CN100375719C - Method of treating phencyclic compound waste water using liquid-liquid extraction - Google Patents
Method of treating phencyclic compound waste water using liquid-liquid extraction Download PDFInfo
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- CN100375719C CN100375719C CNB2006100499405A CN200610049940A CN100375719C CN 100375719 C CN100375719 C CN 100375719C CN B2006100499405 A CNB2006100499405 A CN B2006100499405A CN 200610049940 A CN200610049940 A CN 200610049940A CN 100375719 C CN100375719 C CN 100375719C
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- 239000002351 wastewater Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 32
- 150000001875 compounds Chemical class 0.000 title claims abstract description 17
- 238000000638 solvent extraction Methods 0.000 title claims abstract description 13
- 238000000622 liquid--liquid extraction Methods 0.000 title claims abstract description 12
- 238000000605 extraction Methods 0.000 claims abstract description 75
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 238000011084 recovery Methods 0.000 claims abstract description 5
- 239000002551 biofuel Substances 0.000 claims description 37
- -1 benzene ring compound Chemical class 0.000 claims description 21
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 6
- 229930195729 fatty acid Natural products 0.000 claims description 6
- 239000000194 fatty acid Substances 0.000 claims description 6
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 235000019387 fatty acid methyl ester Nutrition 0.000 claims description 4
- 150000002632 lipids Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 26
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 12
- 239000000284 extract Substances 0.000 abstract description 7
- 239000010815 organic waste Substances 0.000 abstract description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 239000002283 diesel fuel Substances 0.000 abstract 3
- 239000000203 mixture Substances 0.000 abstract 1
- 238000011017 operating method Methods 0.000 abstract 1
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- 230000031018 biological processes and functions Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000009284 supercritical water oxidation Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- Extraction Or Liquid Replacement (AREA)
- Physical Water Treatments (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method for treating waste water of compounds containing benzene rings by liquid-liquid extraction. The method comprises the following steps: step 1.1, fractional extraction of waste water of compounds containing benzene rings is carried out for 1 to 5 times at an ordinary temperature, biologic diesel oil is used as an extraction solvent, the volume ratio of the extraction solvent to the waste water of compounds containing benzene rings is from 5: 1 to 1: 10, the pH value is from 4 to 10, the extraction lasts for 3 to 30 min each time, and the mixture is made to stand for several minutes after the extraction and then is separated; step 1.2, extract phases containing benzene ring compounds and biologic diesel oil are respectively treated by reduced pressure distillation to recover the compounds containing benzene rings and the biologic diesel oil; step 1.3, general biochemical treatment of medium and low concentration organic waste water which is formed after the extraction is carried out, and then the treated organic waste water is discharged. The method has the advantages that the operating method is simple, the condition is mild, and the efficiency is notable; the extraction agent can be repeatedly used after the distillation recovery, the use efficiency is basically unchanged, and thus, the cost of waste water treatment is greatly lowered; and when the method is adopted, useful compounds in waste water can be further extracted and recovered.
Description
Technical field
The present invention relates to the method for a kind of wastewater treatment method, particularly a kind for the treatment of phencyclic compound waste water using liquid-liquid extraction.
Background technology
The a large amount of trade effluents that discharged in industry such as chemical industry and petrochemical complex, pharmacy, food, kind is many because of having, complicated component, COD
CrCharacteristics such as (chemical oxygen demand (COD)) concentration height, biodegradability are poor, poisonous and harmful if fail effectively to control and administer, will cause serious pollution and destruction to environment.Numbers of the enterprise such as China's chemical industry, pharmacy, dyestuff are big, and it is wide to distribute, and contains a large amount of organism in the sewage of discharging, and the benzene ring substance that contains wherein then belongs to the organism that contaminated area is wide, toxicity is bigger.On the other hand, containing the phenyl ring type organic is again important chemical material.Therefore, developing wastewater processing technology efficiently, realize the efficient utilization and the recycle of the innoxious and resource of pollutant effluents, is the effective way that alleviates environmental pollution.
For many years, the various countries investigators have worked out the method that multiple improvement high density contains benzene ring compound waste water, as physics method (vaporizing extract process, solvent extration), chemical method (micro-electrolysis method, reagent oxidation method, supercritical water oxidation method, ultrasonic wave air oxidation style, ozone oxidation method) and biological process etc.It is higher that chemical process is handled the cost that contains benzene ring compound waste water, and organism is decomposed, and is unfavorable for the resource circulation utilization.Biological process needs to dilute with a large amount of water earlier, has increased the weight of the burden of biological treatment so greatly, has increased cost, has also caused the huge waste of water resources simultaneously.And the vaporizing extract process in the physics method is not only not high to the clearance that contains benzene ring compound, and owing to be water more than 90% in the waste water, the specific heat of water and the latent heat of vaporization are big, and steam stripped energy consumption is high, and rare people adopts.
Perfect method is: high concentrated organic wastewater is adopted method of extraction earlier, extract major part or whole organism, make it to become " organic waste water of lower concentration ", carry out biochemical treatment again, the organism recycle that extraction obtains, or utilize again after further separating, as shown in Figure 1 and Figure 2.Solvent extration uses in the recycling that contains benzene ring compound extensively, advantage be need not heat or cooling, energy consumption are low, continuous production, the processing water yield is big, equipment simple, operational safety, fast, cost is low.In order to reach satisfied water treatment effect, general at present multi-stage solvent extraction method or extraction process and the additive method associated treatment of adopting.Have for the higher waste water of organic content and to use the report as extraction agent such as benzene,toluene,xylene.(No.3 P93-94) extracts aniline waste water for three grades with toluene for Northeast Forestry University's journal, Vol.25, and the aniline clearance is more than 90% as Zou Hefeng.Waste water after three grades of extractions, COD
CrReduce to 1521mg/L by 19060mg/L, clearance reaches 92%.But above-mentioned solvent exists big, the generation secondary pollution problem of solubleness in the water, the large-scale production of difficult realization.
Summary of the invention
The objective of the invention is to deficiency at the prior art scheme, and provide a kind of method for the treatment of phencyclic compound waste water using liquid-liquid extraction, adopted a kind of economical and effective, eco-friendly processing to contain the solvent of phenyl ring type organic waste water, with the COD of the water after this solvent treatment
CrClearance can reach more than 95%, and, reuse after this solvent should be able to reclaim, regenerate, and can from waste water, extract the useful benzene ring type compounds that contains.
The present invention finishes above-mentioned purpose by the following technical programs.The method of this treating phencyclic compound waste water using liquid-liquid extraction comprises the steps:
1.1), at normal temperatures will contain benzene ring compound waste water with biofuel as extraction solvent fractional extraction 1～5 time, also can adopt counter current continuous extraction, extraction solvent is 5: 1～1: 10 with the volume ratio that contains benzene ring compound waste water, pH value is 4～10, each extraction time is 3～30min, separates after leaving standstill several minutes after the extraction;
1.2), the extraction phase that contains benzene ring compound and contain biofuel reclaims respectively through underpressure distillation and contains benzene ring compound, as aniline, oil of mirbane etc.; And biofuel, the biofuel of recovery still recycles as extraction solvent, and the performance index of regeneration back extraction solvent biofuel return to the level before the extraction substantially;
1.3), the organic waste water of the middle lower concentration that forms after the extraction treatment, carry out conventional biochemical treatment again, then discharging.
Biofuel (being fatty acid ester) used among the present invention is fatty acid methyl ester, fatty-acid ethyl ester or lipid acid propyl ester, boiling point is higher than 350 ℃ during the biofuel normal pressure, and contain the organic atmospheric boiling point of phenyl ring is about 200 ℃, adopt underpressure distillation, can will contain benzene ring compound and separate, and separate more thorough with biofuel.
During extraction, the pH value of waste water has a significant impact effect of extracting, and preferred pH value is 6～8, is 7 to be the best with PH.Preferred extraction solvent is 2: 1～1: 1 with the volume ratio preferred range that contains benzene ring compound waste water when extraction, and most preferred extraction progression is 3 times.
The effect that the present invention is useful:
1, the present invention adopts biofuel as extraction agent the high-load phenyl ring waste water that contains to be handled, and its working method is simple, mild condition, and effect is remarkable.Through three grades of extractions, can make the COD of aniline waste water
CrReduce to 735mg/L by 80741mg/L, the COD of phenolic waste water
CrReduce to 621mg/L by 14604mg/L, the clearance of aniline and phenol reaches 99.1% and 95.7% respectively.
2, the used extraction agent of present method is reusable after distillation is reclaimed, and recovery method economy is simple, and result of use is constant substantially, thereby has saved the cost of wastewater treatment greatly.Simultaneously, because the mutual solubility of water and biofuel is extremely low, the solubleness of biofuel in water only is 0.002% under the normal temperature, makes that the biofuel content of handling in the water of back is very little, and biofuel has biodegradable characteristics again, and this is that other extraction agents are incomparable.
3, adopt method of the present invention, can further extract and reclaim useful compound in the waste water, as aniline, phenol, oil of mirbane etc.
Therefore, technical scheme treatment effect of the present invention is good, and working cost is low, has tangible environmental benefit and social benefit, has important use to be worth.
Description of drawings:
Fig. 1 is former process block schematic flow sheet;
Fig. 2 is a block flowsheet synoptic diagram of the present invention;
Embodiment:
Below in conjunction with accompanying drawing and specific embodiment the present invention is further described:
Embodiment 1: the method for the treatment of phencyclic compound waste water using liquid-liquid extraction of the present invention comprises the steps:
1.1), at normal temperatures will contain benzene ring compound waste water with biofuel as extraction solvent fractional extraction 3 times, also can adopt counter current continuous extraction; Aniline waste water is the tap water preparation, concentration～7838.33 μ g/mL, COD
Cr～21267.6mg/L, pH～7.0; Get waste water 100ml, add extraction solvent biofuel (fatty acid methyl ester) 200ml, the extraction time is 10min, leaves standstill after the extraction after 5 minutes and takes out water; With the extraction of biofuel equal-volume, as above, carry out 3 grades of extractions altogether again.The detected result of water outlet is: aniline concentration～1.04 μ g/mL, COD
Cr～672.5mg/L.
1.2), the extraction phase that contains benzene ring compound and contain biofuel reclaims respectively through underpressure distillation and contains benzene ring compound, as aniline, oil of mirbane etc.; And biofuel, the biofuel of recovery still recycles as extraction solvent, and the performance index of regeneration back extraction solvent biofuel return to the level before the extraction substantially; Boiling point is higher than 350 ℃ during the biofuel normal pressure, is about 200 ℃ and contain the organic atmospheric boiling point of phenyl ring, adopts underpressure distillation, can will contain benzene ring compound and separate with biofuel, and separate more thorough.
1.3), the organic waste water of the middle lower concentration that forms after the extraction treatment, carry out conventional biochemical treatment again, then discharging.
Embodiment 2: be with the difference of embodiment 1:
Aniline waste water is the tap water preparation, COD
Cr～80741mg/L, pH～7.0.
Get waste water 100ml, add biofuel (employing fatty-acid ethyl ester) 100ml, extracted 10 minutes, leave standstill after 5 minutes and take out water; With the extraction of biofuel equal-volume, as above, carry out 3 grades of extractions altogether again.The detected result of water outlet is: COD
Cr～735mg/L.
Embodiment 3: be with the difference of embodiment 1:
Phenolic waste water is the tap water preparation, COD
Cr～14604mg/L, pH～7.0.
Get waste water 100ml, add biofuel (lipid acid propyl ester) 100ml, extracted 10 minutes, leave standstill after 5 minutes and take out water; With the extraction of biofuel equal-volume, as above, carry out 3 grades of extractions altogether again.The detected result of water outlet is: COD
Cr～621mg/L.
Embodiment 4: be with the difference of embodiment 1:
Get waste water 100ml, add extraction solvent biofuel (fatty acid methyl ester) 1000ml, the extraction time is 20min, leaves standstill after the extraction after 5 minutes and takes out water; With the extraction of biofuel equal-volume, as above, carry out 5 grades of extractions altogether again.
Embodiment 5: be with the difference of embodiment 1:
Get waste water 100ml, add extraction solvent biofuel (fatty-acid ethyl ester) 30ml, the extraction time is 5min, leaves standstill after the extraction after 5 minutes and takes out water; With the extraction of biofuel equal-volume, as above, carry out 2 grades of extractions altogether again.
Embodiment 6: be with the difference of embodiment 1:
Phenolic waste water is the tap water preparation, CODcr～14604mg/L, pH～6.0.
Get waste water 100ml, add extraction solvent biofuel (lipid acid propyl ester) 500ml, the extraction time is 15min, leaves standstill after the extraction after 5 minutes and takes out water; With the extraction of biofuel equal-volume, as above, carry out 4 grades of extractions altogether again.
Claims (5)
1. the method for a treating phencyclic compound waste water using liquid-liquid extraction is characterized in that, mainly comprises the steps:
1.1), at normal temperatures will contain benzene ring compound waste water with biofuel as extraction solvent fractional extraction 1～5 time or counter current continuous extraction, extraction solvent is 5: 1～1: 10 with the volume ratio that contains benzene ring compound waste water, pH value is 4～10, each extraction time is 3～30min, separates after leaving standstill several minutes after the extraction;
1.2), the extraction phase that contains benzene ring compound and contain biofuel reclaims respectively through underpressure distillation and contains benzene ring compound and biofuel, the biofuel of recovery still recycles as extraction solvent.
2. the method for the treatment of phencyclic compound waste water using liquid-liquid extraction according to claim 1 is characterized in that: in step 1.1) in, used biofuel, promptly fatty acid ester is fatty acid methyl ester, fatty-acid ethyl ester or lipid acid propyl ester.
3. the method for the treatment of phencyclic compound waste water using liquid-liquid extraction according to claim 1 is characterized in that: the pH value when extraction is 6～8.
4. the method for the treatment of phencyclic compound waste water using liquid-liquid extraction according to claim 3 is characterized in that: the pH value when extraction is 7.
5. the method for the treatment of phencyclic compound waste water using liquid-liquid extraction according to claim 1 is characterized in that: the extraction solvent when extraction is 2: 1～1: 1 with the volume ratio that contains benzene ring compound waste water.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| AU2010274399A1 (en) * | 2009-07-22 | 2012-02-09 | Issei Co., Ltd. | Method for treatment of liquid waste of coating agent |
| CN103613159A (en) * | 2013-11-12 | 2014-03-05 | 南京工业大学 | Treatment process of phenol-containing wastewater in dicumyl peroxide production |
| CN106957083B (en) * | 2017-03-06 | 2019-11-12 | 聊城市鲁西化工工程设计有限责任公司 | A kind of anti-back-mixing static state oily-water seperating equipment, separation system and separation method |
| CN110016370B (en) * | 2019-04-29 | 2021-04-27 | 佛山市光烨环保科技有限公司 | Method for preparing anti-emulsification high-stability biodiesel by utilizing phenolic wastewater |
| EP3966189A1 (en) * | 2019-05-07 | 2022-03-16 | Lyondell Chemical Technology, L.P. | Methods of chemical recovery for propylene oxide-styrene monomer processes |
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| JP2003071204A (en) * | 2001-09-05 | 2003-03-11 | National Institute Of Advanced Industrial & Technology | Method for separating and collecting water soluble organic substance from water to be treated |
| JP2003081896A (en) * | 2001-09-05 | 2003-03-19 | National Institute Of Advanced Industrial & Technology | Method for recovering water soluble organic substance from water to be treated |
| CN1600696A (en) * | 2004-10-12 | 2005-03-30 | 南化集团研究院 | Nitrobenzene extraction method for treating aniline wastewater |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003071204A (en) * | 2001-09-05 | 2003-03-11 | National Institute Of Advanced Industrial & Technology | Method for separating and collecting water soluble organic substance from water to be treated |
| JP2003081896A (en) * | 2001-09-05 | 2003-03-19 | National Institute Of Advanced Industrial & Technology | Method for recovering water soluble organic substance from water to be treated |
| CN1600696A (en) * | 2004-10-12 | 2005-03-30 | 南化集团研究院 | Nitrobenzene extraction method for treating aniline wastewater |
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