CN116351396A - 一种气体吸附剂的制备方法及应用 - Google Patents
一种气体吸附剂的制备方法及应用 Download PDFInfo
- Publication number
- CN116351396A CN116351396A CN202310319555.1A CN202310319555A CN116351396A CN 116351396 A CN116351396 A CN 116351396A CN 202310319555 A CN202310319555 A CN 202310319555A CN 116351396 A CN116351396 A CN 116351396A
- Authority
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- China
- Prior art keywords
- source
- sulfate
- sodium
- precursor
- gas adsorbent
- Prior art date
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- Granted
Links
- 239000003463 adsorbent Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title abstract description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 68
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000001301 oxygen Substances 0.000 claims abstract description 36
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 36
- 229910052786 argon Inorganic materials 0.000 claims abstract description 34
- 238000001179 sorption measurement Methods 0.000 claims abstract description 34
- 239000007789 gas Substances 0.000 claims abstract description 33
- 238000000926 separation method Methods 0.000 claims abstract description 23
- 239000002243 precursor Substances 0.000 claims description 63
- 238000010438 heat treatment Methods 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- 238000006243 chemical reaction Methods 0.000 claims description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 42
- 239000008367 deionised water Substances 0.000 claims description 40
- 229910021641 deionized water Inorganic materials 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 39
- 229910052751 metal Inorganic materials 0.000 claims description 36
- 239000002184 metal Substances 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 27
- 229910052710 silicon Inorganic materials 0.000 claims description 27
- 239000010703 silicon Substances 0.000 claims description 27
- 230000004048 modification Effects 0.000 claims description 24
- 238000012986 modification Methods 0.000 claims description 24
- 239000011734 sodium Substances 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 20
- 229910052708 sodium Inorganic materials 0.000 claims description 19
- 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 17
- 235000002639 sodium chloride Nutrition 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- -1 polytetrafluoroethylene Polymers 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 11
- 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 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000005216 hydrothermal crystallization Methods 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 239000010935 stainless steel Substances 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 9
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 229910021485 fumed silica Inorganic materials 0.000 claims description 6
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 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
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 4
- QOYRNHQSZSCVOW-UHFFFAOYSA-N cadmium nitrate tetrahydrate Chemical compound O.O.O.O.[Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QOYRNHQSZSCVOW-UHFFFAOYSA-N 0.000 claims description 4
- MEXSQFDSPVYJOM-UHFFFAOYSA-J cerium(4+);disulfate;tetrahydrate Chemical compound O.O.O.O.[Ce+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O MEXSQFDSPVYJOM-UHFFFAOYSA-J 0.000 claims description 4
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims description 4
- CHPZKNULDCNCBW-UHFFFAOYSA-N gallium nitrate Chemical compound [Ga+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CHPZKNULDCNCBW-UHFFFAOYSA-N 0.000 claims description 4
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims description 4
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 4
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims description 4
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- BGQMOFGZRJUORO-UHFFFAOYSA-M tetrapropylammonium bromide Chemical compound [Br-].CCC[N+](CCC)(CCC)CCC BGQMOFGZRJUORO-UHFFFAOYSA-M 0.000 claims description 4
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- DIMYTQPLZWDZFE-UHFFFAOYSA-L beryllium sulfate tetrahydrate Chemical compound [Be+2].O.O.O.O.[O-]S([O-])(=O)=O DIMYTQPLZWDZFE-UHFFFAOYSA-L 0.000 claims description 3
- MEYVLGVRTYSQHI-UHFFFAOYSA-L cobalt(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Co+2].[O-]S([O-])(=O)=O MEYVLGVRTYSQHI-UHFFFAOYSA-L 0.000 claims description 3
- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 claims description 3
- 229940119177 germanium dioxide Drugs 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 claims description 2
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 claims description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 claims description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 2
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 claims description 2
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 2
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims description 2
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 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
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 claims description 2
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims description 2
- RKGLUDFWIKNKMX-UHFFFAOYSA-L dilithium;sulfate;hydrate Chemical compound [Li+].[Li+].O.[O-]S([O-])(=O)=O RKGLUDFWIKNKMX-UHFFFAOYSA-L 0.000 claims description 2
- 229940044658 gallium nitrate Drugs 0.000 claims description 2
- 229910000373 gallium sulfate Inorganic materials 0.000 claims description 2
- SBDRYJMIQMDXRH-UHFFFAOYSA-N gallium;sulfuric acid Chemical compound [Ga].OS(O)(=O)=O SBDRYJMIQMDXRH-UHFFFAOYSA-N 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 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
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 239000005049 silicon tetrachloride Substances 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- 229910000367 silver sulfate Inorganic materials 0.000 claims description 2
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- VDNSGQQAZRMTCI-UHFFFAOYSA-N sulfanylidenegermanium Chemical compound [Ge]=S VDNSGQQAZRMTCI-UHFFFAOYSA-N 0.000 claims description 2
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- RZLVQBNCHSJZPX-UHFFFAOYSA-L zinc sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Zn+2].[O-]S([O-])(=O)=O RZLVQBNCHSJZPX-UHFFFAOYSA-L 0.000 claims description 2
- RYQXMDPEDBWKBF-UHFFFAOYSA-N C.C(C)O[SiH](OCC)OCC.C(C)O[SiH](OCC)OCC Chemical compound C.C(C)O[SiH](OCC)OCC.C(C)O[SiH](OCC)OCC RYQXMDPEDBWKBF-UHFFFAOYSA-N 0.000 claims 1
- 230000001276 controlling effect Effects 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 150000001768 cations Chemical class 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 125000000962 organic group Chemical group 0.000 description 4
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- NIINUVYELHEORX-UHFFFAOYSA-N triethoxy(triethoxysilylmethyl)silane Chemical compound CCO[Si](OCC)(OCC)C[Si](OCC)(OCC)OCC NIINUVYELHEORX-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本发明属于气体吸附剂制备领域,具体涉及一种用于吸附分离氩气和氧气的吸附剂的制备方法,制备过程主要包括前体的合成和后处理改性等步骤,具有简单易行、重复性好、适合规模放大合成、成本低等优点。本发明制备的吸附剂对氩气的吸附容量显著高于对氧气的吸附容量,即具有高氩气/氧气分离系数,适用于对氩气的吸附、对氩气和氧气混合气体的吸附分离等,拥有吸附分离效率高、稳定性好等优点。
Description
技术领域
本发明属于气体吸附剂制备领域,具体涉及一种用于吸附分离氩气和氧气的吸附剂的制备方法。
背景技术
现代工业、医疗健康及社会生活等领域对高纯氧气的需求日益迫切。例如,医学、金属切割等用氧要求氧浓度大于95%,而军用飞行器使用气体中若氩气含量过高将导致人体中毒。
工业上主要通过吸附分离空气中的氧气(物理法)生产氧气。变压吸附(PressureSwing Adsorption,PSA)过程因具有操作灵活方便、自动化程度高、运行成本低等优势而得到广泛应用。但是目前通过PSA过程制氧浓度最高仅约95%,这主要是因为变压吸附技术使用的吸附剂对氧气和氩气的吸附能力相当,无法实现对氧气和氩气的高效分离。专利US6432170B1、201210288026.1和202010832382.X、文献Microporous and MesoporousMaterials(2008,107,577)、American Institute of Chemical Engineers(2013,59,982)分别公开了一种银交换X沸石、Ag-LiLSX沸石和Ag-ETS-10沸石分子筛的制备方法和对氩气和氧气的吸附分离应用,但上述吸附剂存在的主要问题是对氧气和氩气的分离效率较低,Ar/O2分离系数通常仅为1.2~1.5。
发明内容
针对现有吸附剂对氩气、氧气吸附分离系数低的问题,本发明的目的为提供一种具有高氩气、氧气吸附分离系数的吸附剂,100KPa下Ar/O2分离系数高于1.8,此外此吸附剂还具有制备工艺简单,成本低等优点。
本发明的技术方案为:一种气体吸附剂的制备方法,包括以下步骤:
步骤一、将无机硅源、有机硅源、铝源、钠源、金属源、模板剂、去离子水在室温下搅拌混合均匀制成凝胶,在30~65℃下陈化0.5~24小时制得凝胶,将凝胶转移至聚四氟乙烯内衬不锈钢反应釜中,反应釜密封后固定于具有加热功能且可绕水平轴线进行转动的反应器内,将反应器加热后保温,温度为100~250℃,反应器从加热时刻起开始绕水平轴线以5~25rpm的转动速率转动,设置每小时切换一次转动方向,使反应凝胶进行动态水热晶化,总晶化时间为1~5天,后经抽滤、洗涤、烘干、焙烧得到前体;
步骤二、将步骤一得到的前体进行后处理改性,后处理改性过程包括:前体与去离子水按质量比1:10~100充分混合得到前体溶液并保持搅拌,将金属盐溶液在氮气保护的条件下,在搅拌过程中逐滴缓慢加入到前体溶液中,前体溶液控制温度为30~95℃,搅拌时间为0.5~24小时,前体溶液与金属盐溶液的质量比为1:1~10,然后过滤,将所得固体用去离子水洗涤至pH值为7,然后真空干燥;上述后处理改性过程重复2~5次,制得气体吸附剂。
优选的,步骤一中,无机硅源为气相二氧化硅、四氯化硅、正硅酸乙酯中的一种或多种,有机硅源为二甲基二乙氧基硅烷、甲基三乙氧基硅烷或双(三乙氧基硅基)甲烷中的一种或多种,铝源为硫酸铝、偏铝酸钠、氧化铝中的一种或多种,钠源为氢氧化钠、氯化钠、碳酸钠、硝酸钠、硫酸钠、亚硫酸钠中的一种或多种,金属源为二氧化钛、钛酸四丁酯、三氯化钛、二氧化锗、四氯化锗、硫化锗、七水合硫酸钴、四水合乙酸钴、三氯六氨合钴、硫酸镓、水合硝酸镓、无水氯化镓、六水合硝酸锌、七水合硫酸锌、氧化锌、氯化锌、氧化铍、四水合硫酸铍中的一种或多种,模板剂为四丙基溴化铵、四丙基氢氧化铵、正丁胺、叔丁醇中的一种或多种。
优选的,步骤一中,各反应原料的摩尔比为铝源:无机硅源:有机硅源:金属盐:钠源:模板剂:去离子水=1:(20~100):(5~80):(0.68~5.13):(6.84~51.3):(21.2~38.2):(3800~11350),其中:铝源以Al2O3计,无机硅源、有机硅源均以SiO2计,钠源以Na2O计,金属源以金属M计。
优选的,步骤一中反应器为带有水平转轴的烘箱,且旋转方向可以通过程序设置进行顺时针、反时针两个方向的切换,步骤一中反应釜转动速率为10rpm。
优选的,步骤一中的焙烧在马弗炉中进行,450~600℃通氮气条件下煅烧4~6h,升温过程需要控制升温速率为1~10℃/min。
优选的,步骤二中金属盐为氯化锂、一水合氢氧化锂、一水合硫酸锂、无水溴化锂、草酸锂、无水氯化钙、氧化钙、二水合硫酸钙、氢氧化钙、氢氧化钾、溴化钾、氯化钾、铬酸钾、硝酸钾、硫酸钾、四水合硫酸铈、氧化铈、醋酸铈、四水合硝酸镉、硫酸镉、氯化镉、氧化镉、硝酸银、硫酸银、乙酸银中的一种或几种。
优选的,步骤二中,金属盐溶液中金属离子浓度为0.01~0.5mol/L。
优选的,步骤二中,真空干燥为在真空干燥箱80~100℃下处理12~24h。进一步的,步骤二中,在真空干燥箱80℃下处理12h。
本发明还提供一种气体吸附剂,由以上任一气体吸附剂的制备方法制备得到。
本发明还提供上述气体吸附剂的应用,所述吸附剂应用于混合气体中氩气吸附。
本发明中:所述吸附剂对氩气的吸附容量显著高于对氧气的吸附容量,即具有高氩气/氧气分离系数,适用于对氩气的吸附、对氩气和氧气混合气体的吸附分离等。
本发明中凝胶组成、合成过程、后处理所使用的溶液及处理条件对吸附剂的制备均十分关键:
本发明中吸附剂前体的合成,凝胶中加入的有机硅源是带有小尺寸末端有机基团(甲基或二甲基)或桥连有机基团(亚甲基)的有机硅,金属源是金属阳离子半径大于硅的盐,后处理中使用的金属盐是易于对前体孔道中离子进行交换的盐,合成到吸附剂前体骨架中的小尺寸有机基团、半径大于硅的金属阳离子和孔道中的金属阳离子三者共同对吸附剂材料的孔道尺寸、电场局部微环境、表面性质等进行有效调变,协同作用起到选择性筛分氩气和氧气分子的作用,对提高氩气/氧气吸附分离系数具有至关重要的作用,适用于作为吸附剂应用于变压吸附分离氩气和氧气。
本发明中陈化步骤对吸附剂前体的合成至关重要,有利于制得尺寸较小且均一的吸附剂前体颗粒。顺反切换转动过程对晶化中凝胶的均一性和各反应原料的快速动态平衡以及最终产物的性能稳定性均具有至关重要的作用。顺反切换转动的原理为在前体的晶化周期内阶段性的使反应釜朝着顺、反两个方向切换转动。相比于单一方向的转动,在顺反切换动态水热合成条件下各反应原料更容易实现快速动态平衡,从而使合成凝胶中的有机组分和无机组分进行充分混合,而凝胶各部分组成的均一性有利于有机基团和金属阳离子在前体孔结构中的均匀分布,从而实现对前体孔尺寸的有效调控,进而对最终吸附剂筛分氩气和氧气起到至关重要的作用。
本发明后处理改性所涉及的气体保护与溶液缓慢滴加处理直接影响吸附剂性能,溶液交换温度、时间可有效调控金属阳离子与前体中阳离子的交换比例,制得性能优异的吸附剂材料。
与现有技术相比,本发明的有益效果为:
本发明提供的气体吸附剂的制备过程简单,成本低,易于实现大规模生产,氩气和氧气吸附分离性能优异,稳定性好。
附图说明
图1为实施例1中制得吸附剂的氩气和氧气吸附等温线。
具体实施方式
下面具体实施例对本发明作进一步的详细说明(以下实施例中有机硅源、无机硅源均以SiO2计、金属源以金属M计、钠源以Na2O计、铝源以Al2O3计)。实施例中所用的药品未经特别说明均为市售产品,所用方法未经特别说明均为本领域常规方法。
实施例1
本实施例提供一种气体吸附剂的制备方法,按以下步骤进行:
步骤一、将0.88g气相二氧化硅、0.54g二甲基二乙氧基硅烷、0.25g硫酸铝、1.00g氢氧化钠、0.10g氧化钛、3.15g四丙基氢氧化铵和100ml去离子水在室温下搅拌混合均匀制成凝胶,在50℃低温陈化10h,本实施中各物质的摩尔比为铝源:无机硅源:有机硅源:金属盐:钠源:模板剂:水=1:20:5:1.71:17.11:21.2:7600;得到的凝胶转移至聚四氟乙烯内衬不锈钢反应釜中,反应釜密封后固定于具有加热功能且可绕水平轴线进行转动的反应器内,将反应器加热后保温,温度为150℃,反应器从加热时刻起开始绕水平轴线以10rpm的转动速率转动,设置每小时切换一次转动方向(顺时针、反时针切换),使反应凝胶进行动态水热晶化,总晶化时间为1天,后经抽滤、洗涤、烘干、焙烧得到前体,焙烧为550℃通氮气条件下焙烧6h,升温过程需要控制升温速率为5℃/min;
步骤二、将步骤一得到的前体与去离子水充分混合得到前体溶液并保持搅拌,前体与去离子水的质量比为1:10。在氮气保护的条件下,缓慢逐滴加入硝酸银溶液,进行后处理改性,银离子浓度为0.1mol/L,处理温度为80℃,搅拌时间为0.5小时,前体溶液与硝酸银溶液的质量比为1:1,然后过滤,用去离子水洗涤至pH值为7,然后在80℃真空干燥箱中处理12小时;上述后处理改性过程重复2次,制得吸附剂。
实施例2
本实施例与实施例1不同的是:步骤一中将制成的溶液在50℃下低温陈化24h。其它与实施例1相同。
实施例3
本实施例与实施例1不同的是:步骤一中反应器加热温度为250℃。其它与实施例1相同。
实施例4
本实施例与实施例1不同的是:步骤一中反应器从加热时刻起开始绕水平轴线以20rpm的转动速率转动。其它与实施例1相同。
实施例5
本实施例与实施例1不同的是:步骤一中反应凝胶进行顺反两个方向水热动态晶化合成,总晶化时间为5天。其它与实施例1相同。
实施例6
本实施例与实施例1不同的是:步骤二中银离子浓度为0.5mol/L,前体与离子水的质量比为1:100。其它与实施例1相同。
实施例7
本实施例提供一种气体吸附剂的制备方法,按以下步骤进行:
步骤一、将1.75g气相二氧化硅、1.08g二甲基二乙氧基硅烷、0.25g硫酸铝、1.0g氢氧化钠、0.70g七水合硫酸钴、3.15g四丙基氢氧化铵和100ml去离子水在室温下搅拌混合均匀制成凝胶,在50℃低温陈化10h;本实施方式七中各物质的摩尔比为铝源:无机硅源:有机硅源:金属盐:钠源:模板剂:水=1:40:10:3.41:17.11:21.2:7600;制的凝胶转移至聚四氟乙烯内衬不锈钢反应釜中,反应釜密封后固定于具有加热功能且可绕水平轴线进行转动的反应器内,将反应器加热后保温,温度为150℃,反应器从加热时刻起开始绕水平轴线以10rpm的转动速率转动,设置每小时切换一次转动方向(顺时针、反时针切换),使反应凝胶进行动态水热晶化,总晶化时间为2天,后经抽滤、洗涤、烘干、焙烧得到前体,焙烧为550℃通氮气条件下焙烧6h,升温过程需要控制升温速率为5℃/min;
步骤二、将步骤一得到的前体与去离子水充分混合得到前体溶液并保持搅拌,前体与去离子水的质量比为1:10。在氮气保护的条件下,缓慢逐滴加入氢氧化钾溶液,进行后处理改性,钾离子浓度为0.01mol/L,处理温度为80℃,搅拌时间为0.5小时,前体溶液与氢氧化钾溶液的质量比为1:1,然后过滤,用去离子水洗涤至pH值为7,然后在80℃真空干燥箱中处理12小时;上述后处理改性过程重复2次,制得吸附剂;
实施例8
本实施例与实施例7不同的是:步骤二中处理温度为90℃,搅拌时间为24小时。其它与实施例7相同。
实施例9
本实施例提供一种气体吸附剂的制备方法,按以下步骤进行:
步骤一、将3.50g气相二氧化硅、2.60g甲基三乙氧基硅烷、0.25g硫酸铝、0.50g氢氧化钠、0.22g四水合硫酸铍、3.15g四丙基氢氧化铵和100ml去离子水在室温下搅拌混合均匀制成凝胶,在50℃低温陈化10h;本实施方式九中各物质的摩尔比为铝源:无机硅源:有机硅源:金属盐:钠源:模板剂:水=1:80:20:1.70:8.55:21.2:7600;制的的凝胶转移至聚四氟乙烯内衬不锈钢反应釜中,反应釜密封后固定于具有加热功能且可绕水平轴线进行转动的反应器内,将反应器加热后保温,温度为150℃,反应器从加热时刻起开始绕水平轴线以10rpm的转动速率转动,设置每小时切换一次转动方向(顺时针、反时针切换),使反应凝胶进行动态水热晶化,总晶化时间为1天,后经抽滤、洗涤、烘干、焙烧得到前体,焙烧为550℃通氮气条件下焙烧6h,升温过程需要控制升温速率为5℃/min;
步骤二、将步骤一得到的前体与去离子水充分混合得到前体溶液并保持搅拌,前体与去离子水的质量比为1:10。在氮气保护的条件下,缓慢逐滴加入氯化钙溶液,进行后处理改性,钙离子浓度为0.01mol/L,处理温度为80℃,搅拌时间为2小时,前体溶液与氯化钙溶液的质量比为1:1,然后过滤,用去离子水洗涤至pH值为7,然后在80℃真空干燥箱中处理12小时;上述后处理改性过程重复2次,制得吸附剂。
实施例10
本实施例与实施例9不同的是:步骤二后处理改性过程重复5次,制得吸附剂。其它与实施例9相同。
实施例11
本实施例提供一种气体吸附剂的制备方法,按以下步骤进行:
步骤一、将0.88g气相二氧化硅、0.54g二甲基二乙氧基硅烷、0.25g硫酸铝、1.95g氢氧化钠、0.72g六水合硝酸锌、3.15g四丙基氢氧化铵和100ml去离子水在室温下搅拌混合均匀制成凝胶,在50℃低温陈化10h;实施方式十一中各物质的摩尔比为铝源:无机硅源:有机硅源:金属盐:钠源:模板剂:水=1:20:5:3.31:33.33:7600;制得的凝胶转移至聚四氟乙烯内衬不锈钢反应釜中,反应釜密封后固定于具有加热功能且可绕水平轴线进行转动的反应器内,将反应器加热后保温,温度为150℃,反应器从加热时刻起开始绕水平轴线以10rpm的转动速率转动,设置每小时切换一次转动方向(顺时针、反时针切换),使反应凝胶进行动态水热晶化,总晶化时间为1天,后经抽滤、洗涤、烘干、焙烧得到前体,焙烧为550℃通氮气条件下焙烧6h,升温过程需要控制升温速率为5℃/min;
步骤二、将步骤一得到的前体与去离子水充分混合得到前体溶液并保持搅拌,前体与去离子水的质量比为1:10。在氮气保护的条件下,缓慢逐滴加入氯化锂溶液,进行后处理改性,锂离子浓度为0.01mol/L,处理温度为80℃,搅拌时间为0.5小时,前体溶液与氯化锂溶液的质量比为1:1,然后过滤,用去离子水洗涤至pH值为7,然后在80℃真空干燥箱中处理12小时;上述后处理改性过程重复2次,制得吸附剂。
实施例12
本实施例提供一种气体吸附剂的制备方法,按以下步骤进行:
步骤一、将6.09g正硅酸乙酯、1.08g二甲基二乙氧基硅烷、0.25g硫酸铝、0.75g氢氧化钠、0.14g无水氯化镓、4.13g四丙基溴化铵和100ml去离子水在室温下搅拌混合均匀制成凝胶,在50℃低温陈化10h;实施方式十二中各物质的摩尔比为铝源:无机硅源:有机硅源:金属盐:钠源:模板剂:水=1:40:10:1.09:12.83:21.2:7600;制得的凝胶转移至聚四氟乙烯内衬不锈钢反应釜中,反应釜密封后固定于具有加热功能且可绕水平轴线进行转动的反应器内,将反应器加热后保温,温度为150℃,反应器从加热时刻起开始绕水平轴线以10rpm的转动速率转动,设置每小时切换一次转动方向(顺时针、反时针切换),使反应凝胶进行动态水热晶化,总晶化时间为1天,后经抽滤、洗涤、烘干、焙烧得到前体,焙烧为550℃通氮气条件下焙烧6h,升温过程需要控制升温速率为5℃/min;
步骤二、将步骤一得到的前体与去离子水充分混合得到前体溶液并保持搅拌,前体与去离子水的质量比为1:10。在氮气保护的条件下,缓慢逐滴加入氯化钙溶液,进行后处理改性,钙离子浓度为0.01mol/L,处理温度为80℃,搅拌时间为0.5小时,前体溶液与氯化钙溶液的质量比为1:1,然后过滤,用去离子水洗涤至pH值为7,然后在80℃真空干燥箱中处理12小时;上述后处理改性过程重复3次,制得吸附剂;
实施例13
本实施例提供一种气体吸附剂的制备方法,按以下步骤进行:
步骤一、将3.04g正硅酸乙酯、0.54g二甲基二乙氧基硅烷、0.25g硫酸铝、1.50g氢氧化钠、0.29g三氯化钛、3.15g四丙基氢氧化铵和100ml去离子水在室温下搅拌混合均匀制成凝胶,再50℃低温陈化10h;实施方式十三中各物质的摩尔比为铝源:无机硅源:有机硅源:金属盐:钠源:模板剂:水=1:20:5:2.57:25.66:21.2:7600;制得的凝胶转移至聚四氟乙烯内衬不锈钢反应釜中,反应釜密封后固定于具有加热功能且可绕水平轴线进行转动的反应器内,将反应器加热后保温,温度为150℃,反应器从加热时刻起开始绕水平轴线以10rpm的转动速率转动,设置每小时切换一次转动方向(顺时针、反时针切换),使反应凝胶进行动态水热晶化,总晶化时间为3天,后经抽滤、洗涤、烘干、焙烧得到前体,焙烧为550℃通氮气条件下焙烧6h,升温过程需要控制升温速率为5℃/min;
步骤二、将步骤一得到的前体与去离子水充分混合得到前体溶液并保持搅拌,前体与去离子水的质量比为1:10。在氮气保护的条件下,缓慢逐滴加入四水硝酸镉溶液,进行后处理改性,镉离子浓度为0.2mol/L,处理温度为80℃,搅拌时间为0.5小时,前体溶液与四水硝酸镉溶液的质量比为1:1,然后过滤,用去离子水洗涤至pH值为7,然后在80℃真空干燥箱中处理12小时;上述后处理改性过程重复2次,制得吸附剂;
实施例14
本实施例提供一种气体吸附剂的制备方法,按以下步骤进行:
步骤一、将12.18g正硅酸乙酯、2.17g二甲基二乙氧基硅烷、0.25g硫酸铝、0.75g氢氧化钠、0.19g二氧化锗、3.15g四丙基氢氧化铵和100ml去离子水在室温下搅拌混合均匀制成凝胶,再50℃低温陈化10h;各物质的摩尔比为铝源:无机硅源:有机硅源:金属盐:钠源:模板剂:水=1:80:20:2.49:12.83:21.2:7600;制得的凝胶转移至聚四氟乙烯内衬不锈钢反应釜中,反应釜密封后固定于具有加热功能且可绕水平轴线进行转动的反应器内,将反应器加热后保温,温度为150℃,反应器从加热时刻起开始绕水平轴线以20rpm的转动速率转动,设置每小时切换一次转动方向(顺时针、反时针切换),使反应凝胶进行动态水热晶化,总晶化时间为1天,后经抽滤、洗涤、烘干、焙烧得到前体,焙烧为550℃通氮气条件下焙烧6h,升温过程需要控制升温速率为5℃/min;
步骤二、将步骤一得到的前体与去离子水充分混合得到前体溶液并保持搅拌,前体与去离子水的质量比为1:10。在氮气保护的条件下,缓慢逐滴加入一水合氢氧化锂溶液,进行后处理改性,锂离子浓度为0.01mol/L,处理温度为70℃,搅拌时间为0.5小时,前体溶液与一水合氢氧化锂溶液的质量比为1:1,然后过滤,用去离子水洗涤至pH值为7,然后在80℃真空干燥箱中处理12小时;上述后处理改性过程重复2次,制得吸附剂。
实施例15
本实施例提供一种气体吸附剂的制备方法,按以下步骤进行:
步骤一、将12.18g正硅酸乙酯、2.17g二甲基二乙氧基硅烷、0.25g硫酸铝、3.00g氢氧化钠、0.58g三氯化钛、4.13g四丙基溴化铵和100ml去离子水在室温下搅拌混合均匀制成溶液,再50℃低温陈化10h,实施方式中各物质的摩尔比为铝源:无机硅源:有机硅源:金属盐:钠源:模板剂:水=1:80:20:5.13:51.3:21.2:7600;制得的凝胶转移至聚四氟乙烯内衬不锈钢反应釜中,反应釜密封后固定于具有加热功能且可绕水平轴线进行转动的反应器内,将反应器加热后保温,温度为150℃,反应器从加热时刻起开始绕水平轴线以10rpm的转动速率转动,设置每小时切换一次转动方向(顺时针、反时针切换),使反应凝胶进行动态水热晶化,总晶化时间为1天,后经抽滤、洗涤、烘干、焙烧得到前体,焙烧为550℃通氮气条件下焙烧6h,升温过程需要控制升温速率为5℃/min;
步骤二、将步骤一得到的前体与去离子水充分混合得到前体溶液并保持搅拌,前体与去离子水的质量比为1:10。在氮气保护的条件下,缓慢逐滴加入四水合硫酸铈溶液,进行后处理改性,铈离子浓度为0.1mol/L,处理温度为80℃,搅拌时间为0.5小时,前体溶液与四水合硫酸铈溶液的质量比为1:1,然后过滤,用去离子水洗涤至pH值为7,然后在80℃真空干燥箱中处理12小时;上述后处理改性过程重复2次,制得吸附剂。
性能测试
将实施例1得到的吸附剂进行的氧气、氧气吸附分离过程包括如下步骤:
使用比表面积和孔径分析仪(BET):采用美国Quantachrome公司生产的Autosorb-iQ全自动比表面积分析仪对样品进行氩气吸附测试。测试条件为:测试前对材料进行脱气,以5℃·min-1升温至300℃,并在该温度下脱气4h,并使用氮气进行气体回填。脱气后将样品转移至测试站,在25℃常温条件、0-100KPa下进行氩气、氧气变压吸附测试。测试数据结果如表1所示。
表1实施例1-15所得吸附剂的吸附分离结果(100KPa)
从以上表1可知,本发明制得吸附剂的氩气/氧气吸附分离系数达到1.80~1.86以上,远大于现有技术中的1.2~1.5,整个制备过程简单,成本低,易于实现大规模生产,氩气和氧气吸附分离性能优异,具有较好的应用前景。
图1为实施例1中制得吸附剂的氩气和氧气吸附等温线,从图1可以看出看出本发明吸附剂在25℃时,100KPa下对氩气的吸附容量为8.7265cc/g,对氧气的吸附容量为4.6916cc/g,氩气/氧气吸附分离系数为1.86,氩气和氧气吸附分离性能优异。
Claims (9)
1.一种气体吸附剂的制备方法,其特征在于,包括以下步骤:
步骤一、将无机硅源、有机硅源、铝源、钠源、金属源、模板剂、去离子水在室温下搅拌混合均匀制成凝胶,在30~65 ℃下陈化0.5~24小时制得凝胶,将凝胶转移至聚四氟乙烯内衬不锈钢反应釜中,反应釜密封后固定于具有加热功能且可绕水平轴线进行转动的反应器内,将反应器加热后保温,温度为100~250 ℃,反应器从加热时刻起开始绕水平轴线以5~25rpm的转动速率转动,设置每小时切换一次转动方向,使反应凝胶进行动态水热晶化,总晶化时间为1~5天,后经抽滤、洗涤、烘干、焙烧得到前体;
步骤二、将步骤一得到的前体进行后处理改性,后处理改性过程包括:前体与去离子水按质量比1:10~100充分混合得到前体溶液并保持搅拌,将金属盐溶液在氮气保护的条件下,在搅拌过程中缓慢逐滴加入到前体溶液中,前体溶液控制温度为30~95 ℃,搅拌时间为0.5~24小时,前体溶液与金属盐溶液的质量比为1:1~10,然后过滤,将所得固体用去离子水洗涤至pH值为7,然后真空干燥;上述后处理改性过程重复2~5次,制得气体吸附剂。
2.根据权利要求1所述的气体吸附剂的制备方法,其特征在于,步骤一中,无机硅源为气相二氧化硅、四氯化硅、正硅酸乙酯中的一种或多种,有机硅源为二甲基二乙氧基硅烷、甲基三乙氧基硅烷或双(三乙氧基硅基)甲烷中的一种或多种,铝源为硫酸铝、偏铝酸钠、氧化铝中的一种或多种,钠源为氢氧化钠、氯化钠、碳酸钠、硝酸钠、硫酸钠、亚硫酸钠中的一种或多种,金属源为二氧化钛、钛酸四丁酯、三氯化钛、二氧化锗、四氯化锗、硫化锗、七水合硫酸钴、四水合乙酸钴、三氯六氨合钴、硫酸镓、水合硝酸镓、无水氯化镓、六水合硝酸锌、七水合硫酸锌、氧化锌、氯化锌、氧化铍、四水合硫酸铍中的一种或多种,模板剂为四丙基溴化铵、四丙基氢氧化铵、正丁胺、叔丁醇中的一种或多种。
3.根据权利要求1所述的气体吸附剂的制备方法,其特征在于,步骤一中,各反应原料的摩尔比为铝源:无机硅源:有机硅源:金属源:钠源:模板剂:去离子水=1:(20~100):(5~80):(0.68~5.13):(6.84~51.3):(21.2~38.2):(3800~11350),其中:铝源以Al2O3计,所述无机硅源、有机硅源均以SiO2计,钠源以Na2O计,金属源以金属M计。
4.根据权利要求1所述的气体吸附剂的制备方法,其特征在于,步骤一中,焙烧在马弗炉中进行,450~600 ℃通氮气条件下焙烧4~6 h,升温过程需要控制升温速率为1~10 ℃/min。
5.根据权利要求1所述的气体吸附剂的制备方法,其特征在于,步骤二中,所述金属盐为氯化锂、一水合氢氧化锂、一水合硫酸锂、无水溴化锂、草酸锂、无水氯化钙、氧化钙、二水合硫酸钙、氢氧化钙、氢氧化钾、溴化钾、氯化钾、铬酸钾、硝酸钾、硫酸钾、四水合硫酸铈、氧化铈、醋酸铈、四水合硝酸镉、硫酸镉、氯化镉、氧化镉、硝酸银、硫酸银、乙酸银中的一种或几种。
6.根据权利要求1所述的气体吸附剂的制备方法,其特征在于,步骤二中,金属盐溶液中金属离子浓度为0.01~0.5 mol/L。
7.根据权利要求1所述的气体吸附剂的制备方法,其特征在于,步骤二中,真空干燥为在真空干燥箱80~100 ℃下处理12~24h。
8.一种气体吸附剂,其特征在于,由权利要求1~7中任一气体吸附剂的制备方法制备得到。
9.一种如权利要求8所述的吸附剂的应用,其特征在于,所述吸附剂应用氩气的吸附、对氩气和氧气混合气体的吸附分离。
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