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 PDFInfo
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- 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
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0488—Flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
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- 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
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
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.
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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 |
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