CN106865674A - A kind of method of the phenol wastewater extracting and dephenolizing of multistage mixed intensified separation - Google Patents

A kind of method of the phenol wastewater extracting and dephenolizing of multistage mixed intensified separation Download PDF

Info

Publication number
CN106865674A
CN106865674A CN201710117709.3A CN201710117709A CN106865674A CN 106865674 A CN106865674 A CN 106865674A CN 201710117709 A CN201710117709 A CN 201710117709A CN 106865674 A CN106865674 A CN 106865674A
Authority
CN
China
Prior art keywords
extraction
extractant
hypergravity
phenol
phase
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.)
Granted
Application number
CN201710117709.3A
Other languages
Chinese (zh)
Other versions
CN106865674B (en
Inventor
陈贵锋
高明龙
董卫果
杜松
王吉坤
段锋
付楚芮
贾媛
田陆峰
王亚强
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Coal Research Institute CCRI
Original Assignee
China Coal Research Institute CCRI
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by China Coal Research Institute CCRI filed Critical China Coal Research Institute CCRI
Priority to CN201710117709.3A priority Critical patent/CN106865674B/en
Publication of CN106865674A publication Critical patent/CN106865674A/en
Application granted granted Critical
Publication of CN106865674B publication Critical patent/CN106865674B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/26Treatment of water, waste water, or sewage by extraction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0488Flow sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0492Applications, solvents used
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • C02F2101/345Phenols

Abstract

The invention discloses a kind of method of the phenol wastewater extracting and dephenolizing of multistage mixed intensified separation.The method comprises the following steps:(1) multi-stage counter current extraction is carried out in extractant and phenol wastewater being sent into the multitple extraction device that some hypergravity extracters are constituted by opposite direction, final extraction phase and final raffinate phase is collected;(2) solvent recovery I will be carried out in the final extraction phase feeding solvent recovery tower, obtains crude phenols and extractant I;Solvent recovery II will be carried out in the final raffinate phase feeding solvent stripper, obtain the waste water after dephenolize and extractant II;The extractant I and the extractant II carry out the multi-stage counter current extraction in continuing to be passed through the multitple extraction device with the phenol wastewater.Extraction process of the present invention realizes two-phase laminated flow by hypergravity, and split-phase performance is good, and disposal ability is big;By Powerless spiral or vortex mixer, two-phase reaches that mass transfer balancing speed is fast, and mass-transfer efficiency is high, and stage efficiency is close to 100%.

Description

A kind of method of the phenol wastewater extracting and dephenolizing of multistage mixed intensified separation
Technical field
The invention belongs to field of waste water treatment, and in particular to a kind of phenol wastewater extracting and dephenolizing of multistage mixed intensified separation Method.
Background technology
Phenol for Waste Water class material is poisonous to biology, suppresses the growth of microorganism, causes biochemical system to be unable to stability and high efficiency and transports OK, but simultaneously phenol, as chemicals, can be recycled.At present, the conventional method of industrial wastewater containing phenol is that solvent extraction takes off Except aldehydes matter, wastewater biodegradability is improved, using the similar principle that mixes, most aldehydes matters enter extraction phase, pass through The isolated crude phenols product of rectifying, extractant is recycled, and the extractant for staying in raffinate phase strips recovery by solvent stripper Utilize.Current industrial field phenol wastewater extraction cells are typically what is carried out in extraction tower, mainly material filling type extraction tower and Rotating disc type extraction tower, all there is back mixing between more serious level, cause stage efficiency low in the two, separating interface is difficult to control, raffinate Mutually take away the problems such as extractant amount is larger, and increase stripping reclaims the energy consumption of extractant.
The content of the invention
It is an object of the invention to provide a kind of method of the phenol wastewater extracting and dephenolizing of multistage mixed intensified separation, the method Two-phase laminated flow is realized by hypergravity, split-phase performance is good, disposal ability is big, by Powerless spiral or vortex mixer, two Mutually reach mass transfer balancing speed fast, mass-transfer efficiency is high, stage efficiency is close to 100%.
The method of the phenol wastewater extracting and dephenolizing of the multistage mixed intensified separation that the present invention is provided, comprises the following steps:
(1) extractant and phenol wastewater are sent into the multitple extraction device that some hypergravity extracters are connected by opposite direction In carry out multi-stage counter current extraction, collect final extraction phase and final raffinate phase;
Every hypergravity extracter includes mixing chamber and idetified separation room, is passed through the extraction of the hypergravity extracter Agent and phenol wastewater mix in the mixing chamber in the presence of ribbon mixer or vortex mixer, then in the reinforcing Extracted in the presence of hypergravity in separation chamber;
(2) solvent recovery I is carried out in the extraction phase being sent into solvent recovery tower, crude phenols and extractant I is obtained;Will be described Solvent recovery II is carried out in raffinate phase feeding solvent stripper, the waste water after dephenolize and extractant II is obtained;The He of the extractant I The extractant II carries out the multi-stage counter current extraction in continuing to be passed through the multitple extraction device with the phenol wastewater.
Above-mentioned method, in step (1), the hypergravity extracter (hypergravity extractor) can be any utilization hypergravity The device for being extracted, it includes mixing chamber and idetified separation room;Ribbon mixer or vortex mixing in the mixing chamber In the presence of device, two-phase reaches that mass transfer balancing speed is fast, and mass-transfer efficiency is high, and stage efficiency is close to 100%;In the idetified separation room Two-phase laminated flow is realized in the presence of middle hypergravity, split-phase performance is good, and disposal ability is big;
The number of units of the hypergravity extracter can be 1~10 (it can be 1~10 grade to extract series), concretely 3~7 Platform, 3~5,5~7,3,5 or 7.
The centrifugal rotational speed of the hypergravity extracter can be 0~3000 rev/min, concretely 1500 revs/min.
The residence time of the hypergravity extracter can be 1 second~300 seconds, concretely 100~130 seconds, 100~110 Second, 110~130 seconds, 100 seconds, 110 seconds or 130 seconds.
Above-mentioned method, in step (1), the phenol wastewater can be (1~10) with the volume ratio of the extractant:1, tool Body can be (4~8):1st, (4~5):1st, (4~6):1st, (5~8):1st, (5~6):1st, (6~8):1、6:1、4:1、8:1 or 5:1.
The temperature of the extraction can be 30~85 DEG C, concretely 40~85 DEG C, 50~85 DEG C, 65~85 DEG C, 40~65 DEG C, 50~65 DEG C, 40~50 DEG C, 50 DEG C, 40 DEG C, 85 DEG C or 65 DEG C.
Above-mentioned method, in step (1), total phenol content can be 2000~25000mg/L in the phenol wastewater, such as 5750mg/L。
Total phenol includes unit phenol and polyhydric phenols, and wherein polyphenol content can be 600~12000mg/L, such as 1820mg/ L;Unit phenol content can be 1000~18000mg/L.
The phenol wastewater COD value can be 10000~50000mg/L, such as 19340mg/L.
The pH value of the phenol wastewater can be 4~10, such as 6~8,6~7,7~8,6,7 or 8.
The extractant is included but is not limited to:Hexone, Di Iso Propyl Ether, butyl acetate, sec-butyl acetate Or tert amyl methyl ether(TAME).
Above-mentioned method, in step (2), the number of theoretical plate of the solvent recovery tower can be 5~18 pieces, concretely 10~ 18 pieces, 10~15 pieces, 15~18 pieces, 10 pieces, 15 pieces, 18 pieces;Pressure can be 0.1~0.2Mpa, concretely 0.11~ 0.12Mpa, 0.12~0.13Mpa;Reboiler temperature can be 120~220 DEG C, concretely 200~220 DEG C.
The number of theoretical plate of the solvent stripper can be 3~25 pieces, concretely 4~6 pieces, 4~5 pieces, 5~6 pieces, 4 pieces, 5 pieces, 6 pieces;Pressure can be 0.1~0.2Mpa, concretely 0.11~0.12Mpa, 0.12~0.13Mpa;Reboiler temperature can It is 98~115 DEG C, concretely 105~110 DEG C.
The present invention has the advantages that:
(1) extraction process of the present invention realizes two-phase laminated flow by hypergravity, and split-phase performance is good, and disposal ability is big.
(2) by Powerless spiral or vortex mixer, two-phase reaches mass transfer balancing speed soon to extraction process of the present invention, Mass-transfer efficiency is high, and stage efficiency is close to 100%.
(3) extraction process operation stream of the present invention constant width more non-than scope, driving and parking is convenient, does not destroy set up each after parking Level concentration distribution, easily realizes on-line analysis and automatically controls.
(4) extraction process continuous flow upstream of the present invention is forced to realize by the suction force of every grade of mixing chamber, it is to avoid back mixing phenomenon.
(5) extraction process strong adaptability of the present invention, series boundary clearly, and is easy to regulation, can be according to water water quality Change flexible operating.
Brief description of the drawings
Fig. 1 is the structural representation of hypergravity extracter used in embodiment.
1 mixing chamber, 2 idetified separation rooms, 3 extractant feeds mouth, the outlet of 4 phenol wastewater charging apertures, 5 extraction phases, 6 raffinate phases Outlet.
Fig. 2 is the process chart of the inventive method.
Specific embodiment
Experimental technique used in following embodiments is conventional method unless otherwise specified.
Material used, reagent etc. in following embodiments, unless otherwise specified, commercially obtain.
In following examples and comparative example, the phenol wastewater is coal gasification waste water, total phenol in the phenol wastewater Content bromination volumetric method (the difference is that the step of not carrying out pre-distillation) according to specified in HJ502-2009 is measured;Unit Bromination volumetric method is measured after content pre-distillation according to specified in HJ502-2009 of phenol;The content of polyhydric phenols is total phenol Content subtracts the content of unit phenol;COD value is measured using method specified in HJT399-2007.
As shown in figure 1, every hypergravity extracter used in the present invention includes mixing chamber (1) and idetified separation room (2), The extractant and phenol wastewater of hypergravity extracter are passed through in mixing from extractant feed mouthful (3) and phenol wastewater charging aperture (4) Mix in the presence of Powerless spiral blender or vortex mixer in room (1), then the hypergravity in idetified separation room (2) In the presence of extracted, extraction finish after, extraction phase from extraction phase outlet (5) enter next stage hypergravity extracter extraction Agent charging aperture (3), the charging aperture of the polyphenol containing phenol (4) that raffinate phase enters next stage hypergravity extracter from raffinate phase outlet (6) enters The extraction of row next stage.Using " the efficient energy-saving centrifuge " disclosed in CN204219832U in following embodiments.Comparative example institute The centrifuge for using for CN 103818982A in the supercentrifuge that uses.
As shown in Fig. 2 the method for the phenol wastewater extracting and dephenolizing of the multistage mixed intensified separation that the present invention is provided, including such as Lower step:
(1) it is 1 by volume ratio:Fresh extractant (such as hexone, Di Iso Propyl Ether, the acetic acid fourth of (1~10) Ester, sec-butyl acetate or tert amyl methyl ether(TAME)) and phenol wastewater (total phenol content is 2000~25000mg/L, and polyphenol content is 600~12000mg/L, COD value be 10000~50000mg/L, pH value be 4~10) by opposite direction send into 1~10 hypergravity Multi-stage counter current extraction is carried out in the multitple extraction device of extracter series connection, collect final extraction phase (containing crude phenols and extractant) and most Whole raffinate phase (waste water containing a small amount of extractant);
Every hypergravity extracter includes mixing chamber (1) and idetified separation room (2), from extractant feed mouthful (3) and containing phenol Wastewater feed mouthful (4) is passed through the extractant of hypergravity extracter and phenol wastewater the Powerless spiral blender in mixing chamber (1) Or mix in the presence of vortex mixer, then extracted in the presence of hypergravity in idetified separation room (2), hypergravity The rotating speed of extracter is 0~3000 rev/min, and the residence time is 1 second~300 seconds;Extraction temperature is 30~85 DEG C, and extraction is finished Afterwards, extraction phase enters the extractant feed mouthful (3) of next stage hypergravity extracter from extraction phase outlet (5), and raffinate phase is from raffinate Mutually outlet (6) carries out the extraction of next stage into the charging aperture of the polyphenol containing phenol (4) of next stage hypergravity extracter;
(2) by final extraction phase send into solvent recovery tower (number of theoretical plate be 5~18 pieces, pressure be 0.1~0.2Mpa, then Boiling device temperature is 120~220 DEG C) in carry out solvent recovery I, obtain crude phenols and extractant I;Final raffinate phase is sent into solvent vapour Solvent recovery is carried out in stripper (number of theoretical plate is 3~25 pieces, and pressure is 0.1~0.2Mpa, and reboiler temperature is 98~115 DEG C) II, obtain the waste water after dephenolize and extractant II;Extractant I and extractant II continue to be passed through in multitple extraction device and useless containing phenol Water carries out multi-stage counter current extraction.
The extracting and dephenolizing of embodiment 1, Coal Chemical Industry phenol wastewater
Extracting and dephenolizing is carried out to Coal Chemical Industry phenol wastewater according to process chart shown in Fig. 2, is comprised the following steps that:
(1) it is 1 by volume ratio:6 extractant (hexone) and phenol wastewater (total phenol 5750mg/L, it is polynary Phenol 1820mg/L, COD content 19340mg/L, pH value is 8.0) to send into the multistage extraction that 5 hypergravity extracters are connected by opposite direction Take and carry out in device multi-stage counter current extraction (5 grades), collect final extraction phase (containing crude phenols and extractant) and final raffinate phase (containing lacking Measure the waste water of extractant);
Every hypergravity extracter includes mixing chamber (1) and idetified separation room (2), from extractant feed mouthful (3) and containing phenol Wastewater feed mouthful (4) is passed through the extractant of hypergravity extracter and phenol wastewater in mixing chamber (1) (between exocoel and housing) Wheeled agitating paddle and disperse in the presence of oar (Powerless spiral blender) to make extractant and waste water quickly mix that rotary drum drives And dispersion, mixing mass transfer is completed, then mixed liquor enters idetified separation room (2) in the presence of self priming pump, is produced by centrifugation Raw hypergravity and two-phase density contrast complete two-phase laminated flow, and the rotating speed of hypergravity extracter is 1500 revs/min, and the residence time is 110 seconds;Extraction temperature is 65 DEG C, and after extraction is finished, extraction phase enters next stage hypergravity extracter from extraction phase outlet (5) Extractant feed mouthful (3), raffinate phase enters the phenol wastewater charging aperture of next stage hypergravity extracter from raffinate phase outlet (6) (4) extraction of next stage is carried out, final extraction phase and final raffinate phase is finally recovered out.
(2) by final extraction phase feeding solvent recovery tower, (number of theoretical plate is 15 pieces, and pressure is 0.12~0.13Mpa, then is boiled Device temperature be 200~220 DEG C) in carry out solvent recovery I, tower top obtains extractant I, and tower reactor obtains crude phenols product;To finally extract Remaining phase feeding solvent stripper (number of theoretical plate is 5 pieces, and pressure is 0.12~0.13Mpa, and reboiler temperature is 105~110 DEG C) In carry out solvent recovery II, tower top obtains extractant II, and tower reactor obtains waste water after dephenolize;Extractant I and the extraction after water-oil separating Take during agent II continues to be passed through multitple extraction device carries out multi-stage counter current extraction with phenol wastewater, recycles.
Analyze after testing, waste water total phenol content 262mg/L after dephenolize, polyphenol content 220mg/L, COD are 2690mg/L, Wherein 5 hypergravity extracter motor operation power are 10kW.
The extracting and dephenolizing of embodiment 2, Coal Chemical Industry phenol wastewater
Extracting and dephenolizing is carried out to Coal Chemical Industry phenol wastewater according to process chart shown in Fig. 2, is comprised the following steps that:
(1) it is 1 by volume ratio:4 extractant (hexone) and phenol wastewater (total phenol 5750mg/L, it is polynary Phenol 1820mg/L, COD content 19340mg/L, pH value is 8.0) to send into the multistage extraction that 3 hypergravity extracters are connected by opposite direction Take and carry out in device multi-stage counter current extraction (3 grades), collect final extraction phase (containing crude phenols and extractant) and final raffinate phase (containing lacking Measure the waste water of extractant);
Every hypergravity extracter includes mixing chamber (1) and idetified separation room (2), from extractant feed mouthful (3) and containing phenol Wastewater feed mouthful (4) is passed through the extractant of hypergravity extracter and phenol wastewater in mixing chamber (1) (between exocoel and housing) Wheeled agitating paddle and disperse in the presence of oar (Powerless spiral blender) to make extractant and waste water quickly mix that rotary drum drives And dispersion, mixing mass transfer is completed, then mixed liquor enters idetified separation room (2) in the presence of self priming pump, is produced by centrifugation Raw hypergravity and two-phase density contrast complete two-phase laminated flow, and the rotating speed of hypergravity extracter is 1500 revs/min, and the residence time is 130 seconds;Extraction temperature is 75 DEG C, and after extraction is finished, extraction phase enters next stage hypergravity extracter from extraction phase outlet (5) Extractant feed mouthful (3), raffinate phase enters the phenol wastewater charging aperture of next stage hypergravity extracter from raffinate phase outlet (6) (4) extraction of next stage is carried out, final extraction phase and final raffinate phase is finally recovered out.
(2) by final extraction phase feeding solvent recovery tower, (number of theoretical plate is 18 pieces, and pressure is 0.12~0.13Mpa, then is boiled Device temperature be 200~220 DEG C) in carry out solvent recovery I, tower top obtains extractant I, and tower reactor obtains crude phenols product;To finally extract Remaining phase feeding solvent stripper (number of theoretical plate is 6 pieces, and pressure is 0.12~0.13Mpa, and reboiler temperature is 105~110 DEG C) In carry out solvent recovery II, tower top obtains extractant II, and tower reactor obtains waste water after dephenolize;Extractant I and the extraction after water-oil separating Take during agent II continues to be passed through multitple extraction device carries out multi-stage counter current extraction with phenol wastewater, recycles.
Analyze after testing, waste water total phenol content 310mg/L after dephenolize, polyphenol content 268mg/L, COD are 2994mg/L, Wherein 3 hypergravity extracter motor operation power are 6.6kW.
The extracting and dephenolizing of embodiment 3, Coal Chemical Industry phenol wastewater
Extracting and dephenolizing is carried out to Coal Chemical Industry phenol wastewater according to process chart shown in Fig. 2, is comprised the following steps that:
(1) it is 1 by volume ratio:8 extractant (hexone) and phenol wastewater (total phenol 5750mg/L, it is polynary Phenol 1820mg/L, COD content 19340mg/L, pH value is 7.0) to send into the multistage extraction that 7 hypergravity extracters are connected by opposite direction Take and carry out in device multi-stage counter current extraction (7 grades), collect final extraction phase (containing crude phenols and extractant) and final raffinate phase (containing lacking Measure the waste water of extractant);
Every hypergravity extracter includes mixing chamber (1) and idetified separation room (2), from extractant feed mouthful (3) and containing phenol Wastewater feed mouthful (4) is passed through the extractant of hypergravity extracter and phenol wastewater in mixing chamber (1) (between exocoel and housing) Wheeled agitating paddle and disperse in the presence of oar (Powerless spiral blender) to make extractant and waste water quickly mix that rotary drum drives And dispersion, mixing mass transfer is completed, then mixed liquor enters idetified separation room (2) in the presence of self priming pump, is produced by centrifugation Raw hypergravity and two-phase density contrast complete two-phase laminated flow, and the rotating speed of hypergravity extracter is 1500 revs/min, and the residence time is 100 seconds;Extraction temperature is 40 DEG C, and after extraction is finished, extraction phase enters next stage hypergravity extracter from extraction phase outlet (5) Extractant feed mouthful (3), raffinate phase enters the phenol wastewater charging aperture of next stage hypergravity extracter from raffinate phase outlet (6) (4) extraction of next stage is carried out, final extraction phase and final raffinate phase is finally recovered out.
(2) by final extraction phase feeding solvent recovery tower, (number of theoretical plate is 10 pieces, and pressure is 0.11~0.12Mpa, then is boiled Device temperature be 200~220 DEG C) in carry out solvent recovery I, tower top obtains extractant I, and tower reactor obtains crude phenols product;To finally extract Remaining phase feeding solvent stripper (number of theoretical plate is 4 pieces, and pressure is 0.11~0.12Mpa, and reboiler temperature is 105~110 DEG C) In carry out solvent recovery II, tower top obtains extractant II, and tower reactor obtains waste water after dephenolize;Extractant I and the extraction after water-oil separating Take during agent II continues to be passed through multitple extraction device carries out multi-stage counter current extraction with phenol wastewater, recycles.
Analyze after testing, waste water total phenol content 332mg/L after dephenolize, polyphenol content 291mg/L, COD are 3132mg/L, Wherein 7 hypergravity extracter motor operation power are 14kW.
The extracting and dephenolizing of embodiment 4, Coal Chemical Industry phenol wastewater
Extracting and dephenolizing is carried out to Coal Chemical Industry phenol wastewater according to process chart shown in Fig. 2, is comprised the following steps that:
(1) it is 1 by volume ratio:5 extractant (hexone) and phenol wastewater (total phenol 5750mg/L, it is polynary Phenol 1820mg/L, COD content 19340mg/L, pH value is 6.0) to send into the multistage extraction that 5 hypergravity extracters are connected by opposite direction Take and carry out in device multi-stage counter current extraction (5 grades), collect final extraction phase (containing crude phenols and extractant) and final raffinate phase (containing lacking Measure the waste water of extractant);
Every hypergravity extracter includes mixing chamber (1) and idetified separation room (2), from extractant feed mouthful (3) and containing phenol Wastewater feed mouthful (4) is passed through the extractant of hypergravity extracter and phenol wastewater in mixing chamber (1) (between exocoel and housing) Wheeled agitating paddle and disperse in the presence of oar (Powerless spiral blender) to make extractant and waste water quickly mix that rotary drum drives And dispersion, mixing mass transfer is completed, then mixed liquor enters idetified separation room (2) in the presence of self priming pump, is produced by centrifugation Raw hypergravity and two-phase density contrast complete two-phase laminated flow, and the rotating speed of hypergravity extracter is 1500 revs/min, and the residence time is 110 seconds;Extraction temperature is 40 DEG C, and after extraction is finished, extraction phase enters next stage hypergravity extracter from extraction phase outlet (5) Extractant feed mouthful (3), raffinate phase enters the phenol wastewater charging aperture of next stage hypergravity extracter from raffinate phase outlet (6) (4) extraction of next stage is carried out, final extraction phase and final raffinate phase is finally recovered out.
(2) by final extraction phase feeding solvent recovery tower, (number of theoretical plate is 18 pieces, and pressure is 0.12~0.13Mpa, then is boiled Device temperature be 200~220 DEG C) in carry out solvent recovery I, tower top obtains extractant I, and tower reactor obtains crude phenols product;To finally extract Remaining phase feeding solvent stripper (number of theoretical plate is 6 pieces, and pressure is 0.12~0.13Mpa, and reboiler temperature is 105~110 DEG C) In carry out solvent recovery II, tower top obtains extractant II, and tower reactor obtains waste water after dephenolize;Extractant I and the extraction after water-oil separating Take during agent II continues to be passed through multitple extraction device carries out counter current multi-stage extraction with phenol wastewater, recycles.
Analyze after testing, waste water total phenol content 88mg/L after dephenolize, polyphenol content 83mg/L, COD are 2136mg/L, its In 5 hypergravity extracter motor operation power be 10kW.
The extracting and dephenolizing of comparative example, Coal Chemical Industry phenol wastewater
Extracting and dephenolizing is carried out to Coal Chemical Industry phenol wastewater in accordance with the following steps:
(1) it is 1 by volume ratio:6 extractant (hexone) and phenol wastewater (total phenol 5750mg/L, it is polynary Phenol 1820mg/L, COD content 19340mg/L, pH value is that 8.0) by 5 desk centrifuges of opposite direction feeding, (rotating speed is 1500 revs/min Clock) series connection multitple extraction device in carry out multitple extraction, collect final extraction phase (containing crude phenols and extractant) and final raffinate Phase (waste water containing a small amount of extractant);
(2) by final extraction phase feeding solvent recovery tower, (number of theoretical plate is 15 pieces, and pressure is 0.12~0.13Mpa, then is boiled Device temperature be 180~220 DEG C) in carry out solvent recovery I, tower top obtains extractant I, and tower reactor obtains crude phenols product;To finally extract Remaining phase feeding solvent stripper (number of theoretical plate is 5 pieces, and pressure is 0.12~0.13Mpa, and reboiler temperature is 105~110 DEG C) In carry out solvent recovery II, tower top obtains extractant II, and tower reactor obtains waste water after dephenolize;Extractant I and the extraction after water-oil separating Take during agent II continues to be passed through multitple extraction device carries out counter current multi-stage extraction with phenol wastewater, recycles.
Analyze after testing, waste water total phenol content 276mg/L after dephenolize, polyphenol content 232mg/L, COD are 2760mg/L, Wherein 5 desk centrifuge motor operation power are 65kW.

Claims (6)

1. a kind of method of the phenol wastewater extracting and dephenolizing of multistage mixed intensified separation, comprises the following steps:
(1) enter in extractant and phenol wastewater being sent into the multitple extraction device that some hypergravity extracters are constituted by opposite direction Row multi-stage counter current extraction, collects final extraction phase and final raffinate phase;
Every hypergravity extracter includes mixing chamber and idetified separation room, be passed through the hypergravity extracter extractant and Phenol wastewater mixes in the mixing chamber in the presence of ribbon mixer or vortex mixer, then in the idetified separation Extracted in the presence of hypergravity in room;
(2) solvent recovery I will be carried out in the final extraction phase feeding solvent recovery tower, obtains crude phenols and extractant I;Will be described Solvent recovery II is carried out in final raffinate phase feeding solvent stripper, the waste water after dephenolize and extractant II is obtained;The extraction Agent I and the extractant II carry out the multi-stage countercurrent extraction in continuing to be passed through the multitple extraction device with the phenol wastewater Take.
2. method according to claim 1, it is characterised in that:In step (1), the number of units of the hypergravity extracter is 1 ~10;The centrifugal rotational speed of the hypergravity extracter is 0~3000 rev/min;1 second~300 seconds residence time.
3. method according to claim 1 and 2, it is characterised in that:In step (1), the phenol wastewater and the extraction The volume ratio of agent is (1~10):1;The temperature of the extraction is 30~85 DEG C.
4. the method according to any one of claim 1-3, it is characterised in that:It is total in the phenol wastewater in step (1) Phenol content be 2000~25000mg/L, total phenol include unit phenol and polyhydric phenols, wherein polyphenol content be 600~ 12000mg/L, unit phenol content is 1000~18000mg/L;The phenol wastewater COD value is 10000~50000mg/L;Institute The pH value for stating phenol wastewater is 4~10;The extractant is secondary hexone, Di Iso Propyl Ether, butyl acetate, acetic acid Butyl ester or tert amyl methyl ether(TAME).
5. the method according to any one of claim 1-4, it is characterised in that:In step (2), the solvent recovery tower Number of theoretical plate is 5~18 pieces, and pressure is 0.1~0.2Mpa, and reboiler temperature is 120~220 DEG C.
6. the method according to any one of claim 1-5, it is characterised in that:In step (2), the solvent stripper Number of theoretical plate is 3~25 pieces, and pressure is 0.1~0.2Mpa, and reboiler temperature is 98~115 DEG C.
CN201710117709.3A 2017-03-01 2017-03-01 Method for extracting and dephenolizing phenol-containing wastewater by multistage mixing and enhanced separation Active CN106865674B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710117709.3A CN106865674B (en) 2017-03-01 2017-03-01 Method for extracting and dephenolizing phenol-containing wastewater by multistage mixing and enhanced separation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710117709.3A CN106865674B (en) 2017-03-01 2017-03-01 Method for extracting and dephenolizing phenol-containing wastewater by multistage mixing and enhanced separation

Publications (2)

Publication Number Publication Date
CN106865674A true CN106865674A (en) 2017-06-20
CN106865674B CN106865674B (en) 2020-06-05

Family

ID=59169294

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710117709.3A Active CN106865674B (en) 2017-03-01 2017-03-01 Method for extracting and dephenolizing phenol-containing wastewater by multistage mixing and enhanced separation

Country Status (1)

Country Link
CN (1) CN106865674B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111847564A (en) * 2019-04-28 2020-10-30 华南理工大学 Semi-coke wastewater extraction dephenolization and negative pressure type extractant recovery method and device
CN114470854A (en) * 2022-02-11 2022-05-13 赤峰福纳康生物技术有限公司 Method for removing residual solvent in oil by using supergravity rotating bed gas extraction method

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2382463Y (en) * 1999-03-31 2000-06-14 潘小军 Pneumatic eddy super gravity field reactor
CN1269256A (en) * 1999-04-06 2000-10-11 潘小军 Eddy-current ultragravitational field reactor and its application
CN103818982A (en) * 2014-03-13 2014-05-28 中钢集团鞍山热能研究院有限公司 Centrifugal extracting wastewater dephenolization technology
CN104941246A (en) * 2015-04-21 2015-09-30 昆明理工大学 Impinging stream super-gravity liquid-liquid extractor
CN105712427A (en) * 2016-04-05 2016-06-29 华南理工大学 Extracting agent with high partition coefficient for polyphenol in phenol wastewater and extracting method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2382463Y (en) * 1999-03-31 2000-06-14 潘小军 Pneumatic eddy super gravity field reactor
CN1269256A (en) * 1999-04-06 2000-10-11 潘小军 Eddy-current ultragravitational field reactor and its application
CN103818982A (en) * 2014-03-13 2014-05-28 中钢集团鞍山热能研究院有限公司 Centrifugal extracting wastewater dephenolization technology
CN104941246A (en) * 2015-04-21 2015-09-30 昆明理工大学 Impinging stream super-gravity liquid-liquid extractor
CN105712427A (en) * 2016-04-05 2016-06-29 华南理工大学 Extracting agent with high partition coefficient for polyphenol in phenol wastewater and extracting method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111847564A (en) * 2019-04-28 2020-10-30 华南理工大学 Semi-coke wastewater extraction dephenolization and negative pressure type extractant recovery method and device
CN114470854A (en) * 2022-02-11 2022-05-13 赤峰福纳康生物技术有限公司 Method for removing residual solvent in oil by using supergravity rotating bed gas extraction method

Also Published As

Publication number Publication date
CN106865674B (en) 2020-06-05

Similar Documents

Publication Publication Date Title
CN104649563B (en) A kind of advanced treatment process of sludge containing oil
CN205774724U (en) A kind of rare earth processing stirring linkage extraction equipment
CN204564360U (en) A kind of lily is leached, feed liquid is separated and centrifugal device
CN103130353B (en) High calcium organic wastewater treatment method
CN106865674A (en) A kind of method of the phenol wastewater extracting and dephenolizing of multistage mixed intensified separation
CN206955874U (en) The processing system and its separation equipment of a kind of oily sludge
CN1119286C (en) Process for pre-treating waste liquid of p-benzoic acid by complexing and extraction
CN108298752A (en) A kind of highly salt containing organic waste water processing system and the method for handling waste water
CN204918224U (en) Oil field sewage treatment device
CN209352652U (en) A kind of extracting and dephenolizing device for coal chemical industrial waste water processing
CN101066120B (en) Efficient continuous spicy material eliminating process in capsanthin production
CN109293030A (en) Extracting and dephenolizing device and method for extracting and dephenolizing for coal chemical industrial waste water processing
CN108003082A (en) A kind of solvent recovery process for the production of poly arylidene thio-ester resinoid
CN101486628A (en) Method for extracting resorcin from resorcin-containing salt water solution
CN104129828B (en) A kind of method of phenol wastewater multistage static mixing clarification extracting and dephenolizing
CN105112084A (en) Device and method for extracting phenol products from medium-low temperature coal tar
CN215756548U (en) Phenol-containing wastewater treatment system
CN213313704U (en) Processing device for cholesterol separation
CN210419342U (en) Semi-coke wastewater extraction dephenolization and negative pressure type extractant recovery device
CN211946947U (en) Plant essential oil extraction device of dynamic distillation
CN2666899Y (en) Apparatus for recovering phenol end ammonia in waste water
CN204564361U (en) A kind of lily is leached, feed liquid is separated and concentrated device
CN106039763B (en) The extracting process of phenolic substances extraction equipment and phenolic substances
CN211097906U (en) Post-treatment device for supercritical carbon dioxide extract
CN107699689A (en) The controllable Rapid Extraction neutral section of reaction efficiency and method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant