CN107117749A - A kind of para-aminophenol produces the recycling processing method of waste water - Google Patents
A kind of para-aminophenol produces the recycling processing method of waste water Download PDFInfo
- Publication number
- CN107117749A CN107117749A CN201710350051.0A CN201710350051A CN107117749A CN 107117749 A CN107117749 A CN 107117749A CN 201710350051 A CN201710350051 A CN 201710350051A CN 107117749 A CN107117749 A CN 107117749A
- Authority
- CN
- China
- Prior art keywords
- nitrophenol
- waste water
- para
- aminophenol
- resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000002351 wastewater Substances 0.000 title claims abstract description 93
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000004064 recycling Methods 0.000 title claims abstract description 25
- 238000003672 processing method Methods 0.000 title claims abstract description 17
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims abstract description 90
- 239000011347 resin Substances 0.000 claims abstract description 77
- 229920005989 resin Polymers 0.000 claims abstract description 77
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 72
- 238000001179 sorption measurement Methods 0.000 claims abstract description 59
- 238000011084 recovery Methods 0.000 claims abstract description 36
- 239000000706 filtrate Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000005406 washing Methods 0.000 claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 239000000701 coagulant Substances 0.000 claims abstract description 9
- 238000012805 post-processing Methods 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 238000005345 coagulation Methods 0.000 claims abstract description 3
- 230000015271 coagulation Effects 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 92
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 26
- 238000007254 oxidation reaction Methods 0.000 claims description 23
- 230000003197 catalytic effect Effects 0.000 claims description 22
- 230000003647 oxidation Effects 0.000 claims description 22
- 238000010521 absorption reaction Methods 0.000 claims description 17
- 238000003795 desorption Methods 0.000 claims description 15
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 14
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 239000003456 ion exchange resin Substances 0.000 claims description 13
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 13
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000005868 electrolysis reaction Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 claims description 8
- 238000005342 ion exchange Methods 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 8
- 239000007800 oxidant agent Substances 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- 238000005904 alkaline hydrolysis reaction Methods 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 239000002250 absorbent Substances 0.000 claims description 4
- 230000002745 absorbent Effects 0.000 claims description 4
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 230000020477 pH reduction Effects 0.000 claims description 3
- 238000007539 photo-oxidation reaction Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000004155 Chlorine dioxide Substances 0.000 claims description 2
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 2
- 239000003729 cation exchange resin Substances 0.000 claims description 2
- 235000019398 chlorine dioxide Nutrition 0.000 claims description 2
- 238000007146 photocatalysis Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 claims description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 10
- 238000005189 flocculation Methods 0.000 abstract description 8
- 230000016615 flocculation Effects 0.000 abstract description 8
- 229910052742 iron Inorganic materials 0.000 description 49
- -1 hydroxybenzene amine Chemical class 0.000 description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 18
- 239000005416 organic matter Substances 0.000 description 11
- 239000012528 membrane Substances 0.000 description 10
- 238000012545 processing Methods 0.000 description 10
- 238000007792 addition Methods 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000006386 neutralization reaction Methods 0.000 description 5
- 229960003742 phenol Drugs 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 230000033228 biological regulation Effects 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- 239000004568 cement Substances 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000010612 desalination reaction Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 2
- FFXSKLNKKMNFDZ-UHFFFAOYSA-N iron 4-nitrophenol Chemical compound [Fe].[N+](=O)([O-])C1=CC=C(C=C1)O FFXSKLNKKMNFDZ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- OEHNVKBOQOXOJN-UHFFFAOYSA-N 2-(4-nitrophenyl)phenol Chemical compound OC1=CC=CC=C1C1=CC=C([N+]([O-])=O)C=C1 OEHNVKBOQOXOJN-UHFFFAOYSA-N 0.000 description 1
- JSTCPNFNKICNNO-UHFFFAOYSA-N 4-nitrosophenol Chemical compound OC1=CC=C(N=O)C=C1 JSTCPNFNKICNNO-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DFPAKSUCGFBDDF-UHFFFAOYSA-N Nicotinamide Chemical compound NC(=O)C1=CC=CN=C1 DFPAKSUCGFBDDF-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 229930003451 Vitamin B1 Natural products 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229920001429 chelating resin Polymers 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- UKJLNMAFNRKWGR-UHFFFAOYSA-N cyclohexatrienamine Chemical group NC1=CC=C=C[CH]1 UKJLNMAFNRKWGR-UHFFFAOYSA-N 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- UWQSRFYTPSKUPO-UHFFFAOYSA-N iron 2-nitrophenol Chemical compound [Fe].[N+](=O)([O-])C1=C(C=CC=C1)O UWQSRFYTPSKUPO-UHFFFAOYSA-N 0.000 description 1
- 238000005360 mashing Methods 0.000 description 1
- 229960003966 nicotinamide Drugs 0.000 description 1
- 235000005152 nicotinamide Nutrition 0.000 description 1
- 239000011570 nicotinamide Substances 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 229960005489 paracetamol Drugs 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229960003495 thiamine Drugs 0.000 description 1
- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 description 1
- 239000011691 vitamin B1 Substances 0.000 description 1
- 235000010374 vitamin B1 Nutrition 0.000 description 1
- 239000002699 waste material Substances 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
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
-
- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic 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
- C02F1/30—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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
-
- 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
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
-
- 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
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F2001/5218—Crystallization
-
- 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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
Abstract
The invention discloses the recycling processing method that a kind of para-aminophenol produces waste water, comprise the following steps：(1) pre-process：Para-aminophenol production waste water is adjusted to neutral or meta-alkalescence, coagulant is added and carries out coagulation, filtering obtains filtrate I and filter residue；(2) p-nitrophenol one-level is reclaimed：By filter residue hot wash, washing water outlet is adjusted to acidity and cooled down, filtrate II and p-nitrophenol crystal is filtrated to get, reclaim p-nitrophenol, filtrate II recycled is in washing filter residue；(3) p-nitrophenol secondary recovery：Filtrate I pH is adjusted to 0.5~4, p-nitrophenol is reclaimed using resin adsorption；(4) post-process：Post processing is carried out to resin adsorption water outlet and reclaims inorganic salts.The handling process of the present invention is served as theme with " neutralize flocculation p-nitrophenol one-level and reclaim the post processing of p-nitrophenol secondary recovery ", and the recycling for realizing waste water is recycled and realized " zero-emission ", significantly reduces secondary pollution.
Description
Technical field
The recycling treatment of waste water is produced the present invention relates to field of industrial waste water treatment, more particularly to a kind of para-aminophenol
Method.
Background technology
Para-aminophenol also known as para hydroxybenzene amine, PAP, abbreviation PAP, be one kind be widely used in medicine, fuel and
The important organic intermediate of organic synthesis.In medical industry, para-aminophenol is mainly used in synthesizing medical paracetamol, ANTU
Ketone, vitamin B1, compound niacinamide etc., have application in rubber, fuel, feed, oil and photographic industry.
Para-aminophenol is initially using p-Nitrosophenol as raw material, using the method reduced in acid medium with glass putty
It is made, the method with iron powder reducing p-nitrophenol or para-nitrochloro-benzene is changed to later, so far still for countries in the world institute extensively
Using.The technique that p-nitrophenol iron powder reducing method prepares para-aminophenol is：Sodium hydroxide is added into paranitrochlorobenzene,
Pressurized hydrolysis is carried out under alkalescence condition, after being then acidified with hydrochloric acid be made p-nitrophenol, then by clear water be placed in reduction pot in plus
Heat adds reducing agent iron powder and hydrochloric acid to 98 DEG C, adds p-nitrophenol, and reaction filters off iron cement after terminating, in 98 DEG C of additions
Sodium pyrosulfite, is cooled to 55~60 DEG C, is dried after recrystallization and can obtain the pure crystalline substance of para-aminophenol.Therefore, to nitro
Phenol iron powder reducing method is prepared in the waste water produced in the technical process of para-aminophenol, contains substantial amounts of p-nitrophenol, iron
Ion, sodium chloride salt, while the features such as there is big acidity, high COD and high TOC.
The recovery method of the phenol compound of Pyrogentisinic Acid's class waste water is mainly resin adsorption, but the resinous type used is poor
It is different larger.Publication No. CN102910757A Chinese patent literature discloses a kind of o-nitrophenol production wastewater treatment work
Skill, is pre-processed to waste water first, is entered back into after resin absorbing column absorption, resin adsorption saturation, using NaOH solution to tree
Fat is desorbed, and high concentration desorption liquid is acidified with acid rear recyclable o-nitrophenol；Light concentration desorption liquid is covered for making when being desorbed
With, the o-nitrophenol being recovered to after distilation, can hydrogenation catalyst be used to produce o-aminophenol；Gained adsorption treatment
Waste water afterwards can turn into qualified salt solution after ozone oxidation, neutralization, decolouring.But this method is to the adjacent nitro in waste water
The rate of recovery of phenol is relatively low.
At present, p-nitrophenol iron powder reducing method prepare p-aminophenyl production waste water processing method be generally：(1) it is catalyzed
Oxidative degradation technology；(2) resin adsorption-evaporative desalination technology.Wherein catalyzing oxidizing degrading technology can not reclaim useful in waste water
Material, and need to add oxidant, cost is higher；Resin adsorption-evaporative desalination technology can not reclaim in iron cement to nitro
Phenol, p-nitrophenol reclaims not thorough, and evaporation energy consumption is high, and obtained salt is dangerous waste.
The content of the invention
The present invention provides the recycling processing method that a kind of para-aminophenol produces waste water, by with " neutralization flocculation-resin
Iron cement and right in the handling process that absorption-photochemical catalytic oxidation-resin adsorption-electrolysis with ion-exchange film " is served as theme, separation and recovery waste water
Nitrophenol, and by film electrolytic preparation chlorine, hydrogen and caustic soda, realize " zero-emission " and para-aminophenol production of waste water
The recycling treatment of waste water.
A kind of para-aminophenol produces the recycling processing method of waste water, comprises the following steps：
(1) pre-process：Para-aminophenol production waste water is adjusted to neutral or meta-alkalescence, coagulant is added and carries out coagulation,
Filtering, obtains filtrate I and filter residue；
Described para-aminophenol production waste water is that paranitrochlorobenzene obtains p-nitrophenol by alkaline hydrolysis, acidification technique,
The waste water produced during iron powder reducing prepares para-aminophenol is carried out again；
(2) p-nitrophenol one-level is reclaimed：By filter residue hot wash, washing water outlet is adjusted to acidity and cooled down, mistake
Filter obtains filtrate II and p-nitrophenol crystal, reclaims p-nitrophenol, filtrate II recycled is in washing filter residue；
(3) p-nitrophenol secondary recovery：Filtrate I pH is adjusted to 0.5~4, reclaimed using resin adsorption to nitro
Phenol；
(4) post-process：Post processing is carried out to resin adsorption water outlet and reclaims inorganic salts.
Paranitrochlorobenzene obtains p-nitrophenol, then passes through iron powder reducing by p-nitrophenol by alkaline hydrolysis, acidification technique
The waste water that method is produced during preparing p-aminophenyl phenolic product, containing substantial amounts of p-nitrophenol, hydrogen ion and iron ion,
Wherein p-nitrophenol concentration is 500~5000mg/L, [H+] concentration be 0.1~1mol/L, iron concentration be 200~
COD is that 5000~20000mg/L, TOC are 1000~3000mg/ in 2000mg/L, sodium chloride salt content 5%~25%, waste water
L。
Contain substantial amounts of iron ion in para-aminophenol production waste water, spent acid is in yellow, in step (1) by waste water adjust to
Neutral or meta-alkalescence, adds iron ion after coagulant and flocculates, be filtered to remove iron ion, obtain filtrate I and filter residue.
Preferably, in step (1), the pH that para-aminophenol is produced into waste water is adjusted to 7~9.The iron in the range of the pH
Ion can be hydrolyzed well, preferably be flocculated in the presence of coagulant, while pH controls are 7~9, can subtract as far as possible
The cost of few follow-up acid adjustment.
Preferably, described coagulant is Powdered Activated Carbon and/or aluminium polychloride, waste water is produced with para-aminophenol
Quality on the basis of, the addition of coagulant is 0.1~0.5%.
It is mainly the flocculate of iron ion in filter residue, also containing part p-nitrophenol, in order to improve p-nitrophenol
The rate of recovery, step (2) is reclaimed to the p-nitrophenol in filter residue.Preferably, in step (2), using hot wash filter residue
Method be：Filter residue is beaten for 50~100 DEG C of hot water with temperature, the filter after washing water outlet and washing is filtrated to get
Slag.
It is further preferred that the consumption of hot water is 30~60 times of filter residue quality.
Filter residue impurity after washing is less, is easy to subsequent recovery iron.
It is further preferred that the pH for washing water outlet is adjusted to 0.5~4,5~20 DEG C are cooled to, is stood still for crystals.To nitro
Solubility of the phenol in pH=0.5~4 in water is smaller, crystallizable at 5~20 DEG C to separate out, while other separated out
Material is less, and the p-nitrophenol purity being filtrated to get is higher.
The p-nitrophenol reclaimed from filter residue accounts for 20~30% of p-nitrophenol gross mass in waste water.
It is further preferred that p-nitrophenol crystal is recrystallized, production is back to.
After flocculation filtration, in the filtrate I obtained in step (1) containing most p-nitrophenol, a small amount of iron from
Son and other a small amount of organic matters, step (3) carry out secondary recovery by resin adsorption to the p-nitrophenol in filtrate I.
Preferably, in step (3), the macroporous absorbent resin that the resin that resin adsorption is used is modified for phenolic hydroxyl group.
There is the macroporous absorbent resin of phenolic hydroxyl group modification preferable selective absorption to act on to p-nitrophenol, and iron from
The presence of son does not influence its adsorption effect.
It is further preferred that resin adsorption multiple is 10~100BV, the rate of adsorption is 0.5~4BV/h.
It is further preferred that described macroporous absorbent resin is HYA-103 types or HYA-106 type resins.
After resin adsorption, the p-nitrophenol in filtrate I is adsorbed completely substantially, in resin adsorption water outlet COD and
TOC is greatly reduced.
Reused after the resin desorption of adsorption saturation, substantial amounts of p-nitrophenol is contained in desorption liquid, can by crystallization
Reclaim p-nitrophenol therein.Use 40~60 DEG C, mass fraction resin is desorbed for 4~6% sig water, will be de-
The pH of attached liquid is adjusted to 0.5~4 and is cooled to 5~20 DEG C, is filtrated to get filtrate II I and p-nitrophenol crystal, is reclaimed to nitre
Base phenol, filtrate II I recycleds are in configuration sig water desorption resin.
The p-nitrophenol of secondary recovery accounts for 70~80% of p-nitrophenol gross mass in waste water.
Reclaimed by one-level and secondary recovery, the overall recovery of p-nitrophenol reaches more than 95%, and the rate of recovery is higher.
Containing a large amount of inorganic salts, iron ion and other a small amount of organic matters in resin adsorption water outlet, post-treated removal its
In iron ion and organic matter, reclaim inorganic salts therein, recycling further carried out to waste water.
Preferably, described post processing includes：
Resin adsorption water outlet is carried out ultraviolet catalytic oxidation by (4-1), and the power of uviol lamp is 1~15kW, and ultraviolet light is urged
The reaction time for changing oxidation is 10~200min；It is further preferred that the reaction time of ultraviolet catalytic oxidation be 20~
60min；
Photooxidation water outlet is passed through ion exchange resin by (4-2), and the absorption multiple of ion exchange resin is 20~2000BV,
The rate of adsorption is 0.5~5BV/h；
Ion exchange resin absorption water outlet is carried out electrolysis with ion-exchange film by (4-3), and hydrogen, chlorine and caustic soda is made.
In the resin adsorption water outlet of step (3) contain a small amount of iron ion, iron ion as ultraviolet catalytic oxidation catalysis
Residual organic matter in agent, and ultraviolet cooperating catalytic degradation resin adsorption water outlet.It will can be given up by ultraviolet catalytic oxidation
The TOC of water is reduced to below 10mg/L, meets the water quality requirement of electrolysis with ion-exchange film.
Ultraviolet catalytic oxidation uses the ultraviolet catalytic reactor of super high power in step (4-1), and uviol lamp power can
Select 1~15kw.
It is further preferred that in step (4-1), ultraviolet catalytic is carried out again after adding oxidant into resin adsorption water outlet
Oxidation.
It is further preferred that described oxidant is the one or more in hydrogen peroxide, sodium hypochlorite and chlorine dioxide；With
On the basis of the quality of resin adsorption water outlet, oxidant dosage is 0.1~2%.
In order to further remove the iron ion in oxidation water outlet, photooxidation water outlet is passed through amberlite by step (4-2)
Fat carries out the organic matter of Adsorption iron ion therein and residual.
Preferably, described ion exchange resin is sodium form cationic ion-exchange resin.
After ion exchange resin treatment, iron ion is down to below 0.1mg/L in ion exchange resin water outlet, meet from
The water quality requirement of sub- film electrolysis.
Sodium ion, chlorion and hydrogen ion in electrolysis with ion-exchange film processing by step (4-3), waste water are recycled,
Realize the further recycling of waste water.
Compared with prior art, beneficial effects of the present invention are：
The present invention handling process with " neutralize flocculation-p-nitrophenol one-level recovery-p-nitrophenol secondary recovery-after
Processing " is served as theme, and the recycling for realizing waste water is recycled and realized " zero-emission ", significantly reduces secondary pollution；
The process operations of the present invention are simple, mild condition, and industrial applications can be achieved.
Brief description of the drawings
Fig. 1 is the process chart for the recycling processing method that para-aminophenol of the present invention produces waste water.
Embodiment
Embodiment 1
Waste water is that paranitrochlorobenzene prepares p-nitrophenol by alkaline hydrolysis, acidifying, crystallization and obtained pair by iron powder reducing again
Produced during amino-phenol product, waste water is yellow, TOC is 2033mg/L, [H+] it is 0.4mol/L, iron concentration is
924mg/L, the concentration of p-nitrophenol is 2000mg/L.
(1) add sodium hydroxide solution (30w.t.%) to p-nitrophenol waste water and carry out neutralization flocculation, adjust wastewater pH
It is worth for 8.5, iron concentration is reduced to 18mg/L in 0.1% Powdered Activated Carbon, stirring, flocculation, filtering, filtrate is added, and gives up
Water TOC is down to 1553mg/L, and clearance is 30.9%, and the filter residue of generation accounts for the 1.38% of wastewater quality；
(2) utilize (50 times of solid waste quality) (60 DEG C) hot water to be beaten filter residue to filter, recycle concentrated hydrochloric acid (36w.t.%)
The regulation of filter liquor pH value will be beaten to 1.0, and be cooled to 20 DEG C, standing, crystallization filtering, recovery p-nitrophenol, the rate of recovery
For 23.6%, filtrate is applied mechanically, and continues on for the dissolving washing of filter cake；
(3) pH of the filtrate obtained in step (1) is adjusted to 1.7 using concentrated hydrochloric acid (36w.t.%), then used
Organic matter in HYA-103 resin adsorption waste water, resin adsorption multiple is 50BV, and the rate of adsorption is 1BV/h, resin adsorption water outlet
TOC be 80mg/L；Waste water remaining in resin is excluded after adsorption saturation, and using 1~2BV clear water washing resin, then
It is desorbed using 1~2BV 50 DEG C of sodium hydroxide solution (5w.t.%)；Desorption liquid pH value is adjusted to 1.0, is cooled to
20 DEG C, there is yellow crystals precipitation, main component is p-nitrophenol, filter, reclaim p-nitrophenol, filtrate continues on for preparing
Sig water, circulates the desorption for resin；Resin is recycled after regeneration；The rate of recovery of this step p-nitrophenol is about
72.46%, the overall recovery of p-nitrophenol is 96.06% in waste water after step (2) and (3)；
(4) hydrogen peroxide (27.5w.t.%) added in the resin adsorption water outlet into step (3), the addition of hydrogen peroxide
For the 1% of resin adsorption effluent characteristics, photochemical catalytic oxidation technique is carried out with remaining organic matter in degradation water, the power of uviol lamp is
12kw, reacts 1h；TOC is down to 5mg/L after reaction, and iron concentration is 18mg/L；
(5) the photochemical catalytic oxidation water outlet in step (4) is subjected to absorption by sodium form ion exchange resin and removes iron, absorption speed
Rate is 1BV/h, and it is 0.046ppm that absorption, which removes iron concentration in iron water outlet, is reached into ionic membrane requirement；
(6) water outlet after step (5) processing carries out electrolysis with ion-exchange film, prepares hydrogen, chlorine and caustic soda, passes through waste water
Recycling is obtained after crossing processing.
Recyclable 1.932kg p-nitrophenol in 1 ton of waste water, the purity of p-nitrophenol is 99.2%.
Embodiment 2
Waste water is that paranitrochlorobenzene prepares p-nitrophenol by alkaline hydrolysis, acidifying, crystallization and obtained pair by iron powder reducing again
Produced during amino-phenol product, waste water is yellow, TOC is 2420mg/L, [H+] it is 0.24mol/L, iron concentration
For 864mg/L, the concentration of p-nitrophenol is 2109mg/L.
(1) add sodium hydroxide solution (30w.t.%) to p-nitrophenol waste water and carry out neutralization flocculation, adjust wastewater pH
It is worth for 8.8, iron concentration is reduced to 15mg/L in 0.2% Powdered Activated Carbon, stirring, flocculation, filtering, filtrate is added, and gives up
Water TOC is down to 1672.22mg/L, and clearance is 30.9%, produce filter residue and account for the 1.41% of wastewater quality；
(2) utilize (50 times of solid waste quality) (60 DEG C) hot water to be beaten filter residue to filter, recycle concentrated hydrochloric acid (36w.t.%)
The regulation of filter liquor pH value will be beaten to 1.0, and be cooled to 20 DEG C, standing, crystallization filtering, recovery p-nitrophenol, the rate of recovery
For 25%, filtrate is applied mechanically, and continues on for the dissolving washing of filter cake；
(3) pH of the filtrate obtained in step (1) is adjusted to 1.7 using concentrated hydrochloric acid (36w.t.%), then used
Organic matter in HYA-106 resin adsorption waste water, resin adsorption multiple is 50BV, and the rate of adsorption is 1BV/h, resin adsorption water outlet
TOC be 70mg/L,；Waste water remaining in resin is excluded after adsorption saturation, and using 1~2BV clear water washing resin, then
It is desorbed using 1~2BV 50 DEG C of sodium hydroxide solution (5w.t.%)；Desorption liquid pH value is adjusted to 1.0, is cooled to
20 DEG C, there is yellow crystals precipitation, main component is p-nitrophenol, filter, reclaim p-nitrophenol, filtrate continues on for preparing
Sig water, circulates the desorption for resin；Resin is recycled after regeneration；The rate of recovery of this step p-nitrophenol is about
72%, the overall recovery of p-nitrophenol is 97% in waste water after step (2) and (3)；
(4) hydrogen peroxide (27.5w.t.%) added in the resin adsorption water outlet into step (3), the addition of hydrogen peroxide
For the 1.5% of resin adsorption effluent characteristics, photochemical catalytic oxidation technique is carried out with remaining organic matter in degradation water, photocatalysis is used
5kw uviol lamp, reacts 2.5h；TOC is down to 6mg/L after reaction, and iron concentration is 20mg/L；
(5) the photochemical catalytic oxidation water outlet in step (4) is subjected to absorption by sodium form ion exchange resin and removes iron, absorption speed
1BV/h is spent, it is 0.046mg/L that absorption, which removes iron concentration in iron water outlet, is reached into ionic membrane requirement；
(6) water outlet after step (5) processing carries out electrolysis with ion-exchange film, prepares hydrogen, chlorine and caustic soda, passes through waste water
Recycling is obtained after crossing processing.
Recyclable 2.045kg p-nitrophenols in 1 ton of waste water, the purity of p-nitrophenol is 99.0%.
Embodiment 3
Waste water is that paranitrochlorobenzene prepares p-nitrophenol by alkaline hydrolysis, acidifying, crystallization and obtained pair by iron powder reducing again
Produced during amino-phenol product, waste water is yellow, TOC is 1862mg/L, [H+] it is 0.52mol/L, iron concentration
For 986mg/L, the concentration of p-nitrophenol is 1833mg/L.
(1) add sodium hydroxide solution (30w.t.%) to p-nitrophenol waste water and carry out neutralization flocculation, adjust wastewater pH
It is worth for 9, iron concentration is reduced to 15mg/L, waste water in 0.1% Powdered Activated Carbon, stirring, flocculation, filtering, filtrate is added
TOC is down to 1340.64mg/L, and clearance is 28%, produce filter residue and account for the 1.39% of wastewater quality；
(2) utilize (50 times of solid waste quality) (60 DEG C) hot water to be beaten filter residue to filter, recycle concentrated hydrochloric acid (36w.t.%)
The regulation of filter liquor pH value will be beaten to 1.0, and be cooled to 20 DEG C, standing, crystallization filtering, recovery p-nitrophenol, the rate of recovery
For 24.83%, filtrate is applied mechanically, and continues on for the dissolving washing of filter cake；
(3) pH of the filtrate obtained in step (1) is adjusted to 1.7 using concentrated hydrochloric acid (36w.t.%), then used
Organic matter in HYA-103 resin adsorption waste water, resin adsorption multiple is 50BV, and the rate of adsorption is 1BV/h, resin adsorption water outlet
TOC be 32mg/L,；Waste water remaining in resin is excluded after adsorption saturation, and using 1~2BV clear water washing resin, then
It is desorbed using 1~2BV 50 DEG C of sodium hydroxide solution (5w.t.%)；Desorption liquid pH value is adjusted to 1.0, is cooled to
20 DEG C, there is yellow crystals precipitation, main component is p-nitrophenol, filter, reclaim p-nitrophenol, filtrate continues on for preparing
Sig water, circulates the desorption for resin；Resin is recycled after regeneration；The rate of recovery of this step p-nitrophenol is about
70.28%, the overall recovery of p-nitrophenol is 95.11% in waste water after step (2) and (3)；
(4) hydrogen peroxide (27.5w.t.%) added in the resin adsorption water outlet into step (3), the addition of hydrogen peroxide
For the 1% of resin adsorption effluent characteristics, photochemical catalytic oxidation technique is carried out with remaining organic matter in degradation water, using the ultraviolet of 15kw
Light irradiation reacts 50min；TOC is down to 4.2mg/L after reaction, and iron concentration is 14.2mg/L；
(5) the photochemical catalytic oxidation water outlet in step (4) is subjected to absorption by sodium form ion exchange resin and removes iron, absorption speed
Spend for 1BV/h, it is 0.062mg/L that absorption, which removes iron concentration in iron water outlet, is reached into ionic membrane requirement；
(6) water outlet after step (5) processing carries out electrolysis with ion-exchange film, prepares hydrogen, chlorine and caustic soda, passes through waste water
Recycling is obtained after crossing processing.
Recyclable 1.743kg p-nitrophenols in 1 ton of waste water, the purity of p-nitrophenol is 99.5%.
Embodiment 4
Compared with Example 1, difference is：
Regulation pH value of waste water is to be added without activated carbon powder after 8.5 in step (1), is filtered after stirring, iron ion is dense in filtrate
Degree is reduced to 22mg/L, and waste water TOC is down to 1703mg/L, and clearance is 16.29%, and the filter residue of generation accounts for wastewater quality
1.01%；
After step (2), the rate of recovery of p-nitrophenol is 18.5%；The rate of recovery of p-nitrophenol in step (3)
For 77.0%, the overall recovery of p-nitrophenol is 95.5%.
After step (4) and (5) processing, TOC is down to 7mg/L, and iron concentration is 0.054mg/L, and reaching will into ionic membrane
Ask；
Recyclable 1.904kg p-nitrophenol in 1 ton of waste water, the purity of p-nitrophenol is 99.0%.
Embodiment 5
Compared with Example 1, difference is：
Iron concentration in the activated carbon and 0.2% aluminium polychloride of addition 0.3%, obtained filtrate in step (1)
12mg/L is reduced to, waste water TOC is down to 1200mg/L, and clearance is 40%, and the filter residue of generation accounts for the 1.87% of wastewater quality；
After step (2), the rate of recovery of p-nitrophenol is 28.5%；The rate of recovery of p-nitrophenol in step (3)
For 70.5%, the overall recovery of p-nitrophenol is 99.0%.
After step (4) and (5) processing, TOC is down to 4mg/L, and iron concentration is 0.018mg/L, and reaching will into ionic membrane
Ask；
Recyclable 1.974kg p-nitrophenol in 1 ton of waste water, the purity of p-nitrophenol is 98.4%.
Embodiment 6
Compared with Example 1, difference is：
In step (2), filter residue is beaten with 30 times of 80 DEG C of hot water of solid waste quality and filtered, concentrated hydrochloric acid is recycled
(36w.t.%) adjusts mashing filter liquor pH value to 4.0, and is cooled to 5 DEG C, standing, crystallization filtering, recovery p-nitrophenyl
Phenol, the rate of recovery is 24.6%,
In step (3), the pH of the filtrate obtained in step (1) is adjusted to 0.5, then using HYA-103 resin adsorptions
Organic matter in waste water, resin adsorption multiple is 100BV, and the rate of adsorption is 1BV/h, and the TOC of resin adsorption water outlet is 119mg/
L；Resin desorption condition is constant, and desorption liquid pH value is adjusted into 4.0, is cooled to 5 DEG C, and the rate of recovery of this step p-nitrophenol is about
For 73.95%, the overall recovery of p-nitrophenol is 98.55% in waste water after step (2) and (3)；
Other steps are constant, finally measure, recyclable 1.965kg p-nitrophenol in 1 ton of waste water, p-nitrophenol
Purity is 98.1%.
Comparative example 1
Compared with Example 1, (1)~(3) are identical, and difference is：
(4) hydrogen peroxide (27.5w.t.%) added in the resin adsorption water outlet into step (3), the addition of hydrogen peroxide
For the 2% of resin adsorption effluent characteristics, photochemical catalytic oxidation technique is carried out with remaining organic matter in degradation water, using the ultraviolet of 500w
Light irradiation reacts 1h；TOC is down to 15mg/L after reaction, and iron concentration is 18mg/L.
After being handled by (1)~(4), TOC concentration is 15mg/L in waste water, and iron concentration is 18mg/L, is not reached
To the requirement for entering ionic membrane.
Also find out from comparative example 1, during ultraviolet catalytic oxidation, too low uv power catalysis can not be removed effectively
TOC in waste water.
Comparative example 2
Compared with Example 1, difference is that direct sodium form ion of crossing is handed over without the photochemical catalytic oxidation of (4) step
Change resin and carry out absorption except iron, TOC concentration is 80mg/L in water outlet, and iron concentration is 18mg/L, is not reaching into ionic membrane
Requirement.
When can be seen that from comparative example 2 without photochemical catalytic oxidation, effluent quality is not good, is not reaching into ionic membrane
Requirement.
Comparative example 3
Compared with Example 1, difference is：
(4) hydrogen peroxide (27.5w.t.%) added in the resin adsorption water outlet into step (3), the addition of hydrogen peroxide
For the 5% of resin adsorption effluent characteristics, stirring reaction 1h；TOC is down to 25mg/L after reaction, and iron concentration is 17mg/L.
After being handled by (1)~(4), TOC concentration is 25mg/L in waste water, and iron concentration is 17mg/L, is not reached
To the requirement for entering ionic membrane.
As can be seen that when substituting photochemical catalytic oxidation with hydrogen peroxide oxidation, effluent quality is not good, does not reach from comparative example 3
To the requirement for entering ionic membrane.
Technical scheme and beneficial effect are described in detail embodiment described above, it should be understood that
The specific embodiment of the present invention is the foregoing is only, is not intended to limit the invention, it is all to be done in the spirit of the present invention
Any modification, supplement and equivalent substitution etc., should be included in the scope of the protection.
Claims (10)
1. a kind of para-aminophenol produces the recycling processing method of waste water, it is characterised in that comprise the following steps：
(1) pre-process：Para-aminophenol production waste water is adjusted to neutral or meta-alkalescence, coagulant is added and carries out coagulation, filter,
Obtain filtrate I and filter residue；
Described para-aminophenol production waste water is that paranitrochlorobenzene obtains p-nitrophenol, then entered by alkaline hydrolysis, acidification technique
The waste water that row iron powder reducing is produced during preparing para-aminophenol；
(2) p-nitrophenol one-level is reclaimed：By filter residue hot wash, washing water outlet is adjusted to acidity and cooled down, is filtered
To filtrate II and p-nitrophenol crystal, p-nitrophenol is reclaimed, filtrate II recycled is in washing filter residue；
(3) p-nitrophenol secondary recovery：Filtrate I pH is adjusted to 0.5~4, p-nitrophenol is reclaimed using resin adsorption；
(4) post-process：Post processing is carried out to resin adsorption water outlet and reclaims inorganic salts.
2. para-aminophenol according to claim 1 produces the recycling processing method of waste water, it is characterised in that step
(1) in, the pH that para-aminophenol is produced into waste water is adjusted to 7~9.
3. para-aminophenol according to claim 1 or 2 produces the recycling processing method of waste water, it is characterised in that institute
On the basis of the coagulant stated is Powdered Activated Carbon and/or aluminium polychloride, the quality for producing waste water by para-aminophenol, coagulant
Addition be 0.1~0.5%.
4. para-aminophenol according to claim 1 produces the recycling processing method of waste water, it is characterised in that step
(2) in, the pH for washing water outlet is adjusted to 0.5~4,5~20 DEG C is cooled to, stands still for crystals.
5. para-aminophenol according to claim 1 produces the recycling processing method of waste water, it is characterised in that step
(3) in, the macroporous absorbent resin that the resin that resin adsorption is used is modified for phenolic hydroxyl group.
6. para-aminophenol according to claim 5 produces the recycling processing method of waste water, it is characterised in that resin is inhaled
Attached multiple is 10~100BV, and the rate of adsorption is 0.5~4BV/h.
7. para-aminophenol according to claim 1 produces the recycling processing method of waste water, it is characterised in that step
(3) in, use 40~60 DEG C, mass fraction resin is desorbed for 4~6% sig water, by the pH of desorption liquid adjust to
0.5~4 and it is cooled to 5~20 DEG C, is filtrated to get filtrate II I and p-nitrophenol crystal, reclaims p-nitrophenol, filtrate II I
Recycled is in configuration sig water desorption resin.
8. para-aminophenol according to claim 1 produces the recycling processing method of waste water, it is characterised in that step
(4) in, described post processing includes：
Resin adsorption water outlet is carried out ultraviolet catalytic oxidation by (4-1), and the power of uviol lamp is 1~15kW, ultraviolet catalytic oxygen
The reaction time of change is 5~200min；
Photooxidation water outlet is passed through ion exchange resin by (4-2), and the absorption multiple of ion exchange resin is 20~2000BV, absorption
Speed is 0.5~5BV/h；
Ion exchange resin absorption water outlet is carried out electrolysis with ion-exchange film by (4-3), and hydrogen, chlorine and caustic soda is made.
9. para-aminophenol according to claim 8 produces the recycling processing method of waste water, it is characterised in that step
In (4-1), photocatalysis oxidation reaction is carried out again after adding oxidant into resin adsorption water outlet；
Described oxidant is the one or more in hydrogen peroxide, sodium hypochlorite and chlorine dioxide；With the matter of resin adsorption water outlet
On the basis of amount, oxidant dosage is 0.1~2%.
10. para-aminophenol according to claim 8 produces the recycling processing method of waste water, it is characterised in that step
In (4-2), described ion exchange resin is sodium form cationic ion-exchange resin.
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| CN108623092A (en) * | 2018-05-07 | 2018-10-09 | 常州大学 | A kind of method that processing prepares the waste water that para-aminophenol generates |
| CN108706672A (en) * | 2018-04-03 | 2018-10-26 | 浙江奇彩环境科技股份有限公司 | A kind of recycling processing method of ammonia nitrogen waste water |
| CN108726740A (en) * | 2018-06-11 | 2018-11-02 | 山东龙安泰环保科技有限公司 | A kind of high sodium chloride waste water Zero discharge treatment method |
| CN109205851A (en) * | 2018-10-25 | 2019-01-15 | 中科协创环境科技江苏有限公司 | A kind of tail washings discharger handling coal chemical industry high-concentration sewage |
| CN110117115A (en) * | 2019-06-05 | 2019-08-13 | 南京大学盐城环保技术与工程研究院 | A kind of processing method and equipment of industrial waste salt recycling |
| CN113816520A (en) * | 2021-09-06 | 2021-12-21 | 天津长芦汉沽盐场有限责任公司 | Tetrabromo bisphenol A comprehensive wastewater treatment process |
| CN114291916A (en) * | 2021-12-31 | 2022-04-08 | 天富凯业(辽宁)新材料有限公司 | System and method for recycling o-aminophenol from o-aminophenol acidification wastewater |
| CN114772774A (en) * | 2022-02-21 | 2022-07-22 | 安徽东至广信农化有限公司 | Nitrochlorobenzene production wastewater treatment method |
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| CN108706672A (en) * | 2018-04-03 | 2018-10-26 | 浙江奇彩环境科技股份有限公司 | A kind of recycling processing method of ammonia nitrogen waste water |
| CN108706672B (en) * | 2018-04-03 | 2021-03-23 | 浙江奇彩环境科技股份有限公司 | Recycling treatment method of ammonia nitrogen wastewater |
| CN108623092A (en) * | 2018-05-07 | 2018-10-09 | 常州大学 | A kind of method that processing prepares the waste water that para-aminophenol generates |
| CN108726740A (en) * | 2018-06-11 | 2018-11-02 | 山东龙安泰环保科技有限公司 | A kind of high sodium chloride waste water Zero discharge treatment method |
| CN109205851A (en) * | 2018-10-25 | 2019-01-15 | 中科协创环境科技江苏有限公司 | A kind of tail washings discharger handling coal chemical industry high-concentration sewage |
| CN110117115A (en) * | 2019-06-05 | 2019-08-13 | 南京大学盐城环保技术与工程研究院 | A kind of processing method and equipment of industrial waste salt recycling |
| CN113816520A (en) * | 2021-09-06 | 2021-12-21 | 天津长芦汉沽盐场有限责任公司 | Tetrabromo bisphenol A comprehensive wastewater treatment process |
| CN114291916A (en) * | 2021-12-31 | 2022-04-08 | 天富凯业(辽宁)新材料有限公司 | System and method for recycling o-aminophenol from o-aminophenol acidification wastewater |
| CN114772774A (en) * | 2022-02-21 | 2022-07-22 | 安徽东至广信农化有限公司 | Nitrochlorobenzene production wastewater treatment method |
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