CN105565565A - Method for treating highly-enriched phenol-containing coal chemical-industrial waste water by recycling efficient extraction agent - Google Patents
Method for treating highly-enriched phenol-containing coal chemical-industrial waste water by recycling efficient extraction agent Download PDFInfo
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- CN105565565A CN105565565A CN201510937835.4A CN201510937835A CN105565565A CN 105565565 A CN105565565 A CN 105565565A CN 201510937835 A CN201510937835 A CN 201510937835A CN 105565565 A CN105565565 A CN 105565565A
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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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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- 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
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
Abstract
The invention discloses a method for treating highly-enriched phenol-containing coal chemical-industrial waste water by recycling an efficient extraction agent. A dephenolizing extraction solvent adopted by the method disclosed by the invention has a high distribution coefficient for phenolic compounds and particularly extraction on polyphenol, solves the problem that a common extraction solvent cannot effectively extract polyphenol, and is particularly suitable for treatment on highly-enriched gasified waste water which contain various phenols and is slightly neutral and alkaline. According to the method disclosed by the invention, a technical process is simple; conditions are mild; before extraction, acid does not need to be added to regulate acidity and alkalinity of the waste water; after extraction, the solvent can be regenerated by adopting a distillation method, is recycled and is low in loss; adopted equipment has high blockage resistance, and is suitable for gasified waste water with fly ash and tar. The method disclosed by the invention is high in dephenolizing efficiency. In the waste water, a removal rate of total phenols reaches 93%, a removal rate of volatile phenols reaches 99%, a removal rate of CODCr (Chemical Oxygen Demand Cr) is about 85%, the phenolic compounds in the waste water can be effectively recovered, and the method is also beneficial to subsequent treatment and up-to-standard emission of the waste water.
Description
Technical field
The invention belongs to technical field of sewage, be specifically related to a kind ofly recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process.
Background technology
Gasification, oil refining and coking industry produce a large amount of phenolic wastewater in process of production, and waste water quality is very complicated, and phenol concentration is high, and phenol is of a great variety, and existing unit phenol, has polyphenol again; Water quality is middle meta-alkalescence.In addition containing organism, sour gas, tar, flyash etc. such as lipid acid, ketone and amines.Waste water COD
crbe worth high, and be difficult to biological degradation.The dephenolize abstraction technique developing such waste water significantly can reduce the phenol content of waste water on the one hand, reduces the pollution to environment; On the other hand, the multiple pollutants such as phenols wherein are also important industrial chemicals, thus, remove efficiently and reclaim the pollutents such as the phenols in coal chemical industrial waste water, are the effective ways realizing the innoxious and resource utilization of waste water.
The method reclaiming phenol in high-concentration phenolic wastewater has solvent extration, absorption method, steam blow-off method, ion exchange method, chemical precipitation, reverse osmosis method etc.Solvent extration utilizes phenol solubleness to be in organic solvent greater than the solubleness in water, thus the phenol extraction in waste water out.Solvent extration dephenolize efficiency is high, extraction agent source is wide, all uses in a large number both at home and abroad.But for the extracting and dephenolizing of high density containing phenol gasification, oil refining and coke-oven waste water, the subject matter existed at present has: (1) common extraction agent to the phenolic wastewater of meta-alkalescence and the extraction efficiency of polyphenol low; (2) in extraction process, loss of extractant is large, recycles rate low; (3) heightening efficiency is low; (4) extraction equipment easily blocks.
Aldehydes matter ionizes in acid condition hardly, exists with molecularity.And in basic solution as pH>8, phenol starts to ionize (for phenol): PhOHfPh0
-+ H
+, as pH>9, dissociation is more obvious.The Ph0 of ionic state
-group wetting ability strengthens, and the solubleness in water increases substantially, thus causes effect of extracting to decline.And the polyphenol in waste water due to many through the effect of base, it is water-soluble larger than unit phenol, is usually also difficult to effective extraction.
Harbin Gas Works adopts diisopropyl ether as extraction agent, carries out extracting and dephenolizing process to this factory's gasification phenolic wastewater.Diisopropyl ether has boiling point and saturation steam forces down, water-soluble little, reclaim easily, consume energy the advantage such as little, but its dephenolize, particularly polyphenol efficiency is low.In waste water after dephenolize, total phenol concentration is still up to about 1400mg/L, and wherein polyphenol just has 800 ~ 1100mg/L, COD
crvalue about 6000mg/L.Not only cause the waste of phenol, and this waste water enters subsequent biochemical treating pond, seriously exceed biochemical treatment load, be difficult to reach sewage discharge index request, serious threat is caused to basin, downstream, Song Hua River water body.Diisopropyl ether can meet the demands substantially to the effect of extracting of unit phenol, but is not a kind of well extraction agent for polyphenol, and its partition ratio is very low.The partition ratio of diisopropyl ether Pyrogentisinic Acid is 36.5, but Resorcinol and hydroxyquinol only has 1.03 and 0.18 respectively, and is not suitable as the extraction solvent of the coal gasification waste water containing polyphenol.In addition, the turntable extracting tower efficiency that this factory now uses is lower, and through on-site proving, the actual effect of extracting only having about 0.9 ~ 1.2 grade, can not meet actual requirement.
In sum, the extracting and dephenolizing technology of current high-concentration phenolic wastewater is not satisfactory, and loss of extractant is large, and extraction agent cyclic utilization rate is low, and the phenol concentration of processed waste water is still quite high, is difficult to the qualified discharge meeting subsequent biochemical process.
Summary of the invention
In order to the shortcoming overcoming prior art is with not enough, the object of the present invention is to provide and a kind ofly recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process.The method makes Phenolic Compounds From Wastewater Containing Phenols material effectively be deviate from and reclaim, and extraction agent can efficiency utilization.
Object of the present invention is achieved through the following technical solutions:
Recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process, comprise the steps:
(1) mixed solution is mixed to get dense for height containing phenol coal chemical industrial waste water and extraction solvent hexone;
(2) mixed solution is left standstill phase-splitting, be extracted mutually and extracting phase;
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate;
(4) extraction phase that step (2), (3) obtain is carried out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate that step (3) obtains is carried out stripping, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and step (5) obtain returns step (1), (3) recycle.
Preferred version of the present invention is as follows:
In described step (1), be total phenol content containing phenol coal chemical industrial waste water be 5000 ~ 20000mg/L, volatile phenol content 3000 ~ 10000mg/L; PH value is 3 ~ 11, is preferably 4 ~ 10, COD
crvalue is 15000 ~ 35000mg/L, and the waste water containing oil content (lipid acid, tar, coal ash).
In step (1), described mixing adopts static mixer carry out and flow mixing, mixeding liquid temperature is 30 ~ 85 DEG C, containing phenol coal chemical industrial waste water pH value in mixed solution is 3 ~ 11, be preferably 4 ~ 10, extraction solvent methyl iso-butyl ketone (MIBK) is 1:(2 ~ 8 with the volume ratio containing phenol coal chemical industrial waste water).
In step (1), described mixeding liquid temperature is 40 ~ 60 DEG C, and the pH value containing phenol coal chemical industrial waste water in mixed solution is 5 ~ 11, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:(2 ~ 8 with the volume ratio containing phenol coal chemical industrial waste water).
The filler that described static mixer uses can be honeycomb structured packing;
The extraction tower that extraction described in step (3) adopts is packing tower, and its filler used is honeycomb structured packing.
In step (2), described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 10 ~ 40min, is preferably 10 ~ 30min; Be more preferably 15 ~ 25min.
In step (3), described extraction adopts extraction tower to carry out 3 ~ 8 stage countercurrent extractions, extraction solvent is methyl iso-butyl ketone (MIBK), its initial total phenol content is less than 50mg/L, the volume ratio of extraction solvent and extracting phase (compared with) be 1:(2 ~ 8), extraction temperature is 30 ~ 85 DEG C, and extraction pH value is 3 ~ 11, is preferably 4 ~ 10.
The wherein volume ratio (compared with) be preferably 1:(2 ~ 6) of extraction solvent and extracting phase, extraction temperature is preferably 40 ~ 60 DEG C, and extraction pH value is preferably 5 ~ 10, and extraction progression is preferably 4 ~ 6 grades.The selection of above-mentioned extraction parameters, reason is as follows:
(1) when extraction pH value is 3 ~ 11, extraction solvent methyl iso-butyl ketone (MIBK) is on the extraction ability of phenol substantially by the impact of pH change, and effect of extracting is good; As pH>11, phenol extraction effect reduces; Then be difficult to during pH>12 go out phenol from Wastewater by Solvent Extraction.Contain a large amount of free ammonias containing in phenol coal chemical industrial waste water, waste water is middle meta-alkalescence, can meet the requirement of extraction pH value.
(2) change of extraction temperature can make extraction equilibrium be moved, and changes Extraction equilibrium constants, thus affects effect of extracting.When extraction temperature is 30 ~ 85 DEG C, the impact of temperature variation on this extraction agent dephenolize is not obvious, considers actual plant effluent temperature, extraction temperature preferably 40 ~ 60 DEG C.
(3) extraction solvent and described extracting phase volume ratio (compared with) selection affect the phenol concentration of extraction tower sum of series raffinate waste water phase, also affect the process cost of solvent reclamation simultaneously.In separation requirement one timing, compare larger, the progression of required extraction tower equipment is lower, and cost of equipment reduces, but solvent reclamation expense increases.Therefore, compare when meeting technique (phenol concentration) and equipment index (extraction progression), usually the smaller the better, therefore the volume ratio (compared with) be 1:(2 ~ 8) of extraction solvent and described extracting phase in the inventive method, preferred 1:(2 ~ 6).
(4) 1:(2 ~ 6 are being compared), when the initial total phenol content of extraction solvent is less than 50mg/L, adopt solvent methylisobutyl ketone by 3 ~ 8 stage countercurrent extractions, the total phenol concentration in waste water can be dropped to below 400mg/L, volatile phenol concentration drops to about 10mg/L.But along with the increase of extraction progression, the amplitude that phenol concentration reduces is more and more less, after progression arrives 8 grades, increase extraction progression again, oneself effectively can not reduce the concentration of phenol, can increase cost on the contrary, therefore the extraction progression in the inventive method is 3 ~ 8 grades, is preferably 4 ~ 6 grades.
In step (4), described rectifying adopts rectifying tower to carry out.
In step (5), described stripping carries out in stripping tower.
Adopt the inventive method process high density containing phenol coal chemical industrial waste water, extraction agent cyclic utilization rate can reach 95%, and can realize total phenol removal rate and reach 93%, the decreasing ratio of volatile phenol reaches 99%, COD
crdecreasing ratio about 85%.The method has reclaimed the aldehydes matter in waste water effectively, and the aldehydes matter of recovery can rectifying purifying further, is converted into useful industrial chemicals.
Principle of the present invention is: water and hexone have azeotropic point at 88 DEG C, and azeotropic consists of MIBK content 75.7%.So raffinate enters gun barrel phase-splitting again mode after can adopting first stripping reclaims extraction agent from raffinate; Under normal pressure, MIBK boiling point is 116 DEG C, phenol boiling point 181.2 DEG C, and Resorcinol boiling point 286.2 DEG C, boiling-point difference is larger.Therefore extraction phase carries out separating and recovering extractant by rectificating method.
The present invention, relative to prior art, has following advantage and effect:
(1) partition ratio of dephenolize extraction solvent to phenolic compound of method employing of the present invention is high, particularly for the extraction of polyphenol, solve the problem that general extraction solvent effectively can not extract polyphenol, be particularly suitable for high dense, containing the process of the coal gasification waste water of multiple phenol, the inclined neutral and alkali of water quality.
(2) method and technology technique of the present invention is simple, mild condition, and regulate waste water potential of hydrogen without the need to acid adding before extraction, the solvent after extraction can adopt rectification method to regenerate, and recycle, solvent loss is little.
(3) equipment that method of the present invention adopts has very strong anti-blocking, is suitable for the coal gasification waste water containing flyash, tar.
(4) method dephenolize efficiency of the present invention is high.Total phenol removal rate in waste water reaches 93%, and the decreasing ratio of volatile phenol reaches 99%, COD
crdecreasing ratio about 85%, can reclaim the aldehydes matter in waste water effectively, is also conducive to the follow-up governance for reaching standard discharge of waste water.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
Select pending containing phenol coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 10000mg/L, volatile phenol content 6000mg/L; PH value is 5, COD
crvalue is 30000mg/L, oil content 200mg/L.
(1) mixed solution will be mixed to get containing phenol coal coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and mixeding liquid temperature is 30 DEG C, and containing phenol coal coal chemical industrial waste water pH value in mixed solution is 10, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:8 with the volume ratio containing phenol coal coal chemical industrial waste water.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; Described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 40min.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction solvent and raffinate, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 3 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, and the volume ratio of extraction solvent and remaining liquid is 1:2, and extraction temperature is 30 DEG C, and extraction pH value is 11.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.
Waste water total phenol content after process is less than 400mg/L, and wherein volatile phenol is less than 20mg/L; COD
crbe about 3800mg/L, decreasing ratio reaches 94.2% respectively, and 99.3%, 82.7%.
Embodiment 2
Select pending containing phenol coal coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 10000mg/L, volatile phenol content 6000mg/L; PH value is 10, COD
crvalue is 15000mg/L, oil content 500mg/L.
(1) mixed solution will be mixed to get containing phenol coal coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and mixeding liquid temperature is 85 DEG C, and containing phenol coal coal chemical industrial waste water pH value in mixed solution is 3, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:6 with the volume ratio containing phenol coal coal chemical industrial waste water.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; Described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 10min.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 8 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, and the volume ratio of extraction solvent and remaining liquid is l:4, and extraction temperature is 85 DEG C, and extraction pH value is 3.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.
Total phenol content in processed waste water is less than 400mg/L, and wherein volatile phenol is less than 15mg/L; COD
crbe about 3600mg/L, decreasing ratio reaches 93.7% respectively, and 99.3%, 83.6%.
Embodiment 3
Select pending containing phenol coal coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 5000mg/L, volatile phenol content 3000mg/L; PH value is 7, COD
crvalue is 25000mg/L, oil content 300mg/L.
(1) mixed solution will be mixed to get containing phenol coal coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and mixeding liquid temperature is in 45 DEG C of mixed solutions be 8 containing phenol coal coal chemical industrial waste water pH value, and extraction solvent methyl iso-butyl ketone (MIBK) and the volume ratio containing phenol coal coal chemical industrial waste water are 1:3.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; Described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 30min.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 5 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, and the volume ratio of extraction solvent and remaining liquid is 1:5, and extraction temperature is 65 DEG C, and extraction pH value is 6.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.Total phenol content in processed waste water is less than 450mg/L, and wherein volatile phenol is less than 20mg/L, COD
crbe about 4200mg/L, decreasing ratio reaches 91.7% respectively, and 99.3%, 80.9%.
Embodiment 4
Select pending containing phenol coal coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 9000mg/L, volatile phenol content 3500mg/L; PH value is 7, COD
crvalue is 19000mg/L, oil content 400mg/L.
(1) mixed solution will be mixed to get containing phenol coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and mixeding liquid temperature is 80 DEG C, and containing phenol coal coal chemical industrial waste water pH value in mixed solution is 10, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:3 with the volume ratio containing phenol coal coal chemical industrial waste water.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; Described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 35min.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 6 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, and the volume ratio of extraction solvent and remaining liquid is 1:6, and extraction temperature is 45 DEG C, and extraction pH value is 5.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.
Total phenol content in processed waste water is less than 350mg/L, and wherein volatile phenol is less than 10mg/L; COD
crbe about 3500mg/L, decreasing ratio reaches 93.5% respectively, and 99.6%, 84.1%.
Embodiment 5
Select pending containing phenol coal coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 10000mg/L, volatile phenol content 4000mg/L; PH value is 5, COD
crvalue is 30000mg/L, oil content 200mg/L.
(1) mixed solution will be mixed to get containing phenol coal coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and described mixeding liquid temperature is 40 DEG C, and the pH value containing phenol coal coal chemical industrial waste water in mixed solution is 11, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:8 with containing phenol coal coal chemical industrial waste water volume ratio.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; Described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 25min.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 4 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, and the volume ratio of extraction solvent and remaining liquid is 1:2, and extraction temperature is 40 DEG C, and extraction pH value is l0.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.
Total phenol content in processed waste water is less than 320mg/L, and wherein volatile phenol is less than 10mg/L; COD
crbe about 3300mg/L, decreasing ratio reaches 94.8% respectively, and 99.6%, 85.3%.
Embodiment 6
Select pending containing phenol coal coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 20000mg/L, volatile phenol content 8000mg/L; PH value is 10, COD
crvalue is 15000mg/L, oil content 500mg/L.
(1) mixed solution will be mixed to get containing phenol coal coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and described mixeding liquid temperature is 60 DEG C, and the pH value containing phenol coal coal chemical industrial waste water in mixed solution is 5, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:2 with the volume ratio containing phenol coal gasification waste water.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; Described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 15min.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 6 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, and the volume ratio of extraction solvent and remaining liquid is 1:8, and extraction temperature is 60 DEG C, and extraction pH value is 5.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.
Total phenol content in processed waste water is less than 500mg/L, and wherein volatile phenol is less than 50mg/L; COD
crbe about 3700mg/L, decreasing ratio reaches 93.8% respectively, and 99.1%, 83.2%.
Embodiment 7
Select pending containing phenol coal coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 20000mg/L, volatile phenol content 10000mg/L; PH value is 10, COD
crvalue is 30000mg/L, oil content 200mg/L.
(1) mixed solution will be mixed to get containing phenol coal coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and described mixeding liquid temperature is 60 DEG C, and the pH value containing phenol coal coal chemical industrial waste water in mixed solution is 10, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:2 with containing phenol coal coal chemical industrial waste water volume ratio.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; Described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 15min.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 6 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, and the volume ratio of extraction solvent and remaining liquid is 1:6, and extraction temperature is 40 DEG C, and extraction pH value is 5.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.
Total phenol content in processed waste water is less than 480mg/L, and wherein volatile phenol is less than 10mg/L; COD
crbe about 3700mg/L, decreasing ratio reaches 92.9% respectively, and 99.1%, 83.2%.
Embodiment 8
Select pending containing phenol coal coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 10000mg/L, volatile phenol content 4000mg/L; PH value is 6, COD
crr value is 15000mg/L, oil content 500mg/L.
(1) mixed solution will be mixed to get containing phenol coal coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and described mixeding liquid temperature is 60 DEG C, and the pH value containing phenol coal coal chemical industrial waste water in mixed solution is 5, and extraction solvent methyl iso-butyl ketone (MIBK) is l:8 with the volume ratio containing phenol coal coal chemical industrial waste water.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; It is 25min that described phase-splitting adopts water-and-oil separator to carry out described mixed solution residence time in water-and-oil separator.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and extraction liquid, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 4 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, and the volume ratio of extraction solvent and remaining liquid is 1:8, and extraction temperature is 60 DEG C, and extraction pH value is l0.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.
Waste water total phenol content after process is less than 420mg/L, and wherein volatile phenol is less than 20mg/L; COD
crbe about 3800mg/L, decreasing ratio reaches 92.8% respectively, and 99.3%, 82.7%.
Embodiment 9
Select pending containing phenol coal coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 10000mg/L, volatile phenol content 4000mg/L; PH value is 5, COD
crvalue is 15000mg/L, oil content 500mg/L.
(1) mixed solution will be mixed to get containing phenol coal coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and described mixeding liquid temperature is 40 DEG C, and the pH value containing phenol coal coal chemical industrial waste water in mixed solution is 5, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:2 with the volume ratio containing phenol coal coal chemical industrial waste water.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; Described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 25min.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 4 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, and the volume ratio of extraction solvent and remaining liquid is 1:2, and extraction temperature is 40 DEG C, and extraction pH value is l0.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.
Total phenol content in processed waste water is less than 420mg/L, and wherein volatile phenol is less than 20mg/L; COD
crbe about 3800mg/L, decreasing ratio reaches 93.2% respectively, and 99.4%, 82.7%.
Embodiment 10
Select pending containing phenol coal coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 8000mg/L, volatile phenol content 3000mg/L; PH value is 10, COD
crvalue is 25000mg/L, oil content 4mg/L.
(1) mixed solution will be mixed to get containing phenol coal coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and described mixeding liquid temperature is 60 DEG C, and the pH value containing phenol coal coal chemical industrial waste water in mixed solution is 10, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:6 with containing phenol coal gasification waste water volume ratio.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; Described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 25min.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 6 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, the volume ratio 1:6 of extraction solvent and remaining liquid, and extraction temperature is 50 DEG C, and extraction pH value is 10.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.
Total phenol content in processed waste water is less than 450mg/L, and wherein volatile phenol is less than 20mg/L; COD
crbe about 4000mg/L, decreasing ratio reaches 93.1% respectively, and 99.5%, 85.7%.
Embodiment 11
Select pending containing phenol coal coal chemical industrial waste water, treatment capacity is 100t/h, and total phenol content is 10000mg/L, volatile phenol content 6000mg/L; PH value is 5, COD
crvalue is 30000mg/L, oil content 500mg/L.
(1) mixed solution will be mixed to get containing phenol coal coal chemical industrial waste water and extraction solvent methyl iso-butyl ketone (MIBK); Described mixing adopts static mixer carry out and flow mixing, and described mixeding liquid temperature is 40 DEG C, and the pH value containing phenol coal coal chemical industrial waste water in mixed solution is 10, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:4 with containing phenol coal coal chemical industrial waste water volume ratio.
(2) by mixed solution phase-splitting, be extracted mutually and extracting phase; Described phase-splitting adopts water-and-oil separator to carry out, and described mixed solution residence time in water-and-oil separator is 25min.
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate, carries out remaining extraction solvent recycling to raffinate; Described extraction adopts extraction tower to carry out 4 stage countercurrent extractions, and extraction solvent is methyl iso-butyl ketone (MIBK), and its initial total phenol content is less than 50mg/L, and the volume ratio of extraction solvent and remaining liquid is 1:4, and extraction temperature is 60 DEG C, and extraction pH value is l0.
(4) send the extraction phase that step (2), (3) obtain to rectifying tower and carry out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate obtained after step (3) multi-stage counter current extraction is inputted in stripping tower, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and the raffinate of step (5) stripping multi-stage counter current extraction obtain returns step (1), (3) recycle.
Total phenol content in processed waste water is less than 310mg/L, and wherein volatile phenol is less than 10mg/L; COD
crbe about 2900mg/L, decreasing ratio reaches 92.3% respectively, and 99.4%, 80.7%.
In embodiment, volatile phenol concentration determination adopts GB GB7491-87 bromination volumetry.
Total phenol concentration determination adopts direct bromination.In detected water sample, add excessive bromine, make aldehydes matter and bromine generate brominated phenol, excessive bromine iodometric titrationiodimetry titration, thus calculate total phenol content.Phenol nearly all in the method energy wastewater measurement, is applicable to the coal gasification waste water large containing many, the non-volatile phenol amounts of phenol kind of the present invention.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (8)
1. recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process, it is characterized in that comprising the steps:
(1) mixed solution is mixed to get dense for height containing phenol coal chemical industrial waste water and extraction solvent hexone;
(2) mixed solution is left standstill phase-splitting, be extracted mutually and extracting phase;
(3) extracting phase that obtains of step (2) is through multi-stage counter current extraction, obtains being rich in phenol extraction phase and raffinate;
(4) extraction phase that step (2), (3) obtain is carried out rectifying, reclaim extraction solvent and crude phenols;
(5) raffinate that step (3) obtains is carried out stripping, reclaim in raffinate the extraction solvent dissolving and carry secretly;
(6) extraction solvent that two portions extraction solvent obtained by step (4) rectifying extraction phase and step (5) obtain returns step (1), (3) recycle.
2. according to claim 1ly recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process, it is characterized in that:
In described step (1), be total phenol content containing phenol coal chemical industrial waste water be 5000 ~ 20000mg/L, volatile phenol content 3000 ~ 10000mg/L; PH value is 3 ~ 11, COD
crvalue is 15000 ~ 35000mg/L, and the waste water containing oil content.
3. according to claim 1ly recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process, it is characterized in that: in step (1), described mixed solution, mixeding liquid temperature is 30 ~ 85 DEG C, containing phenol coal chemical industrial waste water pH value in mixed solution is 3 ~ 11, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:(2 ~ 8 with the volume ratio containing phenol coal chemical industrial waste water).
4. according to claim 1 or 3, recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process, it is characterized in that:
In step (1), described mixeding liquid temperature is 40 ~ 60 DEG C, and the pH value containing phenol coal chemical industrial waste water in mixed solution is 5 ~ 11, and extraction solvent methyl iso-butyl ketone (MIBK) is 1:(2 ~ 8 with the volume ratio containing phenol coal chemical industrial waste water).
5. according to claim 1ly recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process, it is characterized in that: in step (2), the time that described mixed solution leaves standstill phase-splitting is 10 ~ 40min.
6. recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process according to claim 1 or 5, it is characterized in that: in step (2), the time that described mixed solution leaves standstill phase-splitting is 10 ~ 30min.
7. according to claim 1ly recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process, it is characterized in that: in step (3), described extraction is for carrying out 3 ~ 8 stage countercurrent extractions, extraction solvent is methyl iso-butyl ketone (MIBK), the volume ratio of extraction solvent and extracting phase is 1:(2 ~ 8), extraction temperature is 30 ~ 85 DEG C, and extraction pH value is 3 ~ 11.
8. according to claim 1 or 6, recycle the high dense method containing phenol coal chemical industrial waste water of efficient extraction agent process, it is characterized in that: described extraction is for carrying out 4 ~ 6 stage countercurrent extractions, the volume ratio of extraction solvent and extracting phase is 1:(2 ~ 6), extraction temperature is 40 ~ 60 DEG C, and extraction pH value is 5 ~ 10.
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