CN116813101A - Preparation method of fiber composite magnetic particles and application of fiber composite magnetic particles as biological carrier - Google Patents
Preparation method of fiber composite magnetic particles and application of fiber composite magnetic particles as biological carrier Download PDFInfo
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- CN116813101A CN116813101A CN202311043170.3A CN202311043170A CN116813101A CN 116813101 A CN116813101 A CN 116813101A CN 202311043170 A CN202311043170 A CN 202311043170A CN 116813101 A CN116813101 A CN 116813101A
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- magnetic particles
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- composite magnetic
- stirring
- activated sludge
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- 239000006249 magnetic particle Substances 0.000 title claims abstract description 168
- 239000000835 fiber Substances 0.000 title claims abstract description 167
- 239000002131 composite material Substances 0.000 title claims abstract description 141
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 98
- 238000003756 stirring Methods 0.000 claims abstract description 59
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 230000007062 hydrolysis Effects 0.000 claims abstract description 24
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 24
- 238000001914 filtration Methods 0.000 claims abstract description 23
- 238000001291 vacuum drying Methods 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 19
- 239000000178 monomer Substances 0.000 claims abstract description 16
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003999 initiator Substances 0.000 claims abstract description 12
- 230000032683 aging Effects 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 11
- 239000004593 Epoxy Substances 0.000 claims abstract description 8
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000003607 modifier Substances 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 4
- 239000010802 sludge Substances 0.000 claims description 90
- 239000010865 sewage Substances 0.000 claims description 78
- 239000012141 concentrate Substances 0.000 claims description 42
- 238000012986 modification Methods 0.000 claims description 32
- 230000004048 modification Effects 0.000 claims description 32
- 238000004062 sedimentation Methods 0.000 claims description 30
- 238000012163 sequencing technique Methods 0.000 claims description 30
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims description 26
- 230000003301 hydrolyzing effect Effects 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 21
- 238000005273 aeration Methods 0.000 claims description 20
- 238000005070 sampling Methods 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 16
- 239000006228 supernatant Substances 0.000 claims description 14
- 229910021645 metal ion Inorganic materials 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 claims description 11
- 230000000694 effects Effects 0.000 claims description 10
- 230000036284 oxygen consumption Effects 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 8
- 230000009920 chelation Effects 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 239000012266 salt solution Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-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
- 239000001632 sodium acetate Substances 0.000 claims description 4
- 235000017281 sodium acetate Nutrition 0.000 claims description 4
- 239000008399 tap water Substances 0.000 claims description 4
- 235000020679 tap water Nutrition 0.000 claims description 4
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 2
- 229960003280 cupric chloride Drugs 0.000 claims description 2
- 229940032296 ferric chloride Drugs 0.000 claims description 2
- 229940032950 ferric sulfate Drugs 0.000 claims description 2
- 229960002089 ferrous chloride Drugs 0.000 claims description 2
- 229960001781 ferrous sulfate Drugs 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- 229940099596 manganese sulfate Drugs 0.000 claims description 2
- 239000011702 manganese sulphate Substances 0.000 claims description 2
- 235000007079 manganese sulphate Nutrition 0.000 claims description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229940053662 nickel sulfate Drugs 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 2
- 235000011009 potassium phosphates Nutrition 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000945 filler Substances 0.000 abstract description 5
- 239000000969 carrier Substances 0.000 abstract description 4
- 239000002923 metal particle Substances 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 description 19
- 231100000719 pollutant Toxicity 0.000 description 19
- 238000002474 experimental method Methods 0.000 description 17
- 239000011259 mixed solution Substances 0.000 description 16
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000002351 wastewater Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 6
- 244000005700 microbiome Species 0.000 description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 5
- 239000005642 Oleic acid Substances 0.000 description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 5
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000004005 microsphere Substances 0.000 description 4
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 description 3
- 239000004952 Polyamide Substances 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 239000013522 chelant Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 2
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
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- 239000000377 silicon dioxide Substances 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
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- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 2
- 239000005050 vinyl trichlorosilane Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 description 1
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
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- 239000002893 slag Substances 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
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- 238000002798 spectrophotometry method Methods 0.000 description 1
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- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Landscapes
- Purification Treatments By Anaerobic Or Anaerobic And Aerobic Bacteria Or Animals (AREA)
Abstract
The invention discloses a preparation method of fiber composite magnetic particles and application of the fiber composite magnetic particles as biological carriers, relating to the technical field of biological fillers, and the technical scheme is characterized by comprising the following steps: (1) Adding ferroferric oxide magnetic particles into a reactor filled with pure water, carrying out ultrasonic treatment, and homogenizing under the protection of nitrogen by using mechanical stirring; (2) Adding a modifier and a surfactant into the system at 35-55 ℃ and aging; (3) Dropwise adding a mixed monomer solution of styrene, a cross-linking agent and an epoxy monomer into the system; (4) after the dripping is finished, adding fibers, and uniformly stirring; (5) After stirring uniformly, adding an initiator into the system, heating to 65-85 ℃, and preserving heat under stirring; (6) Filtering to obtain fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight; the fiber composite magnetic particles are hydrolyzed and modified or the metal particles are chelated after hydrolysis, and the fiber composite magnetic particles are used as biological carriers to be applied to aerobic or anaerobic biological water treatment.
Description
Technical Field
The invention relates to the technical field of biological fillers, in particular to a preparation method of fiber composite magnetic particles and application of the fiber composite magnetic particles as a biological carrier.
Background
Biological treatment is a mainstream technology of sewage treatment, wherein biofilm method based on biological filler is widely applied to fields of urban sewage, cultivation wastewater, chemical wastewater and the like, and is characterized in that microorganisms adhere to filter materials or certain carriers to grow and reproduce, membranous biological sludge is formed, and the biofilm intercepts microorganisms with a function of removing pollutants, so that loss of the functional microorganisms is reduced, and a certain protection is provided for the microorganisms. Magnetic fillers are receiving great attention due to their high surface area and recyclability, and the surface properties of the fillers, such as hydrophilicity, roughness, porosity, specific surface area, surface charge, etc., are important factors affecting the adsorption and immobilization of microorganisms.
The prior patent application document with reference to application publication number CN 113104959A discloses a magnetic silica particle, wherein the magnetic particle in the inner core has a shell structure, and the silica in the shell can protect the magnetic particle, avoid oxidation and dissolution, and prolong the service life. The method can be applied to sewage treatment, and can obviously improve the removal of ammonia nitrogen and Chemical Oxygen Demand (COD), but the research does not characterize the biocompatibility.
The prior patent application document with reference to application publication number CN 104609567A discloses a hydrophilic magnetic suspended biological filler and a preparation method thereof, wherein the hydrophilic suspended biological carrier is prepared by adding composite magnetic powder, rubber powder, zeolite powder, slag powder, polyethylene and the like, and performing extrusion molding, mechanical opening, short wave ultraviolet irradiation, crushing and the like, but the processing technology is complex and the cost is high.
None of the above prior art solves the problem of biocompatibility as a carrier.
Disclosure of Invention
The first aim of the invention is to provide a preparation method of fiber composite magnetic particles, and the second aim is to provide application of the fiber composite magnetic particles, and the treated fiber composite magnetic particles solve the problem of biocompatibility of the fiber composite magnetic particles serving as carriers.
In order to achieve the first object, the present invention provides the following technical solutions: the preparation method of the fiber composite magnetic particles comprises the following steps:
(1) Adding ferroferric oxide magnetic particles into a reactor filled with pure water, carrying out ultrasonic treatment for 15-30min, and homogenizing under the protection of nitrogen by using mechanical stirring;
(2) Adding a modifier and a surfactant into the system at 35-55 ℃ and aging for 2 hours;
(3) Then adding a mixed monomer solution of styrene, a cross-linking agent and an epoxy monomer into the system in a dropwise manner;
(4) After the dripping of the mixed monomer solution is finished, adding fibers, and uniformly stirring;
(5) After stirring uniformly, adding an initiator into the system, heating to 65-85 ℃, and preserving heat for 3-6h under stirring;
(6) Filtering to obtain fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight.
Further, the mass ratio of the modifier to the ferroferric oxide magnetic particles is 1:1-1.5:1.
Further, the amount of styrene is 60 to 80%, the amount of the crosslinking agent is 10 to 20%, and the amount of the epoxy monomer is 10 to 20% based on the total mass of the mixed monomer solution of styrene, the crosslinking agent and the epoxy monomer.
Further, the fiber diameter is 1-10 μm and the fiber length is 300-1000 μm.
Further, the mass ratio of the fiber to the mixed monomer solution is 1:200-1:5.
further, the prepared fiber composite magnetic particles are subjected to hydrolytic modification, and the method comprises the following steps:
adding the dried fiber composite magnetic particles into a reactor, adding a hydrolysis agent into the system, and hydrolyzing at 70-90 ℃ for 0.5-6h by using mechanical stirring; filtering to obtain hydrolyzed and modified fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight.
Further, the mass concentration of the hydrolytic agent is 1-20%.
Further, the hydrolytic agent comprises one or more of sodium hydroxide, potassium hydroxide, water glass, sodium phosphate, potassium phosphate and sodium sulfide.
Further, the fiber composite magnetic particles are subjected to chelated metal ion modification, and the method comprises the following steps:
adding the dried hydrolyzed fiber composite magnetic particles into a reactor, adding a metal salt solution into the system, and stirring for 2-5h at normal temperature; filtering to obtain fiber composite magnetic particles after hydrolysis modification and metal ion chelation, washing with pure water and ethanol, and vacuum drying to constant weight.
Further, the metal salt solution comprises one or more of ferric chloride, ferric sulfate, ferrous chloride, ferrous sulfate, cupric chloride, cupric sulfate, nickel chloride, nickel sulfate, manganese chloride and manganese sulfate.
Further, the mass concentration of the metal salt solution is 1-20%, and the mass ratio of the metal salt solution to the fiber composite magnetic particles is (200-5): 1.
in order to achieve the second object, the present invention provides the following technical solutions:
the application of the fiber composite magnetic particles or the modified particles thereof as a carrier in sewage treatment in an aerobic activated sludge reactor comprises the following steps:
1) Adding 1-20g/L of aerobic activated sludge and 1-20g/L of fiber composite magnetic particles or modified particles thereof into an activated sludge reactor, and controlling the air flow rate to be 200mL/min through a gas rotameter;
2) The method is operated in a sequencing batch mode, 12 hours is a period, each period of aeration is 11 hours, sedimentation is carried out for 30 minutes, and water draining and water inflow operations are carried out for 30 minutes; 500mL of supernatant liquid is discharged each time, 490mL of tap water and 10mL of simulated sewage concentrated solution are added; wherein the simulated sewage concentrate is prepared from ammonium chloride and sodium acetate, the ammonia nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L;
3) And continuously running for 10 days, sampling and measuring COD and ammonia nitrogen concentration in supernatant before each period of drainage, taking 50mL of sludge after 10 days to measure oxygen consumption rate, and observing the surface aerobic activated sludge of the fiber composite magnetic particles or the modified particles after 10 days.
The application of the fiber composite magnetic particles or the modified particles thereof as a carrier in sewage treatment by an anaerobic activated sludge reactor comprises the following steps:
1) Adding anaerobic activated sludge with the concentration of 5-40g/L and fiber composite magnetic particles or modified particles with the concentration of 1-15g/L into a sequencing batch reactor, stirring by adopting an intermittent stirring device, wherein the stirring frequency is 5min, stirring is 30s, and the temperature is controlled at 35+/-1 ℃;
2) Operating in a sequencing batch mode, wherein 12h is a period; aeration is carried out for 11 hours each cycle, sedimentation is carried out for 30 minutes, and water draining and water inflow operations are carried out for 30 minutes; 100mL of supernatant water is discharged each time, 97.5mL of tap water and 2.5mL of simulated sewage concentrate are added; wherein the simulated sewage concentrate is prepared from potassium nitrate and sodium acetate, the nitrate nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L;
3) The anaerobic activated sludge is continuously operated for 30 days, sampling is carried out before daily drainage, the sedimentation performance and COD removal effect of the anaerobic activated sludge are tested, and the anaerobic activated sludge on the surface of the fiber composite magnetic particles or modified particles thereof is observed after 30 days.
In summary, the invention has the following beneficial effects: the fiber length of the fiber composite magnetic particles is longer than that of the magnetic particles, and the velvet-shaped protrusions can extend out of the surface of the carrier, so that the specific surface area of the magnetic particles is increased; hydrolyzing the fiber on the surface of the fiber composite magnetic particle to form hydrophilic groups such as carboxyl and the like, and exposing the hydrophilic groups of the fiber, thereby realizing hydrophilization modification of the magnetic particle and improving the biological affinity of the magnetic particle; the metal ion chelation is carried out on the hydrolytic fibers on the surfaces of the fiber composite magnetic particles, so that the biological affinity of the magnetic particles is further improved, and the electron transfer efficiency among microorganisms in the activated sludge is promoted; the fiber composite magnetic particles or the modified particles thereof are applied to sewage treatment, so that the film forming speed of a biological film can be improved, the degradation of COD and ammonia nitrogen is promoted in an aerobic system, and the removal rate of COD and nitrate is promoted in an anaerobic system.
Drawings
FIG. 1 is a schematic diagram of the structure of a fiber composite magnetic particle according to the present invention, wherein A is a fiber composite magnetic particle, B is a hydrolysis modified fiber composite magnetic particle, and C: fiber composite magnetic particles that hydrolyze and chelate metal particles;
FIG. 2 is a microscopic view of the fiber composite magnetic particles prepared in example 1;
FIG. 3 is a scanning electron microscope image of the magnetic particles prepared in comparative example 1;
FIG. 4 is a fluorescence microscopy image 3 days after magnetic particle film formation, wherein (a): the fiber composite magnetic particles prepared in example 1, (b): the hydrolytically modified fiber composite magnetic particles produced in example 3, (c): the magnetic particles prepared in comparative example 1.
Detailed Description
In some embodiments, the modifier is selected from one or more of oleic acid, tartaric acid, gamma-aminotriethoxysilane, gamma-glycidoxypropyl trimethoxysilane, vinyl triethoxysilane, vinyl trichlorosilane, gamma-aminotrimethoxysilane.
In some embodiments, the surfactant is selected from one or more of sodium dodecyl sulfate, sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, sodium laurate, sodium oleate. More preferably one or more of sodium dodecyl sulfate, sodium dodecyl sulfonate and sodium dodecyl benzene sulfonate.
In some embodiments, the cross-linking agent is selected from one or more of divinylbenzene, N-methylenebisacrylamide, pentaerythritol triacrylate, ethylene glycol dimethacrylate, and pentaerythritol tetraacrylate.
In some embodiments, the epoxy-based monomer is selected from one or more of allyl glycidyl ether, glycidyl methacrylate, glycidyl acrylate.
In some embodiments, the fibers are one or more of polyester fibers, polyvinyl alcohol fibers, polyamide fibers, polyacrylonitrile fibers, polypropylene fibers, and polyvinyl chloride fibers.
In some embodiments, the initiator is selected from one or more of azobisisobutyronitrile, dibenzoyl peroxide, dodecanoyl peroxide, azobisisoheptonitrile, potassium persulfate, ammonia persulfate.
The present invention will be described in further detail with reference to examples.
Example 1
(1) Preparation of fiber composite magnetic particles
Adding 35g of ferroferric oxide magnetic particles into a 250mL four-mouth bottle filled with 100g of pure water, carrying out ultrasonic treatment for 30min, under the protection of nitrogen, using mechanical stirring to keep the temperature for 30min, adding 35g of oleic acid and 0.1g of sodium dodecyl sulfate into the system, heating to 65 ℃, aging for 2h, then dropwise adding a mixed solution of 75g of styrene, 15g of divinylbenzene and 15g of glycidyl methacrylate into the system, after the dropwise adding of the mixed solution is finished, adding 0.7g of polyester fiber with the length of 350 mu m and the diameter of 2 mu m, stirring uniformly, adding 6g of azo diisobutyronitrile serving as an initiator, keeping the temperature for 3h, filtering, obtaining fiber composite magnetic particles, washing with pure water and ethanol, and carrying out vacuum drying to constant weight.
(2) Film hanging and pollutant removal experiment of aerobic sewage treatment system
In a 1000mL activated sludge reactor, 800mL of aerobic activated sludge with a suspended solid content of 5000mg/L was added, 3.6g of the fiber composite magnetic particles obtained in the step (1) was added, and the gas flow rate was controlled to 200mL/min by a gas rotameter. The method is operated in a sequencing batch mode, 12 hours is a period, each period of aeration is 11 hours, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. 500mL of sewage is discharged each time, 490mL of water is fed, 10mL of simulated sewage concentrate is initially added each cycle, wherein the ammonia nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. And continuously running for 10 days, sampling and measuring COD and ammonia nitrogen concentration in supernatant before each period of drainage, taking 50mL of sludge after 10 days to measure oxygen consumption rate, and observing the aerobic activated sludge on the surface of the fiber composite magnetic particles after 10 days.
(3) Film forming and pollutant removal experiment of anaerobic sewage treatment system
And adding the inoculated anaerobic activated sludge and the fiber composite magnetic particles into a 250mL sequencing batch reactor, stirring by adopting an intermittent stirring device, wherein the stirring frequency is 5min, stirring is 30s, and the temperature is controlled at 35+/-1 ℃. Run in a sequencing batch mode, 12h is a period. Aeration is carried out for 11 hours each cycle, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. Each time 100mL of wastewater is discharged, 97.5mL of water is fed, 2.5mL of simulated sewage concentrate is initially added in each period, wherein the nitrate nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. The anaerobic activated sludge is continuously operated for 30 days, sampling is carried out before daily drainage, the sedimentation performance and COD removal effect of the anaerobic activated sludge are tested, and the anaerobic activated sludge on the surface of the fiber composite magnetic particles is observed after 30 days.
Example 2
(1) Preparation of fiber composite magnetic particles
Adding 35g of ferroferric oxide magnetic particles into a 250mL four-mouth bottle filled with 100g of pure water, carrying out ultrasonic treatment for 30min, under the protection of nitrogen, using mechanical stirring to keep the temperature for 30min, adding 35g of oleic acid and 0.1g of sodium dodecyl sulfate into the system, heating to 65 ℃, aging for 2h, then dropwise adding a mixed solution of 75g of styrene, 15g of divinylbenzene and 15g of glycidyl methacrylate into the system, after the dropwise adding of the mixed solution is finished, adding 0.7g of polyvinyl alcohol fiber with the length of 400 mu m and the diameter of 2 mu m, stirring uniformly, adding 6g of dibenzoyl peroxide serving as an initiator, keeping the temperature for 3h, filtering, obtaining fiber composite magnetic particles, washing with pure water and ethanol, and carrying out vacuum drying to constant weight.
(2) Film hanging and pollutant removal experiment of aerobic sewage treatment system
In a 1000mL activated sludge reactor, 800mL of aerobic activated sludge with a suspended solid content of 5000mg/L was added, 3.6g of the fiber composite magnetic particles obtained in the step (1) was added, and the gas flow rate was controlled to 200mL/min by a gas rotameter. The method is operated in a sequencing batch mode, 12 hours is a period, each period of aeration is 11 hours, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. 500mL of sewage is discharged each time, 490mL of water is fed, 10mL of simulated sewage concentrate is initially added each cycle, wherein the ammonia nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. And continuously running for 10 days, sampling and measuring COD and ammonia nitrogen concentration in supernatant before each period of drainage, taking 50mL of sludge after 10 days to measure oxygen consumption rate, and observing the aerobic activated sludge on the surface of the fiber composite magnetic particles after 10 days.
(3) Film forming and pollutant removal experiment of anaerobic sewage treatment system
And adding the inoculated anaerobic activated sludge and the fiber composite magnetic particles into a 250mL sequencing batch reactor, stirring by adopting an intermittent stirring device, wherein the stirring frequency is 5min, stirring is 30s, and the temperature is controlled at 35+/-1 ℃. Run in a sequencing batch mode, 12h is a period. Aeration is carried out for 11 hours each cycle, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. Each time 100mL of wastewater is discharged, 97.5mL of water is fed, 2.5mL of simulated sewage concentrate is initially added in each period, wherein the nitrate nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. The anaerobic activated sludge is continuously operated for 30 days, sampling is carried out before daily drainage, the sedimentation performance and COD removal effect of the anaerobic activated sludge are tested, and the anaerobic activated sludge on the surface of the fiber composite magnetic particles is observed after 30 days.
Example 3
(1) Preparation of fiber composite magnetic particles
Adding 35g of ferroferric oxide magnetic particles into a 250mL four-mouth bottle filled with 100g of pure water, carrying out ultrasonic treatment for 30min, under the protection of nitrogen, using mechanical stirring to keep the temperature for 30min, adding 40g of tartaric acid and 0.1g of sodium dodecyl sulfate into the system, heating to 65 ℃, aging for 2h, then dropwise adding a mixed solution of 75g of styrene, 15g of divinylbenzene and 15g of glycidyl methacrylate into the system, after the dropwise adding of the mixed solution is finished, adding 0.7g of polyvinyl alcohol fiber with the length of 350 mu m and the diameter of 2 mu m, stirring uniformly, adding 6g of lauroyl peroxide serving as an initiator, keeping the temperature for 3h, filtering, obtaining fiber composite magnetic particles, washing with pure water and ethanol, and carrying out vacuum drying to constant weight.
(2) Hydrolytic modification of fiber composite magnetic particles
Adding 100g of the fiber composite magnetic particles obtained in the step (1) into a reactor, adding 100g of 15% sodium hydroxide solution by mass concentration, and hydrolyzing for 3 hours at a high temperature of 80 ℃ by using mechanical stirring; filtering to obtain hydrolyzed fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight.
(3) Film hanging and pollutant removal experiment of aerobic sewage treatment system
In a 1000mL activated sludge reactor, 800mL of aerobic activated sludge with suspended solid content of 5000mg/L is added, 3.6g of the fiber composite magnetic particles obtained in the step (2) after hydrolysis modification is added, and the gas flow rate is controlled to be 200mL/min through a gas rotameter. The method is operated in a sequencing batch mode, 12 hours is a period, each period of aeration is 11 hours, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. 500mL of sewage is discharged each time, 490mL of water is fed, 10mL of simulated sewage concentrate is initially added each cycle, wherein the ammonia nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. And continuously running for 10 days, sampling and measuring COD and ammonia nitrogen concentration in supernatant before each period of drainage, taking 50mL of sludge after 10 days to measure oxygen consumption rate, and observing the aerobic activated sludge on the surface of the fiber composite magnetic particles after 10 days.
(4) Film forming and pollutant removal experiment of anaerobic sewage treatment system
Adding inoculated anaerobic activated sludge and the fiber composite magnetic particles obtained in the step (2) after hydrolysis modification into a 250mL sequencing batch reactor, stirring by adopting an intermittent stirring device, wherein the stirring frequency is 5min, stirring is 30s, and the temperature is controlled at 35+/-1 ℃. Run in a sequencing batch mode, 12h is a period. Aeration is carried out for 11 hours each cycle, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. Each time 100mL of wastewater is discharged, 97.5mL of water is fed, 2.5mL of simulated sewage concentrate is initially added in each period, wherein the nitrate nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. The anaerobic activated sludge is continuously operated for 30 days, sampling is carried out before daily drainage, the sedimentation performance and COD removal effect of the anaerobic activated sludge are tested, and the anaerobic activated sludge on the surface of the fiber composite magnetic particles is observed after 30 days.
Example 4
(1) Preparation of fiber composite magnetic particles
Adding 35g of ferroferric oxide magnetic particles into a 250mL four-mouth bottle filled with 100g of pure water, carrying out ultrasonic treatment for 30min, under the protection of nitrogen, using mechanical stirring to keep the temperature for 30min, adding 35g of oleic acid and 0.1g of sodium dodecyl sulfate into the system, heating to 65 ℃, aging for 2h, then dropwise adding a mixed solution of 75g of styrene, 15g of pentaerythritol triacrylate and 15g of allyl glycidyl ether into the system, after the dropwise addition of the mixed solution is finished, adding 0.7g of polyamide fiber with the length of 450 mu m and the diameter of 3 mu m, stirring uniformly, adding 6g of azo-diisoheptanenitrile serving as an initiator, keeping the temperature for 3h, filtering, obtaining fiber composite magnetic particles, washing with pure water and ethanol, and carrying out vacuum drying to constant weight.
(2) Hydrolytic modification of fiber composite magnetic particles
Adding 100g of the fiber composite magnetic particles obtained in the step (1) into a reactor, adding 150g of potassium hydroxide solution with mass concentration of 5%, and hydrolyzing for 2 hours at a high temperature of 80 ℃ by using mechanical stirring; filtering to obtain hydrolyzed fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight.
(3) Film hanging and pollutant removal experiment of aerobic sewage treatment system
In a 1000mL activated sludge reactor, 800mL of aerobic activated sludge with suspended solid content of 5000mg/L is added, 3.6g of the fiber composite magnetic particles obtained in the step (2) after hydrolysis modification is added, and the gas flow rate is controlled to be 200mL/min through a gas rotameter. The method is operated in a sequencing batch mode, 12 hours is a period, each period of aeration is 11 hours, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. 500mL of sewage is discharged each time, 490mL of water is fed, 10mL of simulated sewage concentrate is initially added each cycle, wherein the ammonia nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. And continuously running for 10 days, sampling and measuring COD and ammonia nitrogen concentration in supernatant before each period of drainage, taking 50mL of sludge after 10 days to measure oxygen consumption rate, and observing the aerobic activated sludge on the surface of the fiber composite magnetic particles after 10 days.
(4) Film forming and pollutant removal experiment of anaerobic sewage treatment system
Adding inoculated anaerobic activated sludge and the fiber composite magnetic particles obtained in the step (2) after hydrolysis modification into a 250mL sequencing batch reactor, stirring by adopting an intermittent stirring device, wherein the stirring frequency is 5min, stirring is 30s, and the temperature is controlled at 35+/-1 ℃. Run in a sequencing batch mode, 12h is a period. Aeration is carried out for 11 hours each cycle, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. Each time 100mL of wastewater is discharged, 97.5mL of water is fed, 2.5mL of simulated sewage concentrate is initially added in each period, wherein the nitrate nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. The anaerobic activated sludge is continuously operated for 30 days, sampling is carried out before daily drainage, the sedimentation performance and COD removal effect of the anaerobic activated sludge are tested, and the anaerobic activated sludge on the surface of the fiber composite magnetic particles is observed after 30 days.
Example 5
(1) Preparation of fiber composite magnetic particles
Adding 35g of ferroferric oxide magnetic particles into a 250mL four-mouth bottle filled with 100g of pure water, carrying out ultrasonic treatment for 30min, under the protection of nitrogen, using mechanical stirring to keep the temperature for 30min, adding 35g of vinyl triethoxysilane and 0.1g of sodium dodecyl sulfate into the system, heating to 65 ℃, aging for 2h, then dropwise adding a mixed solution of 75g of styrene, 15g of pentaerythritol triacrylate and 15g of glycidyl methacrylate into the system, after the dropwise adding of the mixed solution is finished, adding 0.7g of polyacrylonitrile fiber with the length of 500 mu m and the diameter of 4 mu m, stirring uniformly, adding 6g of initiator potassium persulfate, keeping the temperature for 3h, filtering, and obtaining fiber composite magnetic particles, washing with pure water and ethanol, and carrying out vacuum drying to constant weight.
(2) Hydrolytic modification of fiber composite magnetic particles
Adding 100g of the fiber composite magnetic particles obtained in the step (1) into a reactor, adding 200g of 10% sodium hydroxide solution by mass concentration, and hydrolyzing at 80 ℃ for 6h by using mechanical stirring; filtering to obtain hydrolyzed fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight.
(3) Biological affinity modification of fiber composite magnetic particle chelated metal ions
Adding 20g of the fiber composite magnetic particles obtained in the step (2) after hydrolysis modification into a reactor, adding 500g of 15% copper chloride solution into the system, and stirring for 2-5h at normal temperature; filtering to obtain fiber composite magnetic particles after hydrolysis modification and metal ion chelation, washing with pure water and ethanol, and vacuum drying to constant weight.
(4) Film hanging and pollutant removal experiment of aerobic sewage treatment system
In a 1000mL activated sludge reactor, 800mL of aerobic activated sludge with suspended solid content of 5000mg/L is added, 3.6g of fiber composite magnetic particles which are obtained in the step (3) and are subjected to hydrolysis modification and chelate of metal ions is added, and the gas flow rate is controlled to be 200mL/min through a gas rotameter. The method is operated in a sequencing batch mode, 12 hours is a period, each period of aeration is 11 hours, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. 500mL of sewage is discharged each time, 490mL of water is fed, 10mL of simulated sewage concentrate is initially added each cycle, wherein the ammonia nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. And continuously running for 10 days, sampling and measuring COD and ammonia nitrogen concentration in supernatant before each period of drainage, taking 50mL of sludge after 10 days to measure oxygen consumption rate, and observing the aerobic activated sludge on the surface of the fiber composite magnetic particles after 10 days.
(5) Film forming and pollutant removal experiment of anaerobic sewage treatment system
Adding inoculated anaerobic activated sludge and fiber composite magnetic particles obtained in the step (3) after hydrolysis modification and metal ion chelation into a 250mL sequencing batch reactor, stirring by an intermittent stirring device for 30s at a stirring frequency of 5min, and controlling the temperature at 35+/-1 ℃. Run in a sequencing batch mode, 12h is a period. Aeration is carried out for 11 hours each cycle, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. Each time 100mL of wastewater is discharged, 97.5mL of water is fed, 2.5mL of simulated sewage concentrate is initially added in each period, wherein the nitrate nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. The anaerobic activated sludge is continuously operated for 30 days, sampling is carried out before daily drainage, the sedimentation performance and COD removal effect of the anaerobic activated sludge are tested, and the anaerobic activated sludge on the surface of the fiber composite magnetic particles is observed after 30 days.
Example 6
(1) Preparation of fiber composite magnetic particles
Adding 35g of ferroferric oxide magnetic particles into a 250mL four-mouth bottle filled with 100g of pure water, carrying out ultrasonic treatment for 30min, under the protection of nitrogen, using mechanical stirring to keep the temperature for 30min, adding 35g of oleic acid and 0.1g of sodium dodecyl sulfate into the system, heating to 65 ℃, aging for 2h, then dropwise adding a mixed solution of 75g of styrene, 15g of ethylene glycol dimethacrylate and 15g of glycidyl acrylate into the system, after the dropwise addition of the mixed solution is finished, adding 0.7g of polyvinyl chloride fiber with the length of 200 mu m and the diameter of 5 mu m, stirring uniformly, adding 6g of ammonium persulfate serving as an initiator, keeping the temperature for 3h, filtering, obtaining fiber composite magnetic particles, washing with pure water and ethanol, and carrying out vacuum drying to constant weight.
(2) Hydrolytic modification of fiber composite magnetic particles
Adding 100g of dried fiber composite magnetic particles into a reactor, adding 250g of potassium hydroxide solution with mass concentration of 8%, and hydrolyzing for 4 hours at a high temperature of 80 ℃ by using mechanical stirring; filtering to obtain hydrolyzed fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight.
(3) Biological affinity modification of fiber composite magnetic particle chelated metal ions
Adding 20g of the fiber composite magnetic particles obtained in the step (2) after hydrolysis modification into a reactor, adding 400g of 10% ferrous sulfate solution into the system, and stirring for 2-5h at normal temperature; filtering to obtain fiber composite magnetic particles after hydrolysis modification and metal ion chelation, washing with pure water and ethanol, and vacuum drying to constant weight.
(4) Film hanging and pollutant removal experiment of aerobic sewage treatment system
In a 1000mL activated sludge reactor, 800mL of aerobic activated sludge with suspended solid content of 5000mg/L is added, 3.6g of fiber composite magnetic particles which are obtained in the step (3) and are subjected to hydrolysis modification and chelate of metal ions is added, and the gas flow rate is controlled to be 200mL/min through a gas rotameter. The method is operated in a sequencing batch mode, 12 hours is a period, each period of aeration is 11 hours, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. 500mL of sewage is discharged each time, 490mL of water is fed, 10mL of simulated sewage concentrate is initially added each cycle, wherein the ammonia nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. And continuously running for 10 days, sampling and measuring COD and ammonia nitrogen concentration in supernatant before each period of drainage, taking 50mL of sludge after 10 days to measure oxygen consumption rate, and observing the aerobic activated sludge on the surface of the fiber composite magnetic particles after 15 days.
(5) Film forming and pollutant removal experiment of anaerobic sewage treatment system
Adding inoculated anaerobic activated sludge and fiber composite magnetic particles obtained in the step (3) after hydrolysis modification and metal ion chelation into a 250mL sequencing batch reactor, stirring by an intermittent stirring device for 30s at a stirring frequency of 5min, and controlling the temperature at 35+/-1 ℃. Run in a sequencing batch mode, 12h is a period. Aeration is carried out for 11 hours each cycle, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. Each time 100mL of wastewater is discharged, 97.5mL of water is fed, 2.5mL of simulated sewage concentrate is initially added in each period, wherein the nitrate nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. The anaerobic activated sludge is continuously operated for 30 days, sampling is carried out before daily drainage, the sedimentation performance and COD removal effect of the anaerobic activated sludge are tested, and the anaerobic activated sludge on the surface of the fiber composite magnetic particles is observed after 30 days.
Example 7
(1) Preparation of fiber composite magnetic particles
Adding 35g of ferroferric oxide magnetic particles into a 250mL four-mouth bottle filled with 100g of pure water, carrying out ultrasonic treatment for 30min, under the protection of nitrogen, using mechanical stirring to keep the temperature for 30min, adding 35g of gamma-glycidol ether oxypropyl trimethoxy silane and 0.1g of sodium dodecyl sulfate into the system, heating to 65 ℃, aging for 2h, then dropwise adding a mixed solution of 75g of styrene, 15g of divinylbenzene and 15g of allyl glycidyl ether into the system, after the dropwise adding of the mixed solution is finished, adding 0.7g of polyamide fiber with the length of 400 mu m and the diameter of 6 mu m, stirring uniformly, adding 6g of azo-diisobutyronitrile as an initiator, keeping the temperature for 3h, filtering, washing with pure water and ethanol, and carrying out vacuum drying to constant weight to obtain the composite fiber magnetic particles.
(2) Hydrolytic modification of fiber composite magnetic particles
Adding 100g of dried fiber composite magnetic particles into a reactor, adding 300g of sodium phosphate solution with the mass concentration of 12%, and hydrolyzing for 6 hours at a high temperature of 90 ℃ by using mechanical stirring; filtering to obtain hydrolyzed fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight.
(3) Film hanging and pollutant removal experiment of aerobic sewage treatment system
In a 1000mL activated sludge reactor, 800mL of aerobic activated sludge with suspended solid content of 5000mg/L is added, 3.6g of the fiber composite magnetic particles obtained in the step (2) after hydrolysis modification is added, and the gas flow rate is controlled to be 200mL/min through a gas rotameter. The method is operated in a sequencing batch mode, 12 hours is a period, each period of aeration is 11 hours, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. 500mL of sewage is discharged each time, 490mL of water is fed, 10mL of simulated sewage concentrate is initially added each cycle, wherein the ammonia nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. And continuously running for 10 days, sampling and measuring COD and ammonia nitrogen concentration in supernatant before each period of drainage, taking 50mL of sludge after 10 days to measure oxygen consumption rate, and observing the aerobic activated sludge on the surface of the fiber composite magnetic particles after 10 days.
(4) Film forming and pollutant removal experiment of anaerobic sewage treatment system
Adding inoculated anaerobic activated sludge and the fiber composite magnetic particles obtained in the step (2) after hydrolysis modification into a 250mL sequencing batch reactor, stirring by adopting an intermittent stirring device, wherein the stirring frequency is 5min, stirring is 30s, and the temperature is controlled at 35+/-1 ℃. Run in a sequencing batch mode, 12h is a period. Aeration is carried out for 11 hours each cycle, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. Each time 100mL of wastewater is discharged, 97.5mL of water is fed, 2.5mL of simulated sewage concentrate is initially added in each period, wherein the nitrate nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. The anaerobic activated sludge is continuously operated for 30 days, sampling is carried out before daily drainage, the sedimentation performance and COD removal effect of the anaerobic activated sludge are tested, and the anaerobic activated sludge on the surface of the fiber composite magnetic particles is observed after 30 days.
Example 8
(1) Preparation of fiber composite magnetic particles
Adding 35g of ferroferric oxide magnetic particles into a 250mL four-mouth bottle filled with 100g of pure water, carrying out ultrasonic treatment for 30min, under the protection of nitrogen, using mechanical stirring to keep the temperature for 30min, adding 35g of vinyl trichlorosilane and 0.1g of sodium dodecyl sulfate into the system, heating to 65 ℃, aging for 2h, then dropwise adding a mixed solution of 75g of styrene, 15g of pentaerythritol triacrylate and 15g of glycidyl methacrylate into the system, after the dropwise addition of the mixed solution is finished, adding 0.7g of polypropylene fiber with the length of 350 mu m and the diameter of 7 mu m, stirring uniformly, adding 6g of initiator potassium persulfate, keeping the temperature for 3h, filtering, obtaining fiber composite magnetic particles, washing with pure water and ethanol, and carrying out vacuum drying to constant weight.
(2) Hydrolytic modification of fiber composite magnetic particles
Adding 100g of dried fiber composite magnetic particles into a reactor, adding 350g of sodium sulfide solution with mass concentration of 5%, and hydrolyzing at 80 ℃ for 0.5h by using mechanical stirring; filtering to obtain hydrolyzed fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight.
(3) Film hanging and pollutant removal experiment of aerobic sewage treatment system
In a 1000mL activated sludge reactor, 800mL of aerobic activated sludge with suspended solid content of 5000mg/L is added, 3.6g of the fiber composite magnetic particles obtained in the step (2) after hydrolysis modification is added, and the gas flow rate is controlled to be 200mL/min through a gas rotameter. The method is operated in a sequencing batch mode, 12 hours is a period, each period of aeration is 11 hours, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. 500mL of sewage is discharged each time, 490mL of water is fed, 10mL of simulated sewage concentrate is initially added each cycle, wherein the ammonia nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. And continuously running for 10 days, sampling and measuring COD and ammonia nitrogen concentration in supernatant before each period of drainage, taking 50mL of sludge after 10 days to measure oxygen consumption rate, and observing the aerobic activated sludge on the surface of the fiber composite magnetic particles after 10 days.
(4) Film forming and pollutant removal experiment of anaerobic sewage treatment system
Adding inoculated anaerobic activated sludge and the fiber composite magnetic particles obtained in the step (2) after hydrolysis modification into a 250mL sequencing batch reactor, stirring by adopting an intermittent stirring device, wherein the stirring frequency is 5min, stirring is 30s, and the temperature is controlled at 35+/-1 ℃. Run in a sequencing batch mode, 12h is a period. Aeration is carried out for 11 hours each cycle, sedimentation is carried out for 30 minutes, and operations such as water drainage, water inflow and the like are carried out for 30 minutes. Each time 100mL of wastewater is discharged, 97.5mL of water is fed, 2.5mL of simulated sewage concentrate is initially added in each period, wherein the nitrate nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L. The anaerobic activated sludge is continuously operated for 30 days, sampling is carried out before daily drainage, the sedimentation performance and COD removal effect of the anaerobic activated sludge are tested, and the anaerobic activated sludge on the surface of the fiber composite magnetic particles is observed after 30 days.
Comparative example 1
(1) Preparation of magnetic microparticles
Ferroferric oxide polymer particles were prepared in the same manner as in step (1) of example 1, except that the step of adding 0.7g of polyester fiber having a length of 350 μm and a diameter of 2 μm was not included.
(2) The membrane formation and contaminant removal of the aerobic wastewater treatment system were the same as in example 1.
(3) The membrane formation and contaminant removal of the anaerobic wastewater treatment system were the same as in example 1.
Test method and results:
and (3) microscopic observation: the prepared fiber composite magnetic particles and the magnetic particles which are hydrolyzed, modified and chelated with metal ions are dried and then observed under a microscope, and fluorescent microscope pictures of a photographed material sample are shown in fig. 2 and 3, so that the magnetic microspheres prepared in example 1 can be found to have obvious fibrous structures, while the magnetic microspheres prepared in comparative example 1 can not be observed, namely, the method of example 1 can successfully composite fibers into the magnetic microspheres and enable the surfaces of the microspheres to be in fibrous shapes.
Adsorption activated sludge test: 1g of sterilized biofilm carrier sample was taken and added separately to 250mL Erlenmeyer flasks containing 100mL of activated sludge suspension. Three parallel samples are arranged in each group, the test sample bottles are placed in a shaking table oscillator at 37 ℃ and 200rpm, magnetic particles are taken out for fluorescent staining after shaking for 3 days, under the same test conditions, a fluorescent microscope picture of a photographed material sample is shown in fig. 4, it can be found that the activated sludge adsorbed in the example 1 is obviously more than that in the comparative example 1, and the fibrous protrusions rich in the particles in the example 1 obviously have stronger fluorescent intensity, namely, the compounding of the fibers is favorable for adsorbing more activated sludge.
Aerobic water treatment application test: the fiber composite magnetic particles of the example and the magnetic particles of the comparative example are put into a bioreactor to carry out a film forming and pollutant removal experiment of an aerobic sewage treatment system, the experimental scheme is consistent with the step (2) of the example 1, the COD concentration and the ammonia nitrogen concentration adopt a kit corresponding to Lianhua technology Co., ltd, and the test result is shown in Table 1 and only 10 th day data is taken as an example.
Anaerobic water treatment application test: the fiber composite magnetic particles of the example and the magnetic particles of the comparative example are placed in a bioreactor to carry out film formation and pollutant removal tests of an anaerobic sewage treatment system, the test scheme is consistent with the step (3) of the example 1, the COD concentration is tested by adopting a kit corresponding to Lianhua technology Co., ltd, the nitrate nitrogen concentration is tested by adopting an ultraviolet spectrophotometry, and the test result is shown in Table 1, and only 30 day data are taken as an example.
Table 1 results of water treatment tests for each of examples and comparative examples
As can be seen from Table 1, in the aerobic water treatment, the degradation rates of COD and ammonia nitrogen are superior to those of the common magnetic particles, and after the hydrolysis modification and the chelation of the metal particles are carried out on the fiber composite magnetic particles, the biological affinity is improved, so that the degradation rates of COD and ammonia nitrogen are higher than those of the unmodified fiber composite magnetic particles; in the anaerobic water treatment, the removal rates of COD and nitrate of the fiber composite magnetic particles are higher than those of the common magnetic particles, and the biological affinity of the fiber composite magnetic particles is further improved after the metal particles are hydrolyzed and modified and chelated, so that the degradation rates of COD and ammonia nitrogen are higher than those of the unmodified fiber composite magnetic particles.
The present embodiment is only for explanation of the present invention and is not to be construed as limiting the present invention, and modifications to the present embodiment, which may not creatively contribute to the present invention as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present invention.
Claims (10)
1. The preparation method of the fiber composite magnetic particles is characterized by comprising the following steps:
(1) Adding ferroferric oxide magnetic particles into a reactor filled with pure water, carrying out ultrasonic treatment for 15-30min, and homogenizing under the protection of nitrogen by using mechanical stirring;
(2) Adding a modifier and a surfactant into the system at 35-55 ℃ and aging for 2 hours;
(3) Then adding a mixed monomer solution of styrene, a cross-linking agent and an epoxy monomer into the system in a dropwise manner;
(4) After the dripping of the mixed monomer solution is finished, adding fibers, and uniformly stirring;
(5) After stirring uniformly, adding an initiator into the system, heating to 65-85 ℃, and preserving heat for 3-6h under stirring;
(6) Filtering to obtain fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight.
2. The method for preparing fiber composite magnetic particles according to claim 1, wherein the mass ratio of the modifier to the ferroferric oxide magnetic particles is 1:1-1.5:1..
3. The method for preparing fiber composite magnetic particles according to claim 1, wherein the amount of styrene is 60 to 80%, the amount of the crosslinking agent is 10 to 20%, and the amount of the epoxy-based monomer is 10 to 20% based on the total mass of the mixed monomer solution of styrene, the crosslinking agent and the epoxy-based monomer.
4. The method for producing a fiber composite magnetic particle according to claim 1, wherein the fiber diameter is 1 to 10 μm and the fiber length is 300 to 1000 μm.
5. A method of modifying a fibrous composite magnetic particle comprising the steps of:
adding the dried fiber composite magnetic particles into a reactor, adding a hydrolysis agent into the system, and hydrolyzing at 70-90 ℃ for 0.5-6h by using mechanical stirring; filtering to obtain hydrolyzed and modified fiber composite magnetic particles, washing with pure water and ethanol, and vacuum drying to constant weight.
6. A method of modifying a fibrous composite magnetic particle comprising the steps of:
adding the dried fiber composite magnetic particles subjected to hydrolysis modification according to claim 5 into a reactor, adding a metal salt solution into the system, and stirring for 2-5h at normal temperature; filtering to obtain fiber composite magnetic particles after hydrolysis modification and metal ion chelation, washing with pure water and ethanol, and vacuum drying to constant weight.
7. The method according to claim 5, wherein the hydrolytic agent comprises one or more of sodium hydroxide, potassium hydroxide, water glass, sodium phosphate, potassium phosphate and sodium sulfide, and the mass concentration of the hydrolytic agent is 1-20%.
8. The method according to claim 6, wherein the metal salt solution comprises one or more of ferric chloride, ferric sulfate, ferrous chloride, ferrous sulfate, cupric chloride, cupric sulfate, nickel chloride, nickel sulfate, manganese chloride and manganese sulfate, the mass concentration of the metal salt solution is 1-20%, and the mass ratio of the metal salt solution to the fiber composite magnetic particles is (200-5): 1.
9. use of the fiber composite magnetic particles or modified particles thereof according to any one of claims 1-8 as a carrier in the treatment of sewage in an aerobic activated sludge reactor, comprising the steps of:
1) Adding 1-20g/L of aerobic activated sludge and 1-20g/L of fiber composite magnetic particles or modified particles thereof into an activated sludge reactor, and controlling the air flow rate to be 200mL/min through a gas rotameter;
2) The method is operated in a sequencing batch mode, 12 hours is a period, each period of aeration is 11 hours, sedimentation is carried out for 30 minutes, and water draining and water inflow operations are carried out for 30 minutes; 500mL of supernatant liquid is discharged each time, 490mL of tap water and 10mL of simulated sewage concentrated solution are added; wherein the simulated sewage concentrate is prepared from ammonium chloride and sodium acetate, the ammonia nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L;
3) And continuously running for 10 days, sampling and measuring COD and ammonia nitrogen concentration in supernatant before each period of drainage, taking 50mL of sludge after 10 days to measure oxygen consumption rate, and observing the surface aerobic activated sludge of the fiber composite magnetic particles or the modified particles after 10 days.
10. Use of the fiber composite magnetic particles or modified particles thereof according to any one of claims 1-8 as a carrier in anaerobic activated sludge reactor for treating sewage, comprising the steps of:
1) Adding anaerobic activated sludge with the concentration of 5-40g/L and fiber composite magnetic particles or modified particles with the concentration of 1-15g/L into a sequencing batch reactor, stirring by adopting an intermittent stirring device, wherein the stirring frequency is 5min, stirring is 30s, and the temperature is controlled at 35+/-1 ℃;
2) Operating in a sequencing batch mode, wherein 12h is a period; aeration is carried out for 11 hours each cycle, sedimentation is carried out for 30 minutes, and water draining and water inflow operations are carried out for 30 minutes; 100mL of supernatant water is discharged each time, 97.5mL of tap water and 2.5mL of simulated sewage concentrate are added; wherein the simulated sewage concentrate is prepared from potassium nitrate and sodium acetate, the nitrate nitrogen concentration of the simulated sewage concentrate is 5g/L, and the COD concentration is 50g/L;
3) The anaerobic activated sludge is continuously operated for 30 days, sampling is carried out before daily drainage, the sedimentation performance and COD removal effect of the anaerobic activated sludge are tested, and the anaerobic activated sludge on the surface of the fiber composite magnetic particles or modified particles thereof is observed after 30 days.
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