CN106167332A - A kind of aniline intermediate produces the recycling processing method of waste water - Google Patents
A kind of aniline intermediate produces the recycling processing method of waste water Download PDFInfo
- Publication number
- CN106167332A CN106167332A CN201610550041.7A CN201610550041A CN106167332A CN 106167332 A CN106167332 A CN 106167332A CN 201610550041 A CN201610550041 A CN 201610550041A CN 106167332 A CN106167332 A CN 106167332A
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- China
- Prior art keywords
- treatment fluid
- waste water
- treatment
- processing method
- fluid
- Prior art date
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- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 239000002351 wastewater Substances 0.000 title claims abstract description 69
- 238000004064 recycling Methods 0.000 title claims abstract description 23
- 238000003672 processing method Methods 0.000 title claims abstract description 16
- 239000012530 fluid Substances 0.000 claims abstract description 152
- 238000000034 method Methods 0.000 claims abstract description 61
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 30
- 230000003647 oxidation Effects 0.000 claims abstract description 26
- 239000003463 adsorbent Substances 0.000 claims abstract description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 14
- 238000001179 sorption measurement Methods 0.000 claims abstract description 14
- 239000010413 mother solution Substances 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 9
- 239000007800 oxidant agent Substances 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 239000011780 sodium chloride Substances 0.000 claims abstract description 8
- 238000004061 bleaching Methods 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 5
- 238000010521 absorption reaction Methods 0.000 claims abstract description 5
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 42
- 238000004519 manufacturing process Methods 0.000 claims description 30
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 28
- 239000002253 acid Substances 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Substances [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 229910021529 ammonia Inorganic materials 0.000 claims description 14
- 229920002401 polyacrylamide Polymers 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000005189 flocculation Methods 0.000 claims description 9
- 230000016615 flocculation Effects 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000002699 waste material Substances 0.000 claims description 8
- 244000005700 microbiome Species 0.000 claims description 6
- 230000000844 anti-bacterial effect Effects 0.000 claims description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 230000007613 environmental effect Effects 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 241000894006 Bacteria Species 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
- 239000010802 sludge Substances 0.000 claims description 3
- 241000589220 Acetobacter Species 0.000 claims description 2
- 241000607548 Aeromonas media Species 0.000 claims description 2
- 241000193830 Bacillus <bacterium> Species 0.000 claims description 2
- 244000063299 Bacillus subtilis Species 0.000 claims description 2
- 241000588722 Escherichia Species 0.000 claims description 2
- 241000605122 Nitrosomonas Species 0.000 claims description 2
- 241000589516 Pseudomonas Species 0.000 claims description 2
- 241000168225 Pseudomonas alcaligenes Species 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 241000605118 Thiobacillus Species 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical group [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 2
- 239000004744 fabric Substances 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
- 238000007639 printing Methods 0.000 claims description 2
- 241000607534 Aeromonas Species 0.000 claims 1
- 241000588813 Alcaligenes faecalis Species 0.000 claims 1
- 241000305071 Enterobacterales Species 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 229940005347 alcaligenes faecalis Drugs 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 description 25
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 22
- 239000007788 liquid Substances 0.000 description 20
- 230000000694 effects Effects 0.000 description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 16
- 239000000975 dye Substances 0.000 description 16
- 239000000047 product Substances 0.000 description 16
- 230000008929 regeneration Effects 0.000 description 15
- 238000011069 regeneration method Methods 0.000 description 15
- 238000003756 stirring Methods 0.000 description 14
- 238000003825 pressing Methods 0.000 description 12
- 150000003839 salts Chemical class 0.000 description 12
- 239000003610 charcoal Substances 0.000 description 11
- 238000012545 processing Methods 0.000 description 11
- ZLCUIOWQYBYEBG-UHFFFAOYSA-N 1-Amino-2-methylanthraquinone Chemical compound C1=CC=C2C(=O)C3=C(N)C(C)=CC=C3C(=O)C2=C1 ZLCUIOWQYBYEBG-UHFFFAOYSA-N 0.000 description 10
- 239000000706 filtrate Substances 0.000 description 10
- 229920006395 saturated elastomer Polymers 0.000 description 10
- 235000019270 ammonium chloride Nutrition 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 238000005273 aeration Methods 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 5
- 238000005352 clarification Methods 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000002932 luster Substances 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002910 solid waste Substances 0.000 description 3
- FENJKTQEFUPECW-UHFFFAOYSA-N 3-anilinopropanenitrile Chemical compound N#CCCNC1=CC=CC=C1 FENJKTQEFUPECW-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000004155 Chlorine dioxide Substances 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000001448 anilines Chemical class 0.000 description 2
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 2
- 229940073608 benzyl chloride Drugs 0.000 description 2
- 238000005574 benzylation reaction Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 235000019398 chlorine dioxide Nutrition 0.000 description 2
- 238000007278 cyanoethylation reaction Methods 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000006200 ethylation reaction Methods 0.000 description 2
- -1 has Physical Substances 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- PEMGGJDINLGTON-UHFFFAOYSA-N n-(3-aminophenyl)acetamide Chemical compound CC(=O)NC1=CC=CC(N)=C1 PEMGGJDINLGTON-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000009418 renovation Methods 0.000 description 2
- OWXJKYNZGFSVRC-NSCUHMNNSA-N (e)-1-chloroprop-1-ene Chemical compound C\C=C\Cl OWXJKYNZGFSVRC-NSCUHMNNSA-N 0.000 description 1
- YNAKESQZGPZDDZ-UHFFFAOYSA-N 2-n,2-n-diethylbenzene-1,2-diamine Chemical compound CCN(CC)C1=CC=CC=C1N YNAKESQZGPZDDZ-UHFFFAOYSA-N 0.000 description 1
- 241000607522 Aeromonas sobria Species 0.000 description 1
- 241000588986 Alcaligenes Species 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- SWJZZIVUGZIVNC-UHFFFAOYSA-N NC1=C(OC)C=CC(C1)(N)C(C)=O Chemical compound NC1=C(OC)C=CC(C1)(N)C(C)=O SWJZZIVUGZIVNC-UHFFFAOYSA-N 0.000 description 1
- 241000605154 Nitrobacter winogradskyi Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- LPSCRKGVODJZIB-UHFFFAOYSA-N [I].[C] Chemical class [I].[C] LPSCRKGVODJZIB-UHFFFAOYSA-N 0.000 description 1
- 125000000738 acetamido group Chemical group [H]C([H])([H])C(=O)N([H])[*] 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000000986 disperse dye Substances 0.000 description 1
- 239000005446 dissolved organic matter Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 238000012994 industrial processing Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/74—Treatment of water, waste water, or sewage by oxidation with air
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/02—Aerobic processes
Abstract
The invention provides a kind of aniline intermediate and produce the recycling processing method of waste water, comprise the steps: that (1) flocculate: categorised collection also adjusts the pH value of waste water, adds flocculant and flocculates, and obtains precipitate I and treatment fluid I after filtration；(2) oxidation: regulation treatment fluid I pH value, add oxidant, fully oxidized after treatment fluid II；(3) adsorption bleaching: the pH value of regulation treatment fluid II, adds adsorbent, fully separates to obtain treatment fluid III after absorption；(4) neutralization, condensing crystallizing: the pH value of regulation treatment fluid III, enters enrichment facility and carries out condensing crystallizing, separated rear sodium chloride or the chloride solid of obtaining, and mother solution return enrichment facility continues condensing crystallizing, and collecting condensed fluid is treatment fluid IV；(5) biological treatment: obtain treatment fluid V after treatment fluid IV carries out BAF process, i.e. completes to process.
Description
Technical field
The present invention relates to technical field of waste water processing, be specifically related to a kind of aniline intermediate and produce at the resource of waste water
Reason method.
Background technology
Aniline intermediate is the important industrial chemicals of synthesis disperse dyes, China's aniline dyes intermediate especially
Big producing country, but it is as the raising day by day of dyestuff intermediate yield, dye intermediate wastewater brings serious environmental pollution
Problem, brings immense pressure to dyestuff intermediate industry development.
Aniline dyes intermediate has the features such as structure complexity, synthesis flow length, side reaction be many, causes in production process
Produce a large amount of complicated component, waste water that concentration is high.This type of dye intermediate wastewater belongs to high concentration, high chroma, highly-saline has
Machine waste water, therefore deals with the most thorny.
At present, the industrial processing method for this type of dye intermediate wastewater mainly has Physical, chemical method and biology
Method.
(1) Physical: mainly include extraction and absorption method.Complexing abstraction has that efficiency is high, equipment investment is few, simultaneously
The advantages such as resource reclaim can be realized, but due to amino benzene analog waste water complicated component, therefore cause Resource recovery composition the most up to standard,
Cannot normally use, also result in the waste of organic solvent.Resin adsorption method, has efficiency high, and technique is simple, easy to operate etc.
Advantage, but resin regeneration inefficient, cause using adsorption rate high for the first time, and after regeneration, service efficiency is gradually lowered, with high
Resin cost is compared, and utilizes the method the most uneconomical.
(2) chemical method: mainly include chemical oxidization method, electrochemical process and sonication.Oxidizing process can be by waste water
In poisonous, harmful components degrade further, improve B/C value, beneficially biodegradation, the method can as carry out a biological disposal upon auxiliary
Walker is rapid, it can be difficult to the high salt component removed in waste water, therefore, it is difficult to individual processing aniline intermediate waste water.
(3) bioanalysis: biological treatment is generally divided into anaerobic and aerobic and processes, by the old metabolism of the life of antibacterial, by waste water
In organic components one for self synthesize, a part changes into nontoxic material, thus realizes the Synthetic of waste water
Reason, but antibacterial is less for the demand of salinity, and high salinity waste water will cause antibacterial to be dehydrated and dead, thus cause department of biochemistry
System collapse, thus cannot individually take the method for biological treatment to process high salinity, high COD aniline intermediate waste water.
The Chinese invention patent document of Publication No. CN104803529A discloses one and utilizes resin absorption, multiple-effect evaporation
The method concentrating mixed processing aniline intermediate waste water, the method can process aniline intermediate waste water effectively, but
Owing to resin price is expensive, adsorption rate is low, revival rate variance, and desorbed solution reclaims the problems such as difficult, significantly limit its application.
The Chinese invention patent document of Publication No. CN1769206A discloses a kind of large pore macromolecular utilizing synthesis and gathers
Compound immobilized microorganism strengthening SBR processes the method that phenyl amines produces waste water, and the method is mainly the synthesis as carrier
Large pore macromolecular polymer be added to the bioreactor containing activated sludge, improve the biological treatment clearance to COD, but its
Mainly for low concentration COD aniline waste water, infeasible to high concentration COD aniline waste water.
In the face of increasingly serious environmental protection pressure, the most effectively, economical, process aniline dyes intermediate rationally, easily
Waste water becomes current dye industry and needs a great problem of solution badly.Dyestuff enterprise is except continually developing the production work of cleaning, environmental protection
Outside skill, more constantly to explore the waste water treatment scheme of the treatment of wastes with processes of wastes against one another, reach to become present treatment more to contaminate with minimum waste water control
Material waste water, the exploration of this thinking, not only contribute to the long term growth of middle-size and small-size dyestuff enterprise, before having more wide application
Scape.
Summary of the invention
The invention provides a kind of aniline intermediate and produce the recycling processing method of waste water, the method is by strict control
PH condition processed, sequentially passes through the steps such as flocculation, oxidation, adsorption bleaching, neutralization, condensing crystallizing, biological treatment, it is thus achieved that high-purity is secondary
Product, after biological treatment, recycling condensing water produces in intermediate simultaneously, thus reaches waste water reclaiming recycling and zero-emission
Purpose.
A kind of aniline intermediate produces the recycling processing method of waste water, comprises the steps:
(1) flocculation: categorised collection also adjusts the pH value of waste water to 7～12, adds flocculant and flocculates, must sink after filtration
Shallow lake thing I and treatment fluid I；
(2) oxidation: regulation treatment fluid I pH value to 1～6, add oxidant, fully oxidized after treatment fluid II；
(3) adsorption bleaching: the pH value of regulation treatment fluid II, to 1～6, adds adsorbent, fully separates after absorption to process
Liquid III；
(4) neutralization, condensing crystallizing: the pH value of regulation treatment fluid III, to 3～8, enters enrichment facility and carries out condensing crystallizing, warp
Obtaining sodium chloride or chloride solid after separation, mother solution returns enrichment facility and continues condensing crystallizing, and collection condensed fluid is treatment fluid
Ⅳ；
(5) biological treatment: obtain treatment fluid V after treatment fluid IV carries out BAF process, i.e. completes to process.
The organic components that aniline intermediate produces in waste water includes two parts, respectively dissolved organic matter composition
With insoluble organic components, insoluble organic components removed by the method that this technical scheme is flocculated by alkali tune, and solvable
Property organic components then by Adsorption under acid condition.
It is rich in sodium chloride or ammonium chloride in aniline intermediate production process that described aniline intermediate produces waste water
Waste water, especially taking sodium carbonate is that acid binding agent is prepared N-cyanoethyl-Phenhenzamine and prepares N-with ammonia for acid binding agent
Cyanoethyl-Phenhenzamine, N, acetamido between N-diallyl-2-methoxyl group-5-acetamido aniline or N, N-diethyl
The waste water produced during aniline.
The high-salt wastewater containing chloride ion produced in aniline dyes intermediate production process is carried out categorised collection
Time, according to dyestuff intermediate categorised collection of the same race, in order to the recovery of dyestuff intermediate and applying mechanically of mother solution.
Collect the Intermediate Wastewater containing chloride ion that obtains because the difference of intermediate production technology and content the most not
With, the method being all applicable to the present invention processes.As preferably, chlorine ions hundred in described aniline intermediate waste water
Proportion by subtraction content is 10～30%.
In step (1), regulation waste water pH value time, can use sodium hydroxide, potassium hydroxide, calcium hydroxide, calcium oxide and
At least one in ammonia.As preferably, produced spent lye or deposed ammonia in commercial production is used to regulate the pH of waste water
Value.
In step (1), the pH value of regulation waste water is to 7～12.As preferably, the pH value of regulation waste water to 7～8, pH value mistake
Height, then during oxidation, acid adding amount increases, and finally increases processing cost.
Described flocculant is aluminum sulfate, aluminum chloride, ferrous sulfate, iron chloride, aluminium polychlorid, polyaluminium sulfate, polymerization
At least one in iron sulfate and polyacrylamide.As preferably, described flocculant is polyacrylamide (PAM).Flocculant water
The mass fraction of solution is 0.05～0.5%, and the dosage of flocculant is the 0.02～2% of wastewater quality, and flocculation time is 0.5
～2h.
In step (1), gained precipitate I is dyestuff intermediate, can directly reclaim use.
In step (2), when regulating the pH value for the treatment of fluid I, produced abraum salt in hydrochloric acid or industrial processes can be used
Acid, as preferably, uses produced waste hydrochloric acid in industrial processes to regulate the pH for the treatment of fluid I.
In step (2), the pH value of regulation treatment fluid I is to 1～6.As preferably, the pH value for the treatment of fluid I is regulated to 3～6.
In step (2), the mode of described oxidation is hypochlorite oxidation, hydrogen peroxide oxidation, Chlorine Dioxide Oxidation, ozone oxygen
Change, air oxidation, Fenton oxidation, ultraviolet irradiate at least one in oxidation and oxidization by bleaching powder.
Described oxidant is at least one in sodium hypochlorite, hydrogen peroxide, chlorine dioxide, ozone and air.As preferably,
Described oxidant is hydrogen peroxide.
The dosage of described oxidant is the 0.01～1.0% for the treatment of fluid I mass, the time of described oxidation be 0.5～
12h.As preferably, the dosage of described oxidant is the 0.05～1.0% for the treatment of fluid I mass, and the time of described oxidation is 0.5
～4h.
As preferably, the mode of described oxidation is UV/H2O2Oxidation, H used2O2Mass fraction is 25～50%, purple used
Outer lamp is low pressure mercury lamp, and power is 8～120W.Further preferably, uviol lamp power used is 20～120W.
In step (3), when regulating the pH value for the treatment of fluid II, hydrochloric acid can be used.
In step (3), the pH value of regulation treatment fluid II is to 1～6.PH value of solution is the lowest, and solution percent of decolourization is the highest, and Organic substance goes
Except rate is the biggest.As preferably, the pH value for the treatment of fluid II is regulated to 1～2, under the conditions of this pH, carry out adsorption bleaching, can be notable
Reduce the usage amount of adsorbent.
In step (3), described adsorbent is at least one in activated carbon, kieselguhr, molecular sieve, the dosage of adsorbent
For the 0.05～1.0% for the treatment of fluid II mass, adsorption time is 0.5～4h.As preferably, described adsorbent is activated carbon, inhales
The dosage of attached dose is the 0.1～0.3% for the treatment of fluid II mass, and adsorption time is 0.5～2h.
In step (3), the renovation process of described adsorbent is hot recycling, solvent reclamation, ozone regeneration and ultrasonic regeneration
In at least one.As preferably, the renovation process of described adsorbent is hot recycling, and regeneration temperature is 400～850 DEG C, regeneration
Time is 0.5～4.0h, and the adsorbent after regeneration both can be also used as the decolorising agent of waste water as the adsorbent of waste water, subtracts
Lack the discharge of dangerous solid waste, thus reduce the processing cost of adsorbent.
In step (4), when regulating the pH value for the treatment of fluid III, sodium hydroxide, potassium hydroxide, calcium hydroxide, oxidation can be used
At least one in calcium and ammonia.As preferably, use the produced colourity spent lye or useless less than 50 times in commercial production
Ammonia regulates the pH for the treatment of fluid III.
In step (4), the pH value of regulation treatment fluid III is to 3～8.As preferably, the pH value for the treatment of fluid III is regulated to 3～
6。
In step (4), the mode of described condensing crystallizing is MVR evaporation and concentration, single-action concentration or Multi-effect concentration, as excellent
Choosing, the mode of described condensing crystallizing is MVR evaporation and concentration.
In step (5), in described BAF microorganism at least include raw branch move glue bacterium, wax printing fabric, in
Between Escherichia, escherichia coli, aerobacteria, excrement aerogenesis paracolon, unwrapping wire shape Nocard's bacillus, Bacillus subtillis, excrement
Alcaligenes, bacterium nitrobacter, Nitrosomonas, ball antibacterial, denitrification Thiobacillus, Pseudomonas alcaligenes, acetobacter, cause yellow
Pseudomonas, Aeromonas sobria and Aeromonas media.
Described microorganism is cultivated under treatment fluid IV environmental condition and is screened, and actual conditions state modulator is water temperature
25～38 DEG C, pH 6～8, activated sludge concentration 2～5g/L, dissolved oxygen concentration 2.0～4.5mg/L.Cultivate under this condition
Microorganism strong adaptability, it is possible to notable aniline degradation class material.
In step (5), aeration rate is 2.0～4.5mg/L, and the process time is 8～12h.
In step (5), after BAF processes, obtain treatment fluid V, make treatment fluid V reach industry water reuse mark
Standard, is back to the production of dyestuff intermediate.
Compared with prior art, there is advantages that
1, technique is simple: by realizing recycling of waste water after flocculating, aoxidize, adsorb, concentrate, carrying out a biological disposal upon,
Flow process is succinct, simple to operate, mild condition, it is simple to industrialized production；
2, the treatment of wastes with processes of wastes against one another: acid/base required during this process adjustments pH uses produced spent acid, salkali waste in commercial production,
Not only solve high concentration, high chroma, high salinity aniline intermediate waste water by the method, solve that acid number is big, alkali simultaneously
Property high, acidic and alkaline waste water that corrosivity is big；
3, economize on resources: this technique controls pH condition by strict, and activated carbon dosage is substantially reduced, and processes through hot recycling
After, can circulate applicable, thus reduce the processing cost of solid waste；
4, high financial profit: this process byproducts sodium chloride or purity >=99.5% of ammonium chloride, reaches commercial grade, can
For commercial production, it is favorably improved the economic benefit of enterprise.
5, recycle: in this technique, condensed fluid can be back to intermediate production after biological treatment, and intermediate is every
Qualified, it is achieved thereby that the zero-emission of waste water.
6, no coupling product produces: use UV/H in this technique2O2System carries out wastewater oxidation process, unnecessary H2O2Through height
Temperature is decomposed into water and oxygen, introduces without any by-product.
Accompanying drawing illustrates:
Fig. 1 is the technological process that the aniline intermediate that the embodiment of the present invention uses produces the recycling processing method of waste water
Figure.
Detailed description of the invention:
The aniline intermediate that the embodiment of the present invention uses produces technological process such as Fig. 1 of the recycling processing method of waste water
Shown in.
Embodiment 1
(1) collect respectively and produce the mother liquid coming of N-cyanoethyl-Phenhenzamine (i.e. cyanoethyl aniline and benzyl chloride is at soda
The lower reaction of effect produces the waste water of sodium chloride-containing) and washings, wherein washing water reuse produces in intermediate.Chlorination in mother liquid coming
The mass percentage content of sodium is 15%, and COD is 17400mg/L, and colourity is 1800 times.
Mother liquid coming enters flocculation still, adds produced spent lye regulation pH to 7～8 in commercial production, under stirring condition
Being continuously added to polyacrylamide solution, the mass fraction of polyacrylamide solution is 0.2%, and dosage is mother liquid coming quality
0.1%, after continuous stirring 15min, natural subsidence 1h, filter pressing, be separately recovered intermediate and obtain precipitate I and treatment fluid I.
After measured, in treatment fluid I, COD is 15280mg/L, and colourity is 1600 times.
(2) treatment fluid I is transferred to oxidation trough, adds the abraum salt acid for adjusting pH of generation in production disperse orange 288 and, to 3～4, opens
Open UV, add H2O2, H2O2Dosage is treatment fluid I mass 0.1%, fully react 2h, carry out after filter pressing obtaining treatment fluid
Ⅱ。
After measured, in treatment fluid II, COD is 9930mg/L, and colourity is 800 times.
(3) treatment fluid II enters acid adjustment still, add produce the abraum salt acid for adjusting pH that produces in disperse orange 288 to 1.0～
1.5, after regulation, solution enters decolouring still, adds activated carbon, and the dosage of activated carbon is the 0.2% for the treatment of fluid II mass, fully
After stirring 2h, destaining solution enters filter press plate, collects filtrate and saturated activity charcoal respectively.Saturated activity charcoal is through high temperature regeneration Posterior circle
Using, filtrate is treatment fluid III.
After measured, in treatment fluid III, COD is 1600mg/L, and colourity is 2 times.
(4) treatment fluid III enters and neutralizes still, adds sodium hydroxide regulation pH to 4～5, enters MVR equipment, carry out after regulation
Condensing crystallizing, after machine separates by centrifugation, obtaining purity is 99.5%, the sodium chloride crystal that color and luster is whiter.Crystalline mother solution is back to
MVR equipment, further condensing crystallizing, collecting evaporation condensate is treatment fluid IV, treatment fluid IV achromaticity and clarification.
After measured, in treatment fluid IV, COD is 680mg/L, and colourity is 1 times.
(5) treatment fluid IV carries out BAF process, and aeration rate is 2.0mg/L, obtains treatment fluid V after processing 12h,
After measured, in treatment fluid V COD be 40mg/L, COD clearance be 94.12%.
Treatment fluid V participates in the synthesis of N-cyanoethyl-Phenhenzamine, after cyanoethylation, Benzylation reaction, in obtaining
Mesosome product, product purity is 94.5%, and yield is 95.2%, complies fully with N-cyanoethyl-Phenhenzamine product requirement.
Embodiment 2
(1) collect respectively and produce the mother liquid coming of N-cyanoethyl-Phenhenzamine (i.e. cyanoethyl aniline and benzyl chloride is at ammonia
The lower reaction of effect produces the waste water of containing ammonium chloride) and washings, wherein washing water reuse produces in intermediate.Chlorination in mother liquid coming
The mass percentage content of ammonium is 18%, and COD is 16200mg/L, and colourity is 1700 times.
Mother liquid coming enters flocculation still, adds produced spent lye regulation pH to 7～8 in commercial production, under stirring condition
Being continuously added to polyacrylamide solution, the mass fraction of polyacrylamide solution is 0.2%, and dosage is mother liquid coming quality
0.1%, after continuous stirring 15min, natural subsidence 1h, filter pressing, be separately recovered intermediate and obtain precipitate I and treatment fluid I.
After measured, in treatment fluid I, COD is 14200mg/L, and colourity is 1520 times.
(2) treatment fluid I is transferred to oxidation trough, adds the abraum salt acid for adjusting pH of generation in production disperse orange 288 and, to 4～5, opens
Open UV, add H2O2, H2O2Dosage is treatment fluid I mass 0.1%, fully react 2h, carry out after filter pressing obtaining treatment fluid
Ⅱ。
After measured, in treatment fluid II, COD is 8800mg/L, and colourity is 750 times.
(3) treatment fluid II enters acid adjustment still, add produce the abraum salt acid for adjusting pH that produces in disperse orange 288 to 1.0～
1.5, after regulation, solution enters decolouring still, adds activated carbon, and the dosage of activated carbon is the 0.2% for the treatment of fluid II mass, fully
After stirring 2h, destaining solution enters filter press plate, collects filtrate and saturated activity charcoal respectively.Saturated activity charcoal is through high temperature regeneration Posterior circle
Using, filtrate is treatment fluid III.
After measured, in treatment fluid III, COD is 1280mg/L, and colourity is 3 times.
(4) treatment fluid III enters and neutralizes still, adds ammonia regulation pH to 3～4, enters MVR equipment, concentrate after regulation
Crystallization, after machine separates by centrifugation, obtaining purity is 99.5%, the ammonia chloride crystal that color and luster is whiter.Crystalline mother solution is back to MVR and sets
Standby, further condensing crystallizing, collecting evaporation condensate is treatment fluid IV, treatment fluid IV achromaticity and clarification.
After measured, in treatment fluid IV, COD is 420mg/L, and colourity is 1 times.
(5) treatment fluid IV carries out BAF process, and aeration rate is 2.5mg/L, obtains treatment fluid V after processing 11h,
In treatment fluid V COD be 36mg/L, COD clearance be 91.43%.
Treatment fluid V participates in the synthesis of N-cyanoethyl-Phenhenzamine, after cyanoethylation, Benzylation reaction, in obtaining
Mesosome product, product purity is 95.8%, and yield is 96.0%, and mononitrile is 2.0%, complies fully with N-cyanoethyl-N-benzyl benzene
Amine product requirement.
Embodiment 3
(1) respectively collect produce N, N-diallyl-2-methoxyl group-5-acetamido aniline mother liquid coming (i.e. 2-amino-
4-acetyl-anisidine and chloropropene react the waste water producing containing ammonium chloride under ammonia effect) and washings, wherein wash
Water circulation produces in intermediate.In mother liquid coming, the mass percentage content of ammonium chloride is 12%, and COD is 10960mg/L, and colourity is
1500 times.
Mother liquid coming enters flocculation still, adds produced spent lye regulation pH to 7～8 in commercial production, under stirring condition
Being continuously added to polyacrylamide solution, the mass fraction of polyacrylamide solution is 0.2%, and dosage is mother liquid coming quality
0.1%, after continuous stirring 15min, natural subsidence 1h, filter pressing, be separately recovered intermediate and obtain precipitate I and treatment fluid I.
After measured, in treatment fluid I, COD is 9500mg/L, and colourity is 1360 times.
(2) treatment fluid I is transferred to oxidation trough, adds the abraum salt acid for adjusting pH of generation in production disperse orange 288 and, to 5～6, opens
Open UV, add H2O2, H2O2Dosage is treatment fluid I mass 0.05%, fully react 2h, carry out after filter pressing obtaining treatment fluid
Ⅱ。
After measured, in treatment fluid II, COD is 5220mg/L, and colourity is 550 times.
(3) treatment fluid II enters acid adjustment still, add produce the abraum salt acid for adjusting pH that produces in disperse orange 288 to 1.0～
1.5, after regulation, solution enters decolouring still, adds activated carbon, and the dosage of activated carbon is the 0.3% for the treatment of fluid II mass, fully
After stirring 2h, destaining solution enters filter press plate, collects filtrate and saturated activity charcoal respectively.Saturated activity charcoal is through high temperature regeneration Posterior circle
Using, filtrate is treatment fluid III.
After measured, in treatment fluid III, COD is 480mg/L, and colourity is 2 times.
(4) treatment fluid III enters and neutralizes still, adds ammonia regulation pH to 5～6, enters MVR equipment, concentrate after regulation
Crystallization, after machine separates by centrifugation, obtaining purity is 99.2%, the ammonia chloride crystal that color and luster is whiter.Crystalline mother solution is back to MVR and sets
Standby, further condensing crystallizing, collecting evaporation condensate is treatment fluid IV, treatment fluid IV achromaticity and clarification.
After measured, in treatment fluid IV, COD is 120mg/L, and colourity is 1 times.
(5) treatment fluid IV carries out BAF process, and aeration rate is 3.0mg/L, obtains treatment fluid V after processing 10h,
After measured, in treatment fluid V COD be 20mg/L, COD clearance be 83.33%.
Treatment fluid V participates in the synthesis of N, N-diallyl-2-methoxyl group-5-acetamido aniline, after condensation, dilution,
Obtaining intermediate product, product purity is 96.5%, and yield is 98.0%, complies fully with N, N-diallyl-2-methoxyl group-5-
Acetamido aniline product requirement.
Embodiment 4
(1) mother liquid coming (i.e. m-acetamidoaniline and the chlorine of production N, N-diethyl m-acetamidoaniline is collected respectively
Ethane reacts the waste water producing containing ammonium chloride under ammonia effect) and washings, wherein washing water reuse produces in intermediate.Female
In liquid water, the mass percentage content of ammonium chloride is 20%, and COD is 23760mg/L, and colourity is 2000 times.
Mother liquid coming enters flocculation still, adds produced spent lye regulation pH to 7～8 in commercial production, under stirring condition
Being continuously added to polyacrylamide solution, the mass fraction of polyacrylamide solution is 0.2%, and dosage is mother liquid coming quality
0.1%, after continuous stirring 15min, natural subsidence 1h, filter pressing, be separately recovered intermediate and obtain precipitate I and treatment fluid I.
After measured, in treatment fluid I, COD is 20200mg/L, and colourity is 1640 times.
(2) treatment fluid I is transferred to oxidation trough, adds the abraum salt acid for adjusting pH of generation in production disperse orange 288 and, to 3～4, opens
Open UV, add H2O2, H2O2Dosage is treatment fluid I mass 0.3%, fully react 2h, carry out after filter pressing obtaining treatment fluid
Ⅱ。
After measured, in treatment fluid II, COD is 10320mg/L, and colourity is 1200 times.
(3) treatment fluid II enters acid adjustment still, add produce the abraum salt acid for adjusting pH that produces in disperse orange 288 to 1.0～
1.5, after regulation, solution enters decolouring still, adds activated carbon, and the dosage of activated carbon is the 0.5% for the treatment of fluid II mass, fully
After stirring 2h, destaining solution enters filter press plate, collects filtrate and saturated activity charcoal respectively.Saturated activity charcoal is through high temperature regeneration Posterior circle
Using, filtrate is treatment fluid III.
After measured, in treatment fluid III, COD is 2200mg/L, and colourity is 4 times.
(4) treatment fluid III enters and neutralizes still, adds ammonia regulation pH to 3～4, enters MVR equipment, concentrate after regulation
Crystallization, after machine separates by centrifugation, obtaining purity is 99.6%, the ammonia chloride crystal that color and luster is whiter.Crystalline mother solution is back to MVR and sets
Standby, further condensing crystallizing, collecting evaporation condensate is treatment fluid IV, treatment fluid IV achromaticity and clarification.
After measured, in treatment fluid IV, COD is 720mg/L, and colourity is 2 times.
(5) treatment fluid IV carries out BAF process, and aeration rate is 4.0mg/L, obtains treatment fluid V, warp after processing 9h
Measure, in treatment fluid V COD be 45mg/L, COD clearance be 93.75%, colourity is 1 times.
Treatment fluid V participates in the synthesis of N, N-diethyl m-acetamidoaniline, after acylated, ethylation reaction, in obtaining
Mesosome product, product purity is 97.8%, and yield is 99.0%, complies fully with N, N-diethyl m-acetamidoaniline product and wants
Ask.
Embodiment 5
(1) mother liquid coming (i.e. m-acetamidoaniline and the chlorine of production N, N-diethyl m-acetamidoaniline is collected respectively
Ethane reacts the waste water producing containing ammonium chloride under ammonia effect) and washings, wherein washing water reuse produces in intermediate.Female
In liquid water, the mass percentage content of ammonium chloride is 20%, and COD is 23760mg/L, and colourity is 2000 times.
Mother liquid coming enters flocculation still, adds produced spent lye regulation pH to 7～8 in commercial production, under stirring condition
Being continuously added to polyacrylamide solution, the mass fraction of polyacrylamide solution is 0.2%, and dosage is mother solution water quality
The 0.1% of amount, after continuous stirring 15min, natural subsidence 1h, filter pressing, it is separately recovered intermediate and obtains precipitate I and treatment fluid I.
After measured, in treatment fluid I, COD is 20200mg/L, and colourity is 1640 times.
(2) treatment fluid I is transferred to oxidation trough, adds the abraum salt acid for adjusting pH of generation in production disperse orange 288 and, to 1～3, opens
Open UV, add H2O2, H2O2Dosage is treatment fluid I mass 1.0%, fully react 4h, carry out after filter pressing obtaining treatment fluid
Ⅱ。
After measured, in treatment fluid II, COD is 13940mg/L, and colourity is 1260 times.
(3) treatment fluid II enters acid adjustment still, adds the abraum salt acid for adjusting pH of generation in production disperse orange 288 and, to 2～3, adjusts
After joint, solution enters decolouring still, adds activated carbon, and the dosage of activated carbon is the 0.6% for the treatment of fluid II mass, is sufficiently stirred for 4h
After, destaining solution enters filter press plate, collects filtrate and saturated activity charcoal respectively.Saturated activity charcoal uses through high temperature regeneration Posterior circle,
Filtrate is treatment fluid III.
After measured, in treatment fluid III, COD is 2680mg/L, and colourity is 5 times.
(4) treatment fluid III enters and neutralizes still, adds ammonia regulation pH to 6～8, enters MVR equipment, concentrate after regulation
Crystallization, after machine separates by centrifugation, obtaining purity is 99.1%, the ammonia chloride crystal that color and luster is whiter.Crystalline mother solution is back to MVR and sets
Standby, further condensing crystallizing, collecting evaporation condensate is treatment fluid IV, treatment fluid IV achromaticity and clarification.
After measured, in treatment fluid IV, COD is 810mg/L, and colourity is 2 times.
(5) treatment fluid IV carries out BAF process, and aeration rate is 4.5mg/L, obtains treatment fluid V, warp after processing 8h
Measure, in treatment fluid V COD be 48mg/L, COD clearance be 94.07%, colourity is 1 times.
Treatment fluid V participates in the synthesis of N, N-diethyl m-acetamidoaniline, after acylated, ethylation reaction, in obtaining
Mesosome product, product purity is 95.4%, and yield is 98.0%, and tetraethyl is 0.9%, complies fully with acetyl between N, N-diethyl
Amino aniline product requirement.
Comparative example 1
Compared with Example 1, other treatment conditions are constant, and the pH regulator in step (3) changes 7～8 into, then the throwing of activated carbon
Dosage need to increase to the 0.8% for the treatment of fluid II mass, and the colourity of guarantee gained treatment fluid III is less than 5 times.
Comparative example 2
Compared with Example 1, other treatment conditions are constant, and the pH regulator in step (3) changes 8～9 into, then the throwing of activated carbon
Dosage need to increase to the 1.0% for the treatment of fluid II mass, and the colourity of guarantee gained treatment fluid III is less than 5 times.
Comparative example 3
Compared with Example 1, the treatment conditions of step (1) are constant, in step (2), only open UV, do not add H2O2, then fill
Divide reaction 2h, after carrying out filter pressing, obtain treatment fluid II.In treatment fluid II, COD is 15200mg/L, and colourity is 1580 times, before and after process
COD and colourity are without significant change.
Comparative example 4
Compared with Example 1, the treatment conditions of step (1) are constant, in step (2), are not turned on UV, only add H2O2, H2O2
Dosage is treatment fluid I mass 0.1%, the most fully react 2h, carry out after filter pressing obtaining treatment fluid II.COD in treatment fluid II
For 13680mg/L, colourity is 1400 times, and before and after process, COD and colourity change are little, DeGrain.
Comparative example 5
Compared with Example 1, other treatment conditions are constant, and the activated carbon used in step (3) is regenerated carbon, regeneration
Mode is the microwave reclaiming method in hot recycling method, and concrete regeneration parameter is: frequency 300MHZ, temperature 550 DEG C, time 2h.Through again
Activated carbon-iodine adsorptive value >=750mg/g after life, methylene blue adsorptive value >=160mg/g, activated carbon loss rate 5%～10%.
In step (3), other treatment conditions are constant, and gained treatment fluid III analyzes colourity by the monitoring of online colourity monitor
It it is 3 times.
By comparative example 1～2, carry out adsorption bleaching in acid condition, the usage amount of adsorbent can be substantially reduced.
By comparative example 3～4, in step (2), use UV/H2O2Group technology aoxidizes, and the COD for the treatment of fluid and colourity can be made notable
Declining, and irradiate UV oxidation or hydrogen peroxide oxidation only with ultraviolet, effect is the most inconspicuous.Comparative example 5 uses regeneration activity
Charcoal, the decolorization adsorption effect of regenerated carbon and new activated carbon are without being clearly distinguished from, it is possible to significantly reduce activated carbon use cost with
And danger solid waste discharge.
Claims (9)
1. the recycling processing method of an aniline intermediate production waste water, it is characterised in that comprise the steps:
(1) flocculation: categorised collection also adjusts the pH value of waste water to 7～12, adds flocculant and flocculates, after filtration precipitate
I and treatment fluid I；
(2) oxidation: regulation treatment fluid I pH value to 1～6, add oxidant, fully oxidized after treatment fluid II；
(3) adsorption bleaching: the pH value of regulation treatment fluid II, to 1～6, adds adsorbent, fully separates to obtain treatment fluid III after absorption；
(4) neutralization, condensing crystallizing: the pH value of regulation treatment fluid III, to 3～8, enters enrichment facility and carries out condensing crystallizing, separated
Rear acquisition sodium chloride or chloride solid, mother solution returns enrichment facility and continues condensing crystallizing, and collecting condensed fluid is treatment fluid IV；
(5) biological treatment: obtain treatment fluid V after treatment fluid IV carries out BAF process, i.e. completes to process.
2. aniline intermediate as claimed in claim 1 produces the recycling processing method of waste water, it is characterised in that step
(1), in, described flocculant is aluminum sulfate, aluminum chloride, ferrous sulfate, iron chloride, aluminium polychlorid, polyaluminium sulfate, polymerised sulphur
At least one in acid ferrum and polyacrylamide, the mass fraction of flocculant aqueous solution is 0.05～0.5%, adding of flocculant
Amount is the 0.02～2% of wastewater quality.
3. aniline intermediate as claimed in claim 1 produces the recycling processing method of waste water, it is characterised in that step
(1), in, produced spent lye or deposed ammonia in commercial production is used to regulate the pH value of waste water.
4. aniline intermediate as claimed in claim 1 produces the recycling processing method of waste water, it is characterised in that step
(2) in, the dosage of described oxidant is the 0.05～1.0% for the treatment of fluid I mass, and the time of described oxidation is 0.5～4h.
5. aniline intermediate as claimed in claim 1 produces the recycling processing method of waste water, it is characterised in that step
(2), in, the mode of described oxidation is UV/H2O2Oxidation, H used2O2Mass fraction is 25～50%, and uviol lamp used is low pressure
Mercury lamp, power is 8～120W.
6. aniline intermediate as claimed in claim 1 produces the recycling processing method of waste water, it is characterised in that step
(3) in, described adsorbent is activated carbon, and the dosage of adsorbent is the 0.1～0.3% for the treatment of fluid II mass, and adsorption time is
0.5～2h.
7. aniline intermediate as claimed in claim 1 produces the recycling processing method of waste water, it is characterised in that step
(2) and in (3), produced waste hydrochloric acid in commercial production is used to regulate pH value.
8. aniline intermediate as claimed in claim 1 produces the recycling processing method of waste water, it is characterised in that step
(5), in, in described BAF, microorganism at least includes that raw branch moves glue bacterium, wax printing fabric, middle Escherichia, big
Enterobacteria, aerobacteria, excrement aerogenesis paracolon, unwrapping wire shape Nocard's bacillus, Bacillus subtillis, alcaligenes faecalis, nitrification bar
Bacterium, Nitrosomonas, ball antibacterial, denitrification Thiobacillus, Pseudomonas alcaligenes, acetobacter, cause yellow pseudomonas, gentleness
One in Aeromonas and Aeromonas media.
9. the aniline intermediate as described in claim 1 or 8 produces the recycling processing method of waste water, it is characterised in that institute
Stating microorganism in BAF to cultivate under treatment fluid IV environmental condition and screen, actual conditions state modulator is
Water temperature 25～38 DEG C, pH 6～8, activated sludge concentration 2～5g/L, dissolved oxygen concentration 2.0～4.5mg/L.
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| CN109809434A (en) * | 2019-03-07 | 2019-05-28 | 安徽华星化工有限公司 | A method of production refining industrial salt is recycled based on Cupric sulfate abraum salt |
| CN112093946A (en) * | 2020-08-25 | 2020-12-18 | 中钢集团鞍山热能研究院有限公司 | Electrochemical enhanced pretreatment method for fluorenone wastewater |
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| CN113104865A (en) * | 2019-12-12 | 2021-07-13 | 林齐坤 | Method for treating refined mother liquor of vat blue RSN |
| CN113104865B (en) * | 2019-12-12 | 2023-08-22 | 酒泉宇鹏化工科技有限公司 | Treatment method of vat blue RSN refining mother liquor |
| CN112093946A (en) * | 2020-08-25 | 2020-12-18 | 中钢集团鞍山热能研究院有限公司 | Electrochemical enhanced pretreatment method for fluorenone wastewater |
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Application publication date: 20161130 |