CN107486028B - 一种用于废润滑油处理的高滤通膜及其制备方法 - Google Patents
一种用于废润滑油处理的高滤通膜及其制备方法 Download PDFInfo
- Publication number
- CN107486028B CN107486028B CN201710858048.XA CN201710858048A CN107486028B CN 107486028 B CN107486028 B CN 107486028B CN 201710858048 A CN201710858048 A CN 201710858048A CN 107486028 B CN107486028 B CN 107486028B
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- Prior art keywords
- lubricating oil
- membrane
- hollow fiber
- fiber membrane
- polyacrylonitrile hollow
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- 239000012528 membrane Substances 0.000 title claims abstract description 148
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 63
- 238000001914 filtration Methods 0.000 title claims abstract description 40
- 239000002699 waste material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 80
- 239000012510 hollow fiber Substances 0.000 claims abstract description 74
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 50
- 239000002131 composite material Substances 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims description 27
- 239000011521 glass Substances 0.000 claims description 27
- 238000004528 spin coating Methods 0.000 claims description 27
- 239000002002 slurry Substances 0.000 claims description 26
- 238000000576 coating method Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 229910001868 water Inorganic materials 0.000 claims description 21
- 238000002791 soaking Methods 0.000 claims description 19
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 17
- 239000004793 Polystyrene Substances 0.000 claims description 14
- 229920000578 graft copolymer Polymers 0.000 claims description 14
- 229920002223 polystyrene Polymers 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 10
- 239000012670 alkaline solution Substances 0.000 claims description 10
- 150000001412 amines Chemical class 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000010409 thin film Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 9
- 230000007480 spreading Effects 0.000 claims description 9
- 238000003892 spreading Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 150000003512 tertiary amines Chemical class 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- 229910052900 illite Inorganic materials 0.000 claims description 6
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 claims description 6
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 5
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 claims description 5
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent 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
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 4
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 4
- 229920001400 block copolymer Polymers 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229910001919 chlorite Inorganic materials 0.000 claims description 4
- 229910052619 chlorite group Inorganic materials 0.000 claims description 4
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 claims description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims 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 claims description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 3
- MZWXWSVCNSPBLH-UHFFFAOYSA-N 3-(3-aminopropyl-methoxy-methylsilyl)oxypropan-1-amine Chemical compound NCCC[Si](C)(OC)OCCCN MZWXWSVCNSPBLH-UHFFFAOYSA-N 0.000 claims description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 3
- 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 3
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 3
- 229910001570 bauxite Inorganic materials 0.000 claims description 3
- 239000002311 kaolinite-group mineral Substances 0.000 claims description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 3
- 229920000053 polysorbate 80 Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 3
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052902 vermiculite Inorganic materials 0.000 claims description 3
- 239000010455 vermiculite Substances 0.000 claims description 3
- 235000019354 vermiculite Nutrition 0.000 claims description 3
- LVNLBBGBASVLLI-UHFFFAOYSA-N 3-triethoxysilylpropylurea Chemical compound CCO[Si](OCC)(OCC)CCCNC(N)=O LVNLBBGBASVLLI-UHFFFAOYSA-N 0.000 claims description 2
- LVACOMKKELLCHJ-UHFFFAOYSA-N 3-trimethoxysilylpropylurea Chemical compound CO[Si](OC)(OC)CCCNC(N)=O LVACOMKKELLCHJ-UHFFFAOYSA-N 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 2
- NHBRUUFBSBSTHM-UHFFFAOYSA-N n'-[2-(3-trimethoxysilylpropylamino)ethyl]ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCNCCN NHBRUUFBSBSTHM-UHFFFAOYSA-N 0.000 claims description 2
- 239000003030 smectite-group mineral Substances 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 41
- 230000003197 catalytic effect Effects 0.000 abstract description 15
- 239000002346 layers by function Substances 0.000 abstract description 14
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000003921 oil Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000000835 fiber Substances 0.000 abstract description 3
- 238000001728 nano-filtration Methods 0.000 abstract description 3
- 238000012695 Interfacial polymerization Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 description 9
- 239000002585 base Substances 0.000 description 6
- 238000007670 refining Methods 0.000 description 6
- 239000004927 clay Substances 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 4
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 3
- AFBPFSWMIHJQDM-UHFFFAOYSA-N N-methyl-N-phenylamine Natural products CNC1=CC=CC=C1 AFBPFSWMIHJQDM-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 239000002199 base oil Substances 0.000 description 3
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
- 238000005374 membrane filtration Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- CZZZABOKJQXEBO-UHFFFAOYSA-N 2,4-dimethylaniline Chemical compound CC1=CC=C(N)C(C)=C1 CZZZABOKJQXEBO-UHFFFAOYSA-N 0.000 description 2
- VOWZNBNDMFLQGM-UHFFFAOYSA-N 2,5-dimethylaniline Chemical compound CC1=CC=C(C)C(N)=C1 VOWZNBNDMFLQGM-UHFFFAOYSA-N 0.000 description 2
- UFFBMTHBGFGIHF-UHFFFAOYSA-N 2,6-dimethylaniline Chemical compound CC1=CC=CC(C)=C1N UFFBMTHBGFGIHF-UHFFFAOYSA-N 0.000 description 2
- MLPVBIWIRCKMJV-UHFFFAOYSA-N 2-ethylaniline Chemical compound CCC1=CC=CC=C1N MLPVBIWIRCKMJV-UHFFFAOYSA-N 0.000 description 2
- KDSNLYIMUZNERS-UHFFFAOYSA-N 2-methylpropanamine Chemical compound CC(C)CN KDSNLYIMUZNERS-UHFFFAOYSA-N 0.000 description 2
- DOLQYFPDPKPQSS-UHFFFAOYSA-N 3,4-dimethylaniline Chemical compound CC1=CC=C(N)C=C1C DOLQYFPDPKPQSS-UHFFFAOYSA-N 0.000 description 2
- MKARNSWMMBGSHX-UHFFFAOYSA-N 3,5-dimethylaniline Chemical compound CC1=CC(C)=CC(N)=C1 MKARNSWMMBGSHX-UHFFFAOYSA-N 0.000 description 2
- JJYPMNFTHPTTDI-UHFFFAOYSA-N 3-methylaniline Chemical compound CC1=CC=CC(N)=C1 JJYPMNFTHPTTDI-UHFFFAOYSA-N 0.000 description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical group CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 2
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 description 2
- OJGMBLNIHDZDGS-UHFFFAOYSA-N N-Ethylaniline Chemical compound CCNC1=CC=CC=C1 OJGMBLNIHDZDGS-UHFFFAOYSA-N 0.000 description 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 2
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 2
- 239000010408 film Substances 0.000 description 2
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- -1 hexyldiamine Chemical compound 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- RNVCVTLRINQCPJ-UHFFFAOYSA-N o-toluidine Chemical compound CC1=CC=CC=C1N RNVCVTLRINQCPJ-UHFFFAOYSA-N 0.000 description 2
- RZXMPPFPUUCRFN-UHFFFAOYSA-N p-toluidine Chemical compound CC1=CC=C(N)C=C1 RZXMPPFPUUCRFN-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
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- 238000011069 regeneration method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 1
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 1
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- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
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- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 description 1
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- NJBCRXCAPCODGX-UHFFFAOYSA-N 2-methyl-n-(2-methylpropyl)propan-1-amine Chemical compound CC(C)CNCC(C)C NJBCRXCAPCODGX-UHFFFAOYSA-N 0.000 description 1
- ZDZYGYFHTPFREM-UHFFFAOYSA-N 3-[3-aminopropyl(dimethoxy)silyl]oxypropan-1-amine Chemical compound NCCC[Si](OC)(OC)OCCCN ZDZYGYFHTPFREM-UHFFFAOYSA-N 0.000 description 1
- PXGZUMCOTGAVEC-UHFFFAOYSA-N 3-[dimethoxy(penta-1,4-dien-3-yloxy)silyl]propane-1,1,1-triamine Chemical compound C(=C)C(O[Si](OC)(OC)CCC(N)(N)N)C=C PXGZUMCOTGAVEC-UHFFFAOYSA-N 0.000 description 1
- PNPCRKVUWYDDST-UHFFFAOYSA-N 3-chloroaniline Chemical compound NC1=CC=CC(Cl)=C1 PNPCRKVUWYDDST-UHFFFAOYSA-N 0.000 description 1
- WEZAHYDFZNTGKE-UHFFFAOYSA-N 3-ethoxyaniline Chemical compound CCOC1=CC=CC(N)=C1 WEZAHYDFZNTGKE-UHFFFAOYSA-N 0.000 description 1
- JOZZAIIGWFLONA-UHFFFAOYSA-N 3-methylbutan-2-amine Chemical compound CC(C)C(C)N JOZZAIIGWFLONA-UHFFFAOYSA-N 0.000 description 1
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- QSNSCYSYFYORTR-UHFFFAOYSA-N 4-chloroaniline Chemical compound NC1=CC=C(Cl)C=C1 QSNSCYSYFYORTR-UHFFFAOYSA-N 0.000 description 1
- IMPPGHMHELILKG-UHFFFAOYSA-N 4-ethoxyaniline Chemical compound CCOC1=CC=C(N)C=C1 IMPPGHMHELILKG-UHFFFAOYSA-N 0.000 description 1
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- HTJDQJBWANPRPF-UHFFFAOYSA-N Cyclopropylamine Chemical compound NC1CC1 HTJDQJBWANPRPF-UHFFFAOYSA-N 0.000 description 1
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
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- BHRZNVHARXXAHW-UHFFFAOYSA-N sec-butylamine Chemical compound CCC(C)N BHRZNVHARXXAHW-UHFFFAOYSA-N 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
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- 229910052717 sulfur Inorganic materials 0.000 description 1
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- B01D71/06—Organic material
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- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/182—Phosphorus; Compounds thereof with silicon
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- C—CHEMISTRY; METALLURGY
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- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
- C10G31/09—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for by filtration
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
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- C—CHEMISTRY; METALLURGY
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- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
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Abstract
本发明涉及润滑油技术领域,特别是涉及一种用于废润滑油处理的高滤通膜及其制备方法;所述的高滤通膜包括基膜、覆盖在基膜上表面的功能层和覆盖在功能层上的催化层;其中,所述基膜为对聚丙烯腈中空纤维膜;所述功能层为聚丙烯酰胺层;所述催化层为硅铝磷酸催化层;通过对聚丙烯腈表面预处理,得到羧酸化聚丙烯腈基膜,后经界面聚合在改性聚丙烯腈纤维外表面涂覆一层聚丙烯酰胺功能层,能够提高润滑油的通过量,通过向功能层中引入硅铝磷酸纳米颗粒,可以在功能层中形成纳米水通道,能够将废润滑油中的杂质进行降解,不仅减少杂质的含量,能够显著降低油品的粘度,还避免了大尺寸杂质对滤纸造成堵塞,有效提高复合纳滤膜的分离性能。
Description
技术领域
本发明涉及润滑油技术领域,特别是涉及一种用于废润滑油处理的高滤通膜及其制备方法。
背景技术
润滑油是用在各种类型汽车、机械设备上以减少摩擦,保护机械及加工件的液体或半固体润滑剂,主要起润滑、辅助冷却、防锈、清洁、密封和缓冲等作用,只要是应用于两个相对运动的物体之间,而可以减少两物体因接触而产生的磨擦与磨损之功能,即为润滑油。
润滑油从组成上讲由80%-90%的基础油和10%~20%的添加剂组成的,主要化学成分是多种烃类以及少量非烃类的混合物。然而润滑油在使用一段时间后由于物理、化学或人为因素导致了润滑油的性能劣化,生成了如醛、酮、树脂、沥青胶态物质、碳黑及有机酸、盐、水、金属屑等污染杂质,不能再继续使用而成为废润滑油。实际上废润滑油并不废,而用过的润滑油真正变质的只是其中的百分之几,因此如何有效的去除废润滑油中的这些杂质,是废润滑油再生的关键。目前废润滑油的再生工艺主要有蒸馏-酸洗-白土精制,沉降-酸洗-白土蒸馏,沉降-蒸馏-酸洗-钙土精制,蒸馏-乙醇抽提-白土精制,蒸馏-糠醛精制-白土精制,沉降-絮凝-白土精制等。上述工艺都存在基础油利用率低、产生大量固体废弃物及酸渣的缺点。要克服上述工艺的不足,需采用加氢精制技术,在有氢气存在的条件下,经物理和化学等方法脱除其中的水、硫、氮、氯、氧及各种添加剂,得到润滑油基础油和满足国Ⅴ要求的汽柴油调和组分。
目前,随着我国工业的迅速发展,所需的润滑油使用量快速增长,每年换下来的废旧润滑油量也越来越大。如果这些废油如丢弃到环境中去,将造成严重的环境污染。大力开展再生资源回收利用,是提高资源利用效率,保护环境,建设资源节约型社会的重要途径之一。事实上,废润滑油的组成中,除了含有2%-10%的变质物外,其余的90%~98%都是好的成分,是完全可以再利用的。目前,废润滑油的再生技术存在着难于脱水脱杂质、难于分馏、加工单位费用大等一系列的问题。
膜分离技术是利用特殊制造且具有选择透过性的薄膜,在浓度差﹑电位差﹑压力差等外力推动下,对混合物进行分离、提纯和浓缩的新型技术,与传统技术相比该技术具有高效节能无污染等优点。废润滑油中含有的炭黑、胶体粒子、沥青质和部分添加剂消耗后产生的化合物(常为水溶性盐类)均可利用超滤将其除去。由于废润滑油的黏度较大,膜过滤通量较低,且膜分离过程中存在浓差极化和膜污染严重等问题,也显著影响废润滑油膜过滤速度,降低膜使用寿命。因此,选择合适的膜可以提高再生滑油的品质。
发明内容
针对目前膜分离过程中润滑油浓差极化、膜污染严重和废润滑油膜过滤速度慢,膜使用寿命短的问题,本发明的目的是提供一种用于废润滑油处理的高滤通膜及其制备方法。
为解决上述问题,本发明采用以下技术方案:
一种用于废润滑油处理的高滤通膜,包括基膜、覆盖在基膜上表面的功能层和覆盖在功能层上的催化层;
其中,所述基膜为对聚丙烯腈中空纤维膜;所述功能层为聚丙烯酰胺层;所述催化层为硅铝磷酸催化层。
优选的,所述基膜的厚度为0.3~0.5mm。
优选的,所述功能层厚度为1~3μm。
优选的,所述催化层的厚度为200~600nm。
本发明还提供一种用于废润滑油处理的高滤通膜的制备方法,包括以下步骤:
(1)将对聚丙烯腈中空纤维膜在碱性溶液中浸泡15~45min,然后调节溶液pH至3~5.8,向体系中加入接枝马来酸酐嵌段共聚物溶液、表面活性剂、硅烷偶联剂、催化剂和有机溶剂,在50~60℃下反应1~3h,得到羧酸化的聚丙烯腈中空纤维膜;
(2)将步骤(1)的羧酸化的聚丙烯腈中空纤维膜铺于玻璃板上,用水浸湿,然后将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,厚度为1~3μm;
(3)将步骤(2)的复合膜、硅铝酸盐、磷源、辅助铝源、结构导向剂和水在120~180℃的条件下密闭反应3~8h,然后将复合膜清洗至中性,得到用于废润滑油处理的高滤通膜。
优选的,在步骤(1)中,所述表面活性剂选自十二烷基苯磺酸钠、十二烷基磺酸钠、聚乙烯比咯烷酮、吐温-80和司盘-80中的至少一种;
优选的,所述硅烷偶联剂选自氨丙基三乙氧基硅烷、氨丙基三甲氧基硅烷、2-氨乙基氨丙基三甲氧基硅烷、二乙烯三氨基丙基三甲氧基硅烷、氨乙基氨丙基甲基二甲氧基硅烷、氨乙基氨丙基三乙氧基硅烷、脲基丙基三乙氧基硅烷及脲基丙基三甲氧基硅烷中的至少一种。
优选的,所述接枝马来酸酐嵌段共聚物选自聚苯乙烯-聚丁二烯-聚苯乙烯共聚物的马来酸酐接枝共聚物、聚苯乙烯-聚-聚苯乙烯共聚物的马来酸酐接枝共聚物、聚苯乙烯-聚异戊二烯-聚苯乙烯的马来酸酐接枝共聚物中的至少一种。
优选的,所述催化剂选自吡啶和/或叔胺。
优选的,所述有机溶剂选自N,N-二甲基二酰胺、四氢呋喃、二氧六环、氯仿、N-甲基吡咯烷酮中的至少一种。
优选的,在步骤(2)中,所述聚丙烯酰胺浆料的涂覆工艺为:将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,旋涂得到薄膜,旋涂转速控制在1000~3000rpm,旋涂时间控制在30~40s,然后静置30~50s,再将玻璃板移入烘箱中干燥,在60℃干燥20min,将温度降到30℃干燥12~16h。
优选的,在步骤(3)中,所述硅铝酸盐选自高岭石族矿物,蒙脱石族矿物,云母族矿物,叶腊石,伊利石,铵伊利石,蛭石和绿泥石中的至少一种,所述硅铝酸盐的粒径为2~15μm。
优选的,在步骤(3)中,所述磷源是磷酸、亚磷酸、磷酸铝或磷酸三乙酯中的至少一种。
优选的,所述辅助铝源是拟薄水铝石、氢氧化铝、活性氧化铝、氯化铝、硝酸铝、硫酸铝、铝矾土和异丙醇铝中的至少一种。
优选的,在步骤(3)中,所述结构导向剂为有机胺,所述有机胺为一乙胺、二乙胺、三乙胺、乙二胺、一丙胺、二丙胺、三丙胺、异丙胺、二异丙胺、1,2-二甲基丙胺、1,2-丙二胺、2-丙烯胺、环丙胺、正丁胺、二正丁胺、异丁胺、仲丁胺、1,4-丁二胺、叔丁胺、二异丁胺、N-甲基丁胺、己胺、环己胺、2乙基己胺、己二胺、三辛胺、1,10-癸二胺、二硬脂胺、1,5-二甲基己胺、一乙醇胺、二乙醇胺、三乙醇胺、3-丙醇胺、一异丙醇胺、二异丙醇胺、三异丙醇胺、N,N-二甲基乙醇胺、N,N-二乙基乙醇胺、三亚乙基二胺、三亚乙基三胺、六亚甲基四胺、六亚甲基亚胺、三亚乙基二胺、环乙烯亚胺、吗啉、N甲基吗啉、哌嗪、苯胺、二苯胺、联苯胺、邻苯二胺、间苯二胺、对苯二胺、邻甲基苯胺、间甲基苯胺、对甲基苯胺、2,3二甲基苯胺、2,4-二甲基苯胺、2,5-二甲基苯胺、2,6-二甲基苯胺、3,4-二甲基苯胺、3,5-二甲基苯胺、2,4,6-三甲基苯胺、 邻乙基苯胺、N-丁基苯胺、2,6-二乙基苯胺、N-甲酰苯胺、对丁基苯胺、N-乙酰苯胺、3-甲氧基苯胺、邻氯苯胺、间氯苯胺、对氯苯胺、邻乙氧基苯胺、间乙氧基苯胺、对乙氧基苯胺、N-甲基苯胺、N-乙基苯胺、N,N-二乙基苯胺、N,N-二甲基苯胺中的至少一种。
本发明一种用于废润滑油处理的高滤通膜及其制备方法,与现有技术相比,其突出的特点和优异的效果在于:
本发明的高过滤通膜由中空纤维复合纳滤膜组成,通过对聚丙烯腈表面预处理,得到羧酸化聚丙烯腈基膜,后经界面聚合在改性聚丙烯腈纤维外表面涂覆一层聚丙烯酰胺功能层,能够提高润滑油的通过量,从而提高废润滑油的处理效率,通过向功能层中引入硅铝磷酸纳米颗粒,可以在功能层中形成纳米通道,能够将废润滑油中的杂质进行降解,不仅减少杂质的含量,能够显著降低油品的粘度,还避免了大尺寸杂质对滤纸造成堵塞,有效提高复合纳滤膜的分离性能,提高了膜过滤通量。
具体实施方式
以下通过具体实施方式对本发明作进一步的详细说明,但不应将此理解为本发明的范围仅限于以下的实例。在不脱离本发明上述方法思想的情况下,根据本领域普通技术知识和惯用手段做出的各种替换或变更,均应包含在本发明的范围内。
实施例1
一种用于废润滑油处理的高滤通膜的制备方法:
(1)将对聚丙烯腈中空纤维膜在碱性溶液中浸泡30min,然后调节溶液pH至4.5,向体系中加入聚苯乙烯-聚丁二烯-聚苯乙烯共聚物的马来酸酐接枝共聚物、十二烷基苯磺酸钠、氨丙基三乙氧基硅烷、吡啶和N,N-二甲基二酰胺,在55℃下反应2h,得到羧酸化的聚丙烯腈中空纤维膜;
(2)将步骤(1)的羧酸化的聚丙烯腈中空纤维膜铺于玻璃板上,用水浸湿,然后将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,厚度为2μm,
所述聚丙烯酰胺浆料的涂覆工艺为:将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,旋涂得到薄膜,旋涂 转速控制在2000rpm,旋涂时间控制在35s,然后静置40s,再将玻璃板移入烘箱中干燥,在60℃干燥20min,将温度降到30℃干燥14h;
(3)将步骤(2)的复合膜、高岭石族矿物、磷酸、拟薄水铝石、有机胺和水在160℃的条件下密闭反应5h,然后将复合膜清洗至中性,得到用于废润滑油处理的高滤通膜。
由上述制备方法得到的高滤通膜包括对聚丙烯腈中空纤维膜、覆盖在对聚丙烯腈中空纤维膜上表面的聚丙烯酰胺层和覆盖在聚丙烯酰胺层上的硅铝磷酸催化层;
其中,所述的对聚丙烯腈中空纤维膜的厚度为0.4mm;
所述聚丙烯酰胺层厚度为2μm;
所述硅铝磷酸催化层的厚度为400nm。
实施例2
一种用于废润滑油处理的高滤通膜的制备方法:
(1)将对聚丙烯腈中空纤维膜在碱性溶液中浸泡18min,然后调节溶液pH至3.5,向体系中加入聚苯乙烯-聚丁二烯-聚苯乙烯共聚物的马来酸酐接枝共聚物、十二烷基磺酸钠、氨丙基三甲氧基硅烷、吡啶和四氢呋喃,在52℃下反应1.5h,得到羧酸化的聚丙烯腈中空纤维膜;
(2)将步骤(1)的羧酸化的聚丙烯腈中空纤维膜铺于玻璃板上,用水浸湿,然后将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,厚度为2μm,
所述聚丙烯酰胺浆料的涂覆工艺为:将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,旋涂得到薄膜,旋涂 转速控制在1500rpm,旋涂时间控制在32s,然后静置32s,再将玻璃板移入烘箱中干燥,在60℃干燥20min,将温度降到30℃干燥13h;
(3)将步骤(2)的复合膜、叶腊石、亚磷酸、氯化铝、有机胺和水在140℃的条件下密闭反应4h,然后将复合膜清洗至中性,得到用于废润滑油处理的高滤通膜。
由上述制备方法得到的高滤通膜包括对聚丙烯腈中空纤维膜、覆盖在对聚丙烯腈中空纤维膜上表面的聚丙烯酰胺层和覆盖在聚丙烯酰胺层上的硅铝磷酸催化层;
其中,所述的对聚丙烯腈中空纤维膜的厚度为0.4mm;
所述聚丙烯酰胺层厚度为2μm;
所述硅铝磷酸催化层的厚度为300nm。
实施例3
一种用于废润滑油处理的高滤通膜的制备方法:
(1)将对聚丙烯腈中空纤维膜在碱性溶液中浸泡35min,然后调节溶液pH至4.0,向体系中加入聚苯乙烯-聚-聚苯乙烯共聚物的马来酸酐接枝共聚物、十二烷基苯磺酸钠、2-氨乙基氨丙基三甲氧基硅烷、吡啶和二氧六环,在58℃下反应2h,得到羧酸化的聚丙烯腈中空纤维膜;
(2)将步骤(1)的羧酸化的聚丙烯腈中空纤维膜铺于玻璃板上,用水浸湿,然后将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,厚度为3μm,
所述聚丙烯酰胺浆料的涂覆工艺为:将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,旋涂得到薄膜,旋涂 转速控制在1800rpm,旋涂时间控制在36s,然后静置42s,再将玻璃板移入烘箱中干燥,在60℃干燥20min,将温度降到30℃干燥15h;
(3)将步骤(2)的复合膜、伊利石、磷酸铝、硝酸铝、有机胺和水在150℃的条件下密闭反应6h,然后将复合膜清洗至中性,得到用于废润滑油处理的高滤通膜。
由上述制备方法得到的高滤通膜包括对聚丙烯腈中空纤维膜、覆盖在对聚丙烯腈中空纤维膜上表面的聚丙烯酰胺层和覆盖在聚丙烯酰胺层上的硅铝磷酸催化层;
其中,所述的对聚丙烯腈中空纤维膜的厚度为0.5mm;
所述聚丙烯酰胺层厚度为3μm;
所述硅铝磷酸催化层的厚度为300nm。
实施例4
一种用于废润滑油处理的高滤通膜的制备方法:
(1)将对聚丙烯腈中空纤维膜在碱性溶液中浸泡15min,然后调节溶液pH至3,向体系中加入聚苯乙烯-聚-聚苯乙烯共聚物的马来酸酐接枝共聚物、聚乙烯比咯烷酮、二乙烯三氨基丙基三甲氧基硅烷、叔胺和氯仿,在50℃下反应3h,得到羧酸化的聚丙烯腈中空纤维膜;
(2)将步骤(1)的羧酸化的聚丙烯腈中空纤维膜铺于玻璃板上,用水浸湿,然后将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,厚度为3μm,
所述聚丙烯酰胺浆料的涂覆工艺为:将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,旋涂得到薄膜,旋涂 转速控制在3000rpm,旋涂时间控制在40s,然后静置48s,再将玻璃板移入烘箱中干燥,在60℃干燥20min,将温度降到30℃干燥16h;
(3)将步骤(2)的复合膜、铵伊利石、磷酸三乙酯、硫酸铝、有机胺和水在180℃的条件下密闭反应8h,然后将复合膜清洗至中性,得到用于废润滑油处理的高滤通膜。
由上述制备方法得到的高滤通膜包括对聚丙烯腈中空纤维膜、覆盖在对聚丙烯腈中空纤维膜上表面的聚丙烯酰胺层和覆盖在聚丙烯酰胺层上的硅铝磷酸催化层;
其中,所述的对聚丙烯腈中空纤维膜的厚度为0.5mm;
所述聚丙烯酰胺层厚度为3μm;
所述硅铝磷酸催化层的厚度为200nm。
实施例5
一种用于废润滑油处理的高滤通膜的制备方法:
(1)将对聚丙烯腈中空纤维膜在碱性溶液中浸泡45min,然后调节溶液pH至5.8,向体系中加入聚苯乙烯-聚异戊二烯-聚苯乙烯的马来酸酐接枝共聚物、吐温-80、氨乙基氨丙基甲基二甲氧基硅烷、叔胺和N-甲基吡咯烷酮,在50℃下反应3h,得到羧酸化的聚丙烯腈中空纤维膜;
(2)将步骤(1)的羧酸化的聚丙烯腈中空纤维膜铺于玻璃板上,用水浸湿,然后将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,厚度为1μm,
所述聚丙烯酰胺浆料的涂覆工艺为:将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,旋涂得到薄膜,旋涂 转速控制在3000rpm,旋涂时间控制在40s,然后静置50s,再将玻璃板移入烘箱中干燥,在60℃干燥20min,将温度降到30℃干燥16h;
(3)将步骤(2)的复合膜、蛭石、磷酸、铝矾土、有机胺和水在120℃的条件下密闭反应8h,然后将复合膜清洗至中性,得到用于废润滑油处理的高滤通膜。
由上述制备方法得到的高滤通膜包括对聚丙烯腈中空纤维膜、覆盖在对聚丙烯腈中空纤维膜上表面的聚丙烯酰胺层和覆盖在聚丙烯酰胺层上的硅铝磷酸催化层;
其中,所述的对聚丙烯腈中空纤维膜的厚度为0.3mm;
所述聚丙烯酰胺层厚度为1μm;
所述硅铝磷酸催化层的厚度为600nm。
实施例6
一种用于废润滑油处理的高滤通膜的制备方法:
(1)将对聚丙烯腈中空纤维膜在碱性溶液中浸泡40min,然后调节溶液pH至5.0,向体系中加入聚苯乙烯-聚异戊二烯-聚苯乙烯的马来酸酐接枝共聚物、司盘-80、氨乙基氨丙基三乙氧基硅烷、叔胺和N,N-二甲基二酰胺,在59℃下反应3h,得到羧酸化的聚丙烯腈中空纤维膜;
(2)将步骤(1)的羧酸化的聚丙烯腈中空纤维膜铺于玻璃板上,用水浸湿,然后将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,厚度为2.5μm,
所述聚丙烯酰胺浆料的涂覆工艺为:将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,旋涂得到薄膜,旋涂 转速控制在2500rpm,旋涂时间控制在38s,然后静置48s,再将玻璃板移入烘箱中干燥,在60℃干燥20min,将温度降到30℃干燥16h;
(3)将步骤(2)的复合膜、绿泥石、磷酸、异丙醇铝、有机胺和水在170℃的条件下密闭反应7h,然后将复合膜清洗至中性,得到用于废润滑油处理的高滤通膜。
由上述制备方法得到的高滤通膜包括对聚丙烯腈中空纤维膜、覆盖在对聚丙烯腈中空纤维膜上表面的聚丙烯酰胺层和覆盖在聚丙烯酰胺层上的硅铝磷酸催化层;
其中,所述的对聚丙烯腈中空纤维膜的厚度为0.5mm;
所述聚丙烯酰胺层厚度为2.5μm;
所述硅铝磷酸催化层的厚度为500nm。
对比例1
本发明所用基材聚丙烯腈中空纤维膜作为过滤膜,进行对比试验。
对比例2
(1)将对聚丙烯腈中空纤维膜在碱性溶液中浸泡40min,然后调节溶液pH至5.0,向体系中加入聚苯乙烯-聚异戊二烯-聚苯乙烯的马来酸酐接枝共聚物、司盘-80、氨乙基氨丙基三乙氧基硅烷、叔胺和N,N-二甲基二酰胺,在59℃下反应3h,得到羧酸化的聚丙烯腈中空纤维膜;
(2)将步骤(1)的羧酸化的聚丙烯腈中空纤维膜铺于玻璃板上,用水浸湿,然后将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,厚度为2.5μm,
所述聚丙烯酰胺浆料的涂覆工艺为:将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,旋涂得到薄膜,旋涂 转速控制在2500rpm,旋涂时间控制在38s,然后静置48s,再将玻璃板移入烘箱中干燥,在60℃干燥20min,将温度降到30℃干燥16h;得到用于废润滑油处理的高滤通膜。
其中,所述的对聚丙烯腈中空纤维膜的厚度为0.5mm;
所述聚丙烯酰胺层厚度为2.5μm。
对比例3
(1)将对聚丙烯腈中空纤维膜在碱性溶液中浸泡40min,然后调节溶液pH至5.0,向体系中加入聚苯乙烯-聚异戊二烯-聚苯乙烯的马来酸酐接枝共聚物、司盘-80、氨乙基氨丙基三乙氧基硅烷、叔胺和N,N-二甲基二酰胺,在59℃下反应3h,得到羧酸化的聚丙烯腈中空纤维膜;
(2)将步骤(1)的羧酸化的聚丙烯腈中空纤维膜、绿泥石、磷酸、异丙醇铝、有机胺和水在170℃的条件下密闭反应7h,然后将复合膜清洗至中性,得到用于废润滑油处理的高滤通膜。
其中,所述的对聚丙烯腈中空纤维膜的厚度为0.5mm;
所述硅铝磷酸催化层的厚度为500nm。
将实施例1-5得到的高滤通膜与对比例1-3样膜的滤油性能进行分析,针对同一批次废润滑油,通过溶剂稀释至粘度为80cSt,施加压力0.03MPa加压进行过滤测试,具体性能如表1。
表1:
通过上述对过滤膜效能测试,在改性聚丙烯腈纤维外表面涂覆一层聚丙烯酰胺功能层,能够提高润滑油的通过量,防止油脂堵塞,从而提高废润滑油的处理效率;而且通过向功能层中引入硅铝磷酸纳米颗粒,可以在功能层中形成纳米通道,能够将废润滑油中的杂质进行降解,不仅减少杂质的含量,能够显著降低油品的粘度,还避免了大尺寸杂质对滤纸造成堵塞,有效提高复合纳滤膜的分离性能,提高了膜过滤通量。
Claims (8)
1.一种用于废润滑油处理的高滤通膜的制备方法,其特征在于,包括以下步骤:
(1)将对聚丙烯腈中空纤维膜在碱性溶液中浸泡15~45min,然后调节溶液pH至3~5.8,向体系中加入接枝马来酸酐嵌段共聚物溶液、表面活性剂、硅烷偶联剂、催化剂和有机溶剂,在50~60℃下反应1~3h,得到羧酸化的聚丙烯腈中空纤维膜;
(2)将步骤(1)的羧酸化的聚丙烯腈中空纤维膜铺于玻璃板上,用水浸湿,然后将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,厚度为1~3μm;
(3)将步骤(2)的复合膜、硅铝酸盐、磷源、辅助铝源、结构导向剂和水在120~180℃的条件下密闭反应3~8h,然后将复合膜清洗至中性,得到用于废润滑油处理的高滤通膜。
2.根据权利要求1所述的用于废润滑油处理的高滤通膜的制备方法,其特征在于,在步骤(1)中,所述表面活性剂选自十二烷基苯磺酸钠、十二烷基磺酸钠、聚乙烯比咯烷酮、吐温-80和司盘-80中的至少一种;
所述硅烷偶联剂选自氨丙基三乙氧基硅烷、氨丙基三甲氧基硅烷、2-氨乙基氨丙基三甲氧基硅烷、二乙烯三氨基丙基三甲氧基硅烷、氨乙基氨丙基甲基二甲氧基硅烷、氨乙基氨丙基三乙氧基硅烷、脲基丙基三乙氧基硅烷及脲基丙基三甲氧基硅烷中的至少一种。
3.根据权利要求1所述的用于废润滑油处理的高滤通膜的制备方法,其特征在于,所述接枝马来酸酐嵌段共聚物选自聚苯乙烯-聚丁二烯-聚苯乙烯共聚物的马来酸酐接枝共聚物、聚苯乙烯-聚-聚苯乙烯共聚物的马来酸酐接枝共聚物、聚苯乙烯-聚异戊二烯-聚苯乙烯的马来酸酐接枝共聚物中的至少一种;
所述催化剂选自吡啶和/或叔胺。
4.根据权利要求1所述的用于废润滑油处理的高滤通膜的制备方法,其特征在于,所述有机溶剂选自N,N-二甲基二酰胺、四氢呋喃、二氧六环、氯仿、N-甲基吡咯烷酮中的至少一种。
5.根据权利要求1所述的用于废润滑油处理的高滤通膜的制备方法,其特征在于,在步骤(2)中,所述聚丙烯酰胺浆料的涂覆工艺为:将聚丙烯酰胺浆料涂在羧酸化的聚丙烯腈中空纤维膜上,旋涂得到薄膜,旋涂 转速控制在1000~3000rpm,旋涂时间控制在30~40s,然后静置30~50s,再将玻璃板移入烘箱中干燥,在60℃干燥20min,将温度降到30℃干燥12~16h。
6.根据权利要求1所述的用于废润滑油处理的高滤通膜的制备方法,其特征在于,在步骤(3)中,所述硅铝酸盐选自高岭石族矿物、蒙脱石族矿物、云母族矿物、叶腊石、伊利石、铵伊利石、蛭石、绿泥石中的至少一种。
7.根据权利要求1所述的用于废润滑油处理的高滤通膜的制备方法,其特征在于,在步骤(3)中,所述磷源是磷酸、亚磷酸、磷酸铝或磷酸三乙酯中的至少一种;
所述辅助铝源是拟薄水铝石、氢氧化铝、活性氧化铝、氯化铝、硝酸铝、硫酸铝、铝矾土和异丙醇铝中的至少一种。
8.根据权利要求1所述的用于废润滑油处理的高滤通膜的制备方法,其特征在于,在步骤(3)中,所述结构导向剂为有机胺。
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