CN105668677A - Synergistic extracting agent for oil and phenol in waste water of coal chemical industry - Google Patents
Synergistic extracting agent for oil and phenol in waste water of coal chemical industry Download PDFInfo
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Abstract
The invention discloses a synergistic extracting agent for oil and phenol in waste water of the coal chemical industry. The extracting agent comprises sec-butyl acetate and butyl acetate. A mixture of butyl acetate and sec-butyl acetate is used as the extracting agent; and the extracting agent has good oil removal and phenol removal effect, does not produce oil-containing sludge and secondary pollutants like dross, has a high recovery rate and exerts excellent extraction effect. Butyl acetate and sec-butyl acetate are low in price, safe, stable, widely available and slightly corrosive to equipment, so equipment maintenance cost is reduced, and waste water treatment cost is decreased to a greatest extent. With the extracting agent, the total oil content of purified waste water is decreased to less than 50 mg/L, total phenol content is lower than 400 mg/L, and a COD value is less than 3500 mg/L; an oil removal rate reaches 95.78 to 97.03%, wherein the removal rate of dissolved oil reaches 96.55 to 97.73%; a phenol removal rate reaches 98.19 to 98.40%; and the extracting agent has excellent oil removal, phenol removal and COD reducing effects.
Description
Technical field
The invention belongs to coal chemical industrial waste water process extraction agent technical field, specifically relate to a kind of coal chemical industrial waste water oil phenol synergistic extraction agent.
Background technology
Flourish along with China's coal chemical industry, the blowdown of industrial production is required improve constantly and strengthen by country. Compared with other industry, coal chemical industrial waste water has that the such as water yield is big, phenol content height, oil-contg height, particularly the feature such as the dissolving oil being difficult to process at present containing higher concentration.
Containing a large amount of toxic substance in phenol ammonia waste water, such as phenol, ammonia, hydrogen sulfide etc., phenols wherein is a kind of prototype matter poisonous substance, to all toxic effect of various biont, it enters skin or immerses in organism through oral cavity by skin contact, form insoluble protein matter after contacting with the protein in cell magma thus make cell lose activity, especially have bigger avidity for neural system, cause neural system generation pathology. The water source that mankind's long-term drinking is polluted by aldehydes matter, can cause chronic poisoning, the symptoms such as headache, dizziness, fatigue, insomnia, tinnitus, hypomnesis occurs. And water body water source, hydrobiont, farm crop also can be produced serious impact by aldehydes matter.
Oily substance in phenol ammonia waste water mainly contains following several occurrence status: (1) is floating to oil (particle diameter > 100 μm), is easy to from waste water and is separated; (2) dispersion oil (particle diameter is between 10-100 μm), is suspended in water; (3) (particle diameter is between 10 for oil in water emulsion-3-10 μm), particle diameter is very little, in emulsified state, not easily separated removing; (4) dissolving oil, is also soluble oil, the oil being dissolved completely in water, and its particle diameter is less than 10-3μm, and there is stronger polarity. Oily substance in above waste water, floats and oils and disperse oil all to be removed by the mode of air-float purification, and oil in water emulsion is also removed by adding the mode of emulsion splitter. Have dissolving oil only, presently there is no suitable method and removed. And the oil-contg height in waste water, will seriously affect the removal effect of aldehydes matter in phenol ammonia waste water, and then seriously affect downstream biochemical treatment, cause bio-chemical effluent severe overweight.
There is due to the oils in coal chemical industrial waste water and aldehydes matter so serious harm and toxicity just, only through purification de-oiling, phenol removal, just can enter follow-up treatment process, and then realize qualified discharge
The outstanding shortcoming that existing high-concentration phenol and ammonia waster water process generally exists is: 1) dephenolization effect is not good, and especially during polyphenol content height, dephenolization effect is poor, causes downstream biochemical treatment system to run;2) existing extraction agent has certain requirement for the oily substance content in waste water, and when oil-contg wherein is higher than 100mg/L, dephenolization effect starts decline, when seriously declining higher than dephenolization effect during 400mg/L, causes downstream water treatment system to run; 3) synergistic extraction of the dissolving oil in oil phenol cooperation-removal, particularly waste water and phenol cannot be realized.
In order to application extraction agent or other novel coal chemical industrial waste water dephenolization treating method, researcher has carried out a large amount of further investigations, and achieves some achievements, such as:
CN1087607A discloses the method for a kind of waste water-tar associating dephenolize, and described method alkaline solution, as dephenolizer, comprises the steps: that (1) is water source taking phenolic wastewater, adds inorganic base, be mixed with the alkaline dephenolizer of 5-30%; (2) contacting with tar with above-mentioned dephenolizer, wash temperature is 15-90 DEG C, 10-60 minute reaction times, carries out phenol removal to containing phenolic tar; (3) separation alkalescence phenates aqueous phase and tar phase, decomposite phenols by sulfuric acid decomposition method or carbonic acid gas decomposition method. By process like this, can greatly reduce the phenols in waste water, oil, prussiate, nitrogen class all pollutents.
CN1365953A discloses a kind of for petrochemical industry sour water and the desulfurization of alkaline residue, de-ammonia, dephenolization treating method, it is included in the mixture of sour water or sour water and alkaline residue and adds molysite, and by pressurized air, make the generation thiosulphate of the divalent sulfur in waste water and vitriol with desulfurization; Waste water after desulfurization is promoted in the biological tower filter tank of Gas feeding after sweetening agent retrieving arrangement, utilizes pressurized air and microorganism that ammonium salt is carried out nitrated, generates nitrate with de-ammonia; Microorganism in biological tower filter tank such as bacterium utilizes the oxygen in pressurized air to make the phenol in waste water resolve into carbonic acid gas and water with dephenolize. The desulfuration efficiency of the method up to more than 98%, ammonia removal efficiency reach 95%, the removal efficiency of phenol can reach 80%.
CN1361068A discloses a kind of method refining oil alkaline waste water dephenolize, described method using as extraction phase work in-process gasoline with have adjusted pH value and reclaimed the products such as naphthenic acid, crude phenols, sodium carbonate after containing phenol alkaline waste water, mix through mixing tank with certain proportion, then leave standstill, after layering, isolate work in-process gasoline, thus de-except the phenol in alkaline waste water. The method is simple, extraction efficiency height, floor space are little, cost is low, and can improve the antioxidant property of oil product, does not cause secondary pollution.
CN1683475A discloses a kind of complex extracting and dephenolizing method for alkaline slag of smeltery, by tributyl phosphate, C4-C7Assorted alcohol and toluene, ethylbenzene or dimethylbenzene are mixed to get extraction agent I; By C8-C12Stable hydrocarbon, C4-C7Assorted alcohol and toluene, ethylbenzene or dimethylbenzene are mixed to get extraction agent II; With alkaline residue system, extraction agent I being mixed complexometric extraction, and then adds extraction II, complexometric extraction, obtains three phase extraction system, and a phase is extracting phase, and a phase is the phase I being rich in phenol and extraction agent I, and one for being rich in sulfide and extraction agent III. The method is by utilizing tributyl phosphate, C4-C7Assorted alcohol and the synergistic effect containing the aromatic hydrocarbon three of alkyl group side chain improve the percentage extraction of extraction agent I when weakly alkaline, by extraction agent II, above-mentioned extraction phase medium sulphide content is carried out extracting and separating, reduce the content of phenol medium sulphide content, it is to increase the purity of phenol and utilization ratio.
CN1834040A discloses the method for extracting and dephenolizing of a kind of high density containing phenol coal gasification waste water, described method is separated after mixing with extraction solvent methyl iso-butyl ketone (MIBK) containing phenol coal gasification waste water, obtain liquid more than solvent phase and aqueous phase, solvent phase rectifying is reclaimed extraction solvent and crude phenols;Liquid more than aqueous phase is carried out multi-stage counter current extraction again, and the extraction liquid obtained carries out remaining the step of extraction solvent recycling, and the method technique is simple, mild condition, and extraction solution can recycle.
CN103496812A discloses a kind of method processing high-concentration phenol ammonia waste water, described method is in waste water extracting and dephenolizing step, n-butyl acetate is used to carry out counter-current extraction for extraction agent, re-use depickling deammoniation tower to take off except the sour gas in waste water and ammonia, and use solvent stripper to reclaim the extraction agent in extraction phase and obtain crude phenols product at the bottom of tower. Compared with prior art, the method effect of extracting is good, dephenolize efficiency height, and technical process is short, processing cost is low, method is simple, easy and simple to handle, Disposal quality is reliable.
CN103466873A discloses a kind of de-except the ammonia in waste water, phenol and sour gas, and processes the method for effective, efficient and that cost performance is high process containing high-concentration phenol, ammonia sewage; It adopts n-butyl acetate as extraction agent, not only rate of recovery height, and efficient energy-saving, cost performance height; After can making extraction, the phenol concentration in waste water is down to biochemical treatment and is entered below phenol concentration that water requires; Adopt Double-Tower Structure to make separation more thorough, decrease single tower and be separated not drawback thoroughly; Adopt counter-current extraction method to make extraction more efficient, it is separated more thorough; It is worthy to be popularized and application.
CN103466874A discloses a kind of High-concentration phenol-ammonia sewage treatment method, the method is first with the single tower alkali injection de-ammonia of pressurization stripping depickling, extracting and dephenolizing is carried out again, it may also be useful to solvent recovery tower and solvent stripper reclaim the extraction agent in extraction phase and obtain crude phenols product at the bottom of tower using n-butyl acetate as extraction agent. The method utilizes that n-butyl acetate price azeotropic point that is cheap and water is higher, solubleness is low, in whole production process, loss amount is less, the features such as energy consumption is lower in removal process, it is possible to increases substantially the extrusion rate of phenol or reduces the process cost of extraction section.
Application number disclosed in substantive examination on March 13 in 2014 be 201410093663.2 patent of invention disclose a kind of Centrifugical extraction sewage dephenolizing process, Centrifugical extraction separation is carried out as extraction plant with supercentrifuge, dephenolize extraction agent used is one or more in diisopropyl ether, N-BUTYL ACETATE, hexone, 30% tributyl phosphate and kerosene mixture, kerosene, heavy benzene oil, and the mixed volume of described phenol-containing wastewater and extraction agent is than being 3:1～10:1. This invention adopts the method for Centrifugical extraction, but extraction agent used all exists certain problem, and such as Di Iso Propyl Ether easily volatilizees, and loss is relatively big, can cause water pollution once again; N-BUTYL ACETATE cost is higher, and in water, solubleness is bigger; Hexone is then suitable for the waste water lower containing phenol amount, then processes effect for the waste water higher containing phenol not good; Then there is easily degraded of being heated in tributyl phosphate, degraded product not only easily affects its separation efficiency, and easily forms three-phase in extraction, disturbs normal extraction process; Heavy benzene oil then easily produces secondary pollution; Kerosene mixture, kerosene are then on the high side. All there is a great defect in this kind of extractants, all need to be processed by oil-in-water before extraction treatment, when ensureing to extract, oil-in-water content is lower than 50mg/L, otherwise carry out in treating processes, oil in water can pollute extraction agent, causing the rate of recovery of extraction agent to reduce, and then increase Solvent quantity, cost increases.
As mentioned above, prior art discloses the multiple method of Phenol-Containing Wastewater Treatment, but still there are some shortcomings in these methods, as except phenol effect is not high, polyphenol percentage extraction is too low, it is loaded down with trivial details to process, especially oil phenol synergistic extraction cannot be realized, and when in phenol ammonia waste water during oily substance oil-contg height, when adopting extraction process dephenolize, effect is poor etc.Therefore, exploitation oil phenol synergistic extraction agent and using method are the research focus and emphasis in this field at present, the power that also the present invention is accomplished just and place, basis.
Summary of the invention
Specifically, the problem that the present invention solves is: provide a kind of extraction agent that can solve the waste water that coexists containing phenol ammonia and dissolving oil very well.
A kind of coal chemical industrial waste water oil phenol synergistic extraction agent, described extraction agent is made up of sec-butyl acetate and butylacetate.
A kind of coal chemical industrial waste water oil phenol synergistic extraction agent, described extraction agent comprises sec-butyl acetate and butylacetate.
The volume ratio of described sec-butyl acetate and butylacetate is 1:1～6.
The volume ratio of described sec-butyl acetate and butylacetate is 1:1～3.
The volume ratio of described sec-butyl acetate and butylacetate is 1:2.
In the mixture, the volume ratio of sec-butyl acetate and butylacetate can determine suitable ratio according to the character of phenol ammonia waste water, to realize the best effect of oil phenol synergistic extraction. (1) when described extraction agent is sec-butyl acetate, it to be significantly higher than the decreasing ratio of n-butyl acetate of the prior art for the decreasing ratio of phenolic compound especially polyphenol compound. Unexpectedly, (2) when adding butylacetate further wherein, it is possible to improve the decreasing ratio of polyphenol compound further, oil phenol synergistic extraction can be realized simultaneously.
Above-mentioned extraction agent not only can take off except the pollutent phenolic compound in coal chemical industrial waste water, especially polyphenol compound, and achieve oil phenol synergistic extraction, de-oiling first in existing technique, rear dephenolize two-stage process are united two into one, more solving dissolving oil in current phenol ammonia waste water cannot the difficult problem of effective elimination, such that it is able to be applied in the oily phenol synergistic extraction of coal chemical industrial waste water, there are good industrial applications prospect and potentiality.
In oil phenol cooperation-removal method of the present invention, when described extraction agent is sec-butyl acetate, butylacetate mixture, first sec-butyl acetate is fully mixed with butylacetate.
In the described oil phenol cooperation-removal method of the present invention, when the volume ratio of described extraction agent and pending coal chemical industrial waste water is 1:1-100, such as, can be 1:1,1:10,1:30,1:50,1:80,1:100.
As mentioned above, the present invention provides a kind of coal chemical industrial waste water oil phenol synergistic extraction agent, by the selection of extraction agent component and respective content, thus achieve excellent de-oiling, dephenolization effect, especially there is very high removal effect for dissolving oil and polyphenol compound, it is much better than removal methods of the prior art, has huge application prospect and potentiality in coal chemical technology.
Below in conjunction with useful effect, the present invention is described further:
(1) the present invention breaches the limitation of tradition phenol ammonia waste water treatment process, butylacetate and sec-butyl acetate is utilized to mix as extraction agent, reach the simultaneously oil removing of phenol ammonia waste water or/and dephenolize, particularly remove the object of solvability oil, it is ensured that in processed waste water, oil, phenol content reach subsequent treatment process requirement. And people often select sherwood oil, normal hexane as oil removing extraction agent respectively in existing industrial production, diisopropyl ether, hexone etc. are as dephenolize extraction agent, remove useless oil-in-water, phenol are successively de-, then can not reach oil removing simultaneously or/and the effect of dephenolize.
(2) utilizing butylacetate and sec-butyl acetate to mix as extraction agent, oil removing dephenolization effect is good, does not produce the secondary pollution such as oily sludge and scum silica frost, and extraction agent rate of recovery height, effect of extracting is extremely good.Butylacetate and sec-butyl acetate price are wide, equipment corrosion is little compared with low, safety and stability, source, reduce equipment maintenance cost, reduce cost for wastewater treatment to maximum degree.
(3) testing through a large amount of practical application, after adopting this extraction agent, in the waste water after purification, total oil-contg is down to below 50mg/L (wherein dissolving oil content is lower than 40mg/L), and total phenol content is lower than 400mg/L, and COD value is lower than 3500mg/L. Oil removal rate reaches 95.78～97.03%, and wherein dissolving oil removal rate reaches 94.06～97.73%, and dephenolize rate reaches 98.57～98.74%, and oil removing, dephenolize, to fall COD effect all extremely good.
Embodiment
Below by specific embodiment, the present invention is described in detail; but the purposes of these exemplary enforcement modes and object are only used for enumerating the present invention; not the real protection scope of the present invention is formed any type of any restriction, more non-protection scope of the present invention is confined to this.
Coal Chemical Industry phenolic wastewater
The phenolic wastewater of certain Coal Chemical Industry is sampled, then measures total phenol content wherein, monohydric phenol content and polyphenol content, dissolving oil content (measuring method public affairs are known, this is no longer going to repeat them), shown in each content table specific as follows:
Monohydric phenol content and polyphenol content, dissolving oil content in the phenolic wastewater of table 1 Coal Chemical Industry
| Project | Total phenol content | Monohydric phenol content | Polyphenol content | Dissolving oil content |
| Content (mg/L) | 18950 | 10153 | 8797 | 629 |
Unless otherwise prescribed, otherwise below all embodiments all use this Coal Chemical Industry phenolic wastewater as phenol removal sample.
Embodiment 1: the removal effect contrast experiment of different extraction agent
Above-mentioned phenol removal sample conveniently processes the method for waste water, parameter and step process, difference part is that the volume ratio using following extraction agent and described extraction agent and waste water is 1:5, extraction agent n-butyl acetate, n-butyl acetate and common situation about being combined respectively except phenol agent.
Extraction agent 1: butylacetate.
Extraction agent 2: butylacetate+isopropyl ether
Extraction agent 3: butylacetate+methyl iso-butyl ketone (MIBK)
Extraction agent 4: butylacetate+methyl isopropyl Ketone
Extraction agent 5: butylacetate+methyl phenyl ketone
Extraction agent 6: butylacetate+sec-butyl acetate
Table 2 butylacetate is combined various phenol, oil-contg (mg/L) and decreasing ratio (%) after process with common except phenol agent
Conclusion: can find out from the above-mentioned data of table 2, it is used alone butylacetate, compared with removing phenol agent combination acquisition oil phenol extraction agent with butylacetate and other, the combination extraction agent of the butylacetate+sec-butyl acetate of the present invention can realize monohydric phenol in better trade effluent, polyphenol, dissolving oil removal effect, the dissolving oil in the waste water particularly being difficult to most remove in the industry.
Embodiment 2: the removal effect contrast experiment of different extraction agent
Above-mentioned phenol removal sample conveniently processes the method for waste water, parameter and step process, difference part is that the volume ratio using following extraction agent and described extraction agent and waste water is 1:5, the extraction agent n-butyl acetate of inclined oil removing, n-butyl acetate and the common situation removed phenol agent and be combined respectively.
Extraction agent 1: sec-butyl acetate.
Extraction agent 2: sec-butyl acetate+normal hexane
Extraction agent 3: sec-butyl acetate+hexanaphthene
Extraction agent 4: sec-butyl acetate+octane
Extraction agent 5: sec-butyl acetate+pentane
Extraction agent 6: sec-butyl acetate+butylacetate
Table 3 sec-butyl acetate is combined the rear various phenol of process, oil-contg (mg/L) and decreasing ratio (%) with common degreaser
Conclusion: can find out from above-mentioned data, it is used alone sec-butyl acetate, with sec-butyl acetate compared with the combination acquisition oil phenol extraction agent of other degreasers, the combination extraction agent of the butylacetate+sec-butyl acetate of the present invention can realize monohydric phenol in better trade effluent, polyphenol, oil-in-water removal effect, the dissolving oil in the waste water particularly being difficult to most remove in the industry.
Extraction agent 4: the mixture of sec-butyl acetate and butylacetate.
Through measuring, various phenol in processed waste water, oil-contg and decreasing ratio arrange in table 3.
Table 4. processes rear various phenol, oil-contg (mg/L) and decreasing ratio (%)
From table 4, relative to butylacetate of the prior art, in the present invention when extraction agent is sec-butyl acetate, total phenol removal rate has had and has significantly improved, although monohydric phenol decreasing ratio is about the same, unexpectedly, but, polyphenol decreasing ratio has had and has significantly improved, and dissolving oil there almost is not removal effect by both. And when the mixture that extraction agent is sec-butyl acetate and butylacetate, it has been found that total phenol removal rate and polyphenol decreasing ratio have all had further raising, achieve oil phenol synergistic extraction simultaneously.
Embodiment 3: the investigation of sec-butyl acetate and butylacetate amount ratio in extraction agent 3
Use extraction agent 3, the present embodiment is implemented according to the same procedure of above-described embodiment 1, difference part only is to change the volume ratio of sec-butyl acetate and butylacetate in extraction agent 3, and various phenol content, decreasing ratio in concrete volume ratio and processed waste water arrange in table 3.
Table 5. different ratios sec-butyl acetate and the rear various phenol of butylacetate process, oil-contg (mg/L) and decreasing ratio (%)
From table 5, when the mixture that extraction agent is sec-butyl acetate and butylacetate, both volume ratios have significant impact for removal effect, volume ratio is preferably 1:1.8-2.2, when exceeding this scope, all will cause decreasing ratio decrease to some degree, and find most preferably to be 1:2 simultaneously.
Embodiment 4:
When the ratio of sec-butyl acetate and butylacetate is 1:2, adding other appropriate common except phenol agent, sec-butyl acetate, butylacetate, the common ratio except phenol agent are 1:2:0.1-0.3.
Extraction agent 1: butylacetate+sec-butyl acetate
Extraction agent 2: butylacetate+sec-butyl acetate+isopropyl ether
Extraction agent 3: butylacetate+sec-butyl acetate+methyl iso-butyl ketone (MIBK)
Extraction agent 4: butylacetate+sec-butyl acetate+methyl isopropyl Ketone
Extraction agent 5: butylacetate+sec-butyl acetate+methyl phenyl ketone
Table 6 butylacetate+sec-butyl acetate with common except phenol agent be combined process after
Various phenol, oil-contg (mg/L) and decreasing ratio (%)
Conclusion: from the above-mentioned data of table 6 it can be seen that with butylacetate and sec-butyl acetate suitable ratio with other except phenol agent combination obtains oil phenol extraction agent, substantially increase the extraction agent not adding sec-butyl acetate de-except dissolving oil effect in trade effluent.
Embodiment 5:
When the ratio of sec-butyl acetate and butylacetate is 1:2, adding the common degreaser that other are appropriate, the ratio of sec-butyl acetate, butylacetate, common degreaser is 1:2:0.1-0.3.
Extraction agent 1: sec-butyl acetate+butylacetate.
Extraction agent 2: sec-butyl acetate+butylacetate+normal hexane
Extraction agent 3: sec-butyl acetate+butylacetate+hexanaphthene
Extraction agent 4: sec-butyl acetate+butylacetate+octane
Extraction agent 5: sec-butyl acetate+butylacetate+pentane
Various phenol, oil-contg (mg/L) and decreasing ratio (%) after table 7 combination process
Conclusion: can find out from above-mentioned data, with sec-butyl acetate compared with the combination acquisition oil phenol extraction agent of other degreasers, the combination extraction agent of the butylacetate+sec-butyl acetate of the present invention and other degreasers three combination substantially increases the removal effect of dissolving oil in trade effluent.
Claims (8)
1. a coal chemical industrial waste water oil phenol synergistic extraction agent, it is characterised in that: described extraction agent is made up of sec-butyl acetate and butylacetate.
2. a coal chemical industrial waste water oil phenol synergistic extraction agent, it is characterised in that: described extraction agent comprises sec-butyl acetate and butylacetate.
3. coal chemical industrial waste water oil phenol synergistic extraction agent as claimed in claim 1, it is characterised in that: the volume ratio of described sec-butyl acetate and butylacetate is 1:1～6.
4. coal chemical industrial waste water oil phenol synergistic extraction agent as claimed in claim 1, it is characterised in that: the volume ratio of described sec-butyl acetate and butylacetate is 1:1～3.
5. coal chemical industrial waste water oil phenol synergistic extraction agent as claimed in claim 1, it is characterised in that: the volume ratio of described sec-butyl acetate and butylacetate is 1:2.
6. coal chemical industrial waste water oil phenol synergistic extraction agent as claimed in claim 2, it is characterised in that: the volume ratio of described sec-butyl acetate and butylacetate is 1:1～6.
7. coal chemical industrial waste water oil phenol synergistic extraction agent as claimed in claim 2, it is characterised in that: the volume ratio of described sec-butyl acetate and butylacetate is 1:1～3.
8. coal chemical industrial waste water oil phenol synergistic extraction agent as claimed in claim 2, it is characterised in that: the volume ratio of described sec-butyl acetate and butylacetate is 1:2.
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Application publication date: 20160615 |