and the weight ratio of alcohol and precursor B is (0.5～15): 1.
More preferably, the weight ratio of water and precursor B is (10 ~ 50): 1, and the weight ratio of alcohol and precursor B is (0.5～5): 1.
In the present invention, due to nickel oxide and magnesian presoma are added in preparation system simultaneously, guaranteed that nickel oxide can form homogeneous phase composite oxides with magnesium oxide; And due to the existence of dispersion agent, can guarantee that in presoma, microparticle can not occur to reunite and size homogeneous, and can be by regulating the add-on of dispersion agent to obtain the nickel-magnesia mixed oxide with different specific surface areas and granularity; By changing calcining temperature and time, also can regulate the porosity of product.In addition, in preparation process, the presoma of nickel and magnesium is that original position adds simultaneously, has therefore avoided the back loading process of complex steps.These above measures, nickel-magnesia mixed oxide microparticle size heterogeneity, specific surface area have been solved in traditional preparation method and porosity is low and the difficult problem such as complicated process of preparation simultaneously, obtain efficient, stable nickel-magnesia mixed oxide, obtained good technique effect.
Below by embodiment, the present invention is further elaborated.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of gained nickel-magnesia mixed oxide in [embodiment 3].
Fig. 2 is the transmission electron microscope photo of gained nickel-magnesia mixed oxide in [comparative example].
In Fig. 1, the particle size homogeneous of gained nickel-magnesia mixed oxide, is distributed between 0.5 ~ 5.0 micron.
In Fig. 2, the particle size relative different of gained nickel-magnesia mixed oxide is larger, and macrobead size surpasses 14 microns, and short grained size only has 0.5 micron.
Embodiment
[embodiment 1]
Under 40 ℃ of constant temperature, by 0.5 gram of nickelous nitrate, 15.1 gram magnesium nitrate, 14.5 gram salt of wormwood, 7.4 grams of polyoxyethylene glycol are mixed in 75 grams of water, and stir, finally add 0.1 gram of sodium hydroxide, regulate pH=13 ~ 14, mixing solutions is stirred 20 hours at 50 ℃ of constant temperature, then product is carried out to burin-in process, treatment temp is 150 ℃, time is 15 hours, pressure is 0.3MPa, the cooling rear water respectively of product and alcohol wash, then solid product is dried to 6 hours at 100 ℃, finally in air atmosphere 500 ℃ calcining 10 hours, obtain nickel-magnesia mixed oxide of the present invention.
[embodiment 2～6]
By [embodiment 1] described synthesis step, only change nickel source add-on, can synthesize and obtain nickel content and be respectively 0.1%, 0.5%, 1%, 5%, 15% nickel-magnesia mixed oxide.Nickel-magnesia mixed oxide formula, preparation condition and composition constitutional features are in Table 1 ~ table 4.
[embodiment 7～15]
By [embodiment 1] described synthesis step, (wherein succinate sodium 2-ethylhexyl, sodium hydroxide, potassium hydroxide, ammoniacal liquor, TPAOH, tetraethyl ammonium hydroxide, cetyl trimethylammonium bromide and polyethylene oxide-propylene oxide block copolymer are respectively referred to as AOT, NaOH, KOH, NH to change nickel source, magnesium source, precipitation agent, dispersion agent and alkali
3h
2o, TPAOH TEAOH, CTAB, P123 and F127) kind and quality, regulate preparation condition, all can synthesize and obtain nickel-magnesia mixed oxide of the present invention.Nickel-magnesia mixed oxide formula, preparation condition and structure composition characteristic are in Table 1 ~ table 4.
[embodiment 16～24]
By [embodiment 1] described synthesis step, add source of iron, cobalt source, aluminium source, Tong Yuan, titanium source, manganese source, sodium source, Huo Gai source, potassium source presoma, all can synthesize and obtain nickel-magnesia mixed oxide of the present invention, nickel-magnesia mixed oxide formula and structure composition characteristic are in Table 5.
[comparative example]
Utilize pickling process to prepare nickel-magnesia mixed oxide.Under 40 ℃ of constant temperature, 0.8 gram of nickelous nitrate and 3.5 grams of salt of wormwood mixing are added in 6 grams of water, after dissolution of solid, add 16 grams of magnesium oxide to stir, by at 40 ℃ of mixture constant temperature, stir 10 hours, water is slowly volatilized, then by product at 100 ℃ dry 6 hours, finally in air atmosphere 500 ℃ calcining 5 hours, obtain nickel-magnesia mixed oxide prepared by pickling process.Gained nickel-magnesia mixed oxide structure composition characteristic is in Table 5.
Table 1
Table 2
Table 3
| Embodiment | Water and material ratio | Alcohol and material ratio | Drying temperature (℃) | Time of drying (hour) | Calcining temperature (℃) |
| 1 | 10 | 5.0 | 100 | 6 | 500 |
| 2 | 10 | 5.0 | 100 | 6 | 500 |
| 3 | 10 | 0.5 | 100 | 6 | 500 |
| 4 | 10 | 1.0 | 100 | 6 | 300 |
| 5 | 10 | 1.5 | 60 | 1 | 400 |
| 6 | 15 | 2.0 | 70 | 2 | 500 |
| 7 | 1 | 3.0 | 80 | 3 | 600 |
| 8 | 5 | 4.0 | 90 | 4 | 700 |
| 9 | 20 | 5.0 | 100 | 5 | 800 |
| 10 | 40 | 2.0 | 110 | 6 | 900 |
| 11 | 60 | 2.0 | 120 | 7 | 1000 |
| 12 | 100 | 2.0 | 130 | 8 | 1100 |
| 13 | 120 | 2.0 | 140 | 9 | 1200 |
| 14 | 150 | 2.0 | 150 | 10 | 600 |
| 15 | 20 | 2.0 | 90 | 6 | 600 |
Table 4
Table 5
Claims (10)
1. a nickel-magnesia mixed oxide, in parts by weight, comprises following component: a) nickel oxide of 0.1 ~ 30 part; B) magnesium oxide of 100 parts; Wherein, described nickel-magnesia mixed oxide BET specific surface area is greater than 25 meters
2/ gram, pore space is greater than 0.12 centimetre
3/ gram, microscopic particles size is between 0.5 ~ 5.0 micron.
2. nickel-magnesia mixed oxide according to claim 1, is characterized in that in parts by weight, and the content of nickel oxide is 0.5 ~ 20 part.
3. nickel-magnesia mixed oxide according to claim 1, is characterized in that described nickel-magnesia mixed oxide BET specific surface area is more than or equal to 50 meters
2/ gram, pore space is more than or equal to 0.4 centimetre
3/ gram.
4. nickel-magnesia mixed oxide according to claim 3, is characterized in that described nickel-magnesia mixed oxide BET specific surface area is 50 ~ 150 meters
2/ gram, pore space is 0.4 ~ 0.7 centimetre
3/ gram.
5. nickel-magnesia mixed oxide according to claim 1, is characterized in that microscopic particles size is between 0.8 ~ 4.0 micron.
6. nickel-magnesia mixed oxide according to claim 1, it is characterized in that in parts by weight, in described nickel-magnesia mixed oxide, also comprise 0.1 ~ 10 part at least one in ferric oxide, cobalt oxide, aluminum oxide, cupric oxide, titanium oxide, manganese oxide, sodium oxide, potassium oxide or calcium oxide that be selected from.
7. the preparation method of nickel-magnesia mixed oxide claimed in claim 1, comprises the following steps:
A) nickel source, magnesium source, precipitation agent, dispersion agent and water are formed to mixture, the pH value of adjusting mixture is 7～12, under 5 ~ 90 ℃ of conditions of temperature, stirs 5 ~ 40 hours, obtains precursor A; Wherein, in precursor A, the weight ratio of each material is nickel source: magnesium source: precipitation agent: dispersion agent: water=(0.001～0.3): 1:(0.5～5): (0.05～5): (2～20);
B) precursor A, through burin-in process, obtains precursor B;
C) precursor B, through washing, dry, calcining, obtains described nickel-magnesia mixed oxide;
Wherein, described nickel source is selected from least one in nickelous nitrate, nickelous chloride, single nickel salt, nickel acetate, nickelous bromide, sulfuric acid oxygen nickel, six hydration nickel, hexamine nickel or nickle carbonoxide; Magnesium source is selected from least one in magnesium nitrate, magnesium chloride, magnesium sulfate, magnesium acetate, magnesium fluoride or bischofite; Precipitation agent is selected from least one in sodium carbonate, salt of wormwood, sodium bicarbonate, saleratus, carbonic acid, sodium oxalate, oxalic acid or oxalic acid potassium; Dispersion agent is selected from least one in succinate sodium 2-ethylhexyl, cetyl trimethylammonium bromide, polyethylene oxide-propylene oxide block copolymer, polyoxyethylene glycol or polyvinyl alcohol.
8. the preparation method of nickel-magnesia mixed oxide according to claim 7, the weight ratio that it is characterized in that each material in step a) precursor A is nickel source: magnesium source: precipitation agent: dispersion agent: water=(0.005～0.2): 1:(0.3～2): (0.2～3): (3～10), the pH value of adjusting mixture is 8～10, and temperature is 30 ~ 60 ℃.
9. the preparation method of nickel-magnesia mixed oxide according to claim 7, is characterized in that step b) aging temperature is 100 ~ 200 ℃, and aging pressure is 0.1 ~ 5MPa, and digestion time is 4 ~ 40 hours; Step c) drying temperature is 60～150 ℃, and be 1～10 hour time of drying, and calcining temperature is 300～1200 ℃, and calcination time is 3～10 hours.
10. the preparation method of nickel-magnesia mixed oxide according to claim 7, it is characterized in that in mixture, also comprising at least one being selected from source of iron, cobalt source, aluminium source, Tong Yuan, titanium source, manganese source, sodium source, Huo Gai source, potassium source described in step a), the weight ratio in its consumption and magnesium source is (0.001 ~ 0.1): 1.
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| CN105293591A (en) * | 2015-11-10 | 2016-02-03 | 沈阳化工大学 | Method for preparing magnesium-nickel metal compound oxide with active magnesium oxide as raw material |
| CN105858691A (en) * | 2016-05-18 | 2016-08-17 | 四川大学 | Method for preparing flower-like magnesium oxide microsphere according to precipitation method |
| CN106732608A (en) * | 2016-11-23 | 2017-05-31 | 太原理工大学 | A kind of preparation method of nickeliferous mesoporous catalyst |
| CN107224977A (en) * | 2016-03-25 | 2017-10-03 | 中国石化扬子石油化工有限公司 | A kind of hydrogenation catalyst and preparation method thereof, application |
| CN110465281A (en) * | 2018-07-10 | 2019-11-19 | 吉林大学 | A kind of nickel magnesium sosoloid method for preparing catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105293591A (en) * | 2015-11-10 | 2016-02-03 | 沈阳化工大学 | Method for preparing magnesium-nickel metal compound oxide with active magnesium oxide as raw material |
| CN107224977A (en) * | 2016-03-25 | 2017-10-03 | 中国石化扬子石油化工有限公司 | A kind of hydrogenation catalyst and preparation method thereof, application |
| CN105858691A (en) * | 2016-05-18 | 2016-08-17 | 四川大学 | Method for preparing flower-like magnesium oxide microsphere according to precipitation method |
| CN106732608A (en) * | 2016-11-23 | 2017-05-31 | 太原理工大学 | A kind of preparation method of nickeliferous mesoporous catalyst |
| CN110465281A (en) * | 2018-07-10 | 2019-11-19 | 吉林大学 | A kind of nickel magnesium sosoloid method for preparing catalyst |
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