CN104944496A - Phenol removing method for sodium sulfate waste water of coal tar processing - Google Patents
Phenol removing method for sodium sulfate waste water of coal tar processing Download PDFInfo
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Abstract
The invention provides a phenol removing method for sodium sulfate waste water of coal tar processing. The method comprises the following steps that firstly, the sodium sulfate waste water and an extracting agent are added into a static mixer (1) to be fully mixed; secondly, after extracting is carried out, an obtained mixture is sent to a coalesce (2); thirdly, after the extracting is carried out, the obtained sodium sulfate waste water on the lower layer of the coalesce (2) is discharged to the downstream to be subjected to the further treatment; fourthly, the extracting agent on the upper layer of the coalesce (2) and a third-phase flocculated material generated by two-phase extracting in the middle of the coalesce (2) are sent to another static mixer (3) together, and after alkali liquor mixing is carried out, a re-extracting treatment is carried out; fifthly, after the re-extracting is carried out, an obtained mixture is sent to another coalesce (4) to be subjected to oil-water separating, and the extracting agent is sent back to a storage tank (5) to be recycled; sixthly, after the re-extracting is carried out, a sodium salt solution is processed through a sulfuric acid resolving technology.
Description
Technical field
The invention belongs to field of waste water treatment, relate to a kind of method of wastewater treatment.More particularly, relate to a kind of based on extraction, to the treatment process of the sodium sulfate wastewater produced in coal tar processing process except phenol.
Background technology
Industry phenolic wastewater mainly comes from coking, coal gas, oil refining and take phenols as the industry such as chemical industry, pharmacy of raw material, and its source is wide, harm is large, be comparatively common are one of harmful trade effluent, and difficulty of governance is larger.Phenolic wastewater is listed in one of harmful waste water of emphasis solution in China's water pollution control, and the industry such as chemical industry, oil refining content of phenol in waster is often at more than 1000mg/L.In coal tar processing process, after carrying out alkali cleaning-pickling-alkali cleaning or pickling-alkali cleaning flow process to the tarry cut containing phenol, phenol organic matter with the isolated in form of sodium phenolate out, is admitted to refining of crude phenol technique subsequently.In refining of crude phenol technique, first sodium phenolate completes oil removing, and then slow and sulfuric acid reaction decomposes, thus generates crude phenols and sodium sulfate, after standing separation, can produce a large amount of sodium sulfate wastewaters.
For phenolic wastewater treatment method, treatment technology conventional at present has physico-chemical process, comprises extraction process, absorption method, membrane separation process, distillation method etc.; Chemical method, comprises chemical precipitation method, chemical oxidization method, Wet Catalytic Oxidation Method, catalytic oxidation etc.; Biochemical process, comprises biomembrance process, activated sludge process, according to biological fluidized bed method, anaerobic process and anaerobic-aerobic combination process that activated sludge process principle produces.The absorption regeneration of absorption method and secondary pollution problem seriously limit the concrete practical application of the method.High, the easy pollution of membrane separation process price, equipment complex structure, difficult in maintenance.The steam consumption quantity of distillation method is large, and equipment is huge, and the scope be suitable for is little, lower to the clearance of some phenolic wastewater.Chemical precipitation method subsequent disposal difficulty is larger.The oxidant production cost of chemical oxidization method is high, easily form secondary pollution, makes it apply by restriction to a certain extent; Wet oxidation process is because requiring high temperature, high pressure and considerably increase cost of investment and running cost; Catalytic oxidation requires higher to the technology content of catalyzer, technology relative complex, if use noble metal, cost can be very high.Biological process is mainly applicable to the organic wastewater with difficult degradation thereby of lower concentration, microorganism can be caused normally to work even be poisoned to death for highly difficult organic wastewater with difficult degradation thereby in process.
When adopting extraction process to process phenolic wastewater; usually can there is comparatively serious emulsion; and have third phase flocculence material to generate; hinder the interaction between aqueous phase and organic phase in extraction process; affect extraction efficiency, the effect of carrying secretly of third phase also can cause the loss of organic extractant, simultaneously; the existence of third phase dirt can cause very large difficulty to production operation, impacts whole extraction process.
The sodium sulfate wastewater that this area relates to is that a kind of intractability is high, and the high-salt wastewater that toxic action is large wherein exists the crude phenols of high density, causes larger toxic action to microorganism in downstream treatment systems, causes system treatment efficiency to reduce.Therefore, this area is in the urgent need to developing a kind of simple and effective, and the phenol method that removes of environmental protection and economy effectively processes it, to reduce the pollution to environment, reduces the wastewater treatment pressure in downstream.
Summary of the invention
The invention provides a kind of sodium sulfate wastewater relating to coal tar processing of novelty except phenol method, its equipment is simple, easy to operate, efficiently can remove the very large phenol of waste water toxic rapidly, thus solve problems of the prior art.
The invention provides a kind of sodium sulfate wastewater of coal tar processing that relates to except phenol method, the method comprises the following steps:
A sodium sulfate wastewater and extraction agent add in static mixer and also fully mix by (), make the phenol in sodium sulfate wastewater be extracted in organic phase;
B () will extract the mixture that obtains and send into coalescer, carry out that breakdown of emulsion is coalescent wherein, strengthening extraction and oily water separation;
C () enters downstream be for further processing extracting the lower floor's sodium sulfate wastewater obtained in coalescer;
D upper strata extraction agent in coalescer is sent into another static mixer by () together with the third phase flocculence material produced because of two-phase extraction in the middle part of coalescer, to carry out reextraction process after mixing with alkali lye;
E mixture that () obtains stripping is sent in another coalescer and is carried out oily water separation, and wherein storage tank recycling sent back to by extraction agent; And
F the sodium phenolate solution obtained after reextraction is sent into sulfuric acid decomposition technique by ().
In one preferred embodiment, in step (a), the blending ratio of described sodium sulfate wastewater and extraction agent is 1:5 to 5:1.
Another preferred embodiment in, in step (a), described extraction agent is selected from lower group: benzene, toluene, light oil, tributyl phosphate, n-Octanol or its mixture.
Another preferred embodiment in, in step (a), described sodium sulfate wastewater and the extraction agent time of hybrid extraction in static mixer is no more than 5 minutes.
Another preferred embodiment in, described coalescer is gathering de-oiling type high efficiency oil/water separator, is made up of shell and internals, and wherein said internals comprise coalescing layer, flap separator layer and oleophobic medium layer, and replaceable.
Another preferred embodiment in, the coalescing layer in described coalescer is hydrophilic oleophobic material or oleophilic drainage material.
Another preferred embodiment in, in step (b), described oily water separation adopts Agglomeration methods, and utilize oleophilic drainage material by oil droplet absorption thereon, strengthening phase Contact and mass transfer, to improve percentage extraction.
Another preferred embodiment in, in step (d), use upper strata extraction agent to carry out stripping the static mixer of process simultaneously for alkali cleaning third phase flocculence material.
Another preferred embodiment in, in step (d), described third phase flocculence material is that other oily substances owing to also existing in sodium sulfate wastewater generate other extracted species, the third phase that multiple different extracted species jointly exists and generates when extracting.
Another preferred embodiment in, in step (d), described alkali lye is NaOH solution, and its massfraction is 10-30%, and described alkali lye is simultaneously for alkali cleaning third phase flocculence material.
Accompanying drawing explanation
Fig. 1 removes phenol method process flow sheet according to the sodium sulfate wastewater of an embodiment of the invention.
Fig. 2 is the breakdown of emulsion coalescence principle schematic diagram according to an embodiment of the invention.
Fig. 3 is the coalescer schematic diagram according to an embodiment of the invention.
Embodiment
Present inventor is through extensive and deep research, high for the sodium sulfate wastewater intractability existed in prior art, toxic action is large, the crude phenols that wherein there is high density cause larger toxic action to microorganism in downstream treatment systems, cause the problem that system treatment efficiency reduces, develop a kind of sodium sulfate wastewater of novelty except phenol method, the method is simple to operate, clear process is feasible, do not need main equipment, thoroughly can abolish emulsion, oily water separation is efficiently rapid, strengthening extraction effect, mass-transfer efficiency is high, extraction agent after back extraction can realize recycle, any pollution is not caused to waste water water body, decrease cost for wastewater treatment, phenol can be recovered utilization, turn waste into wealth, green high-efficient, economical convenient.
The invention provides a kind of sodium sulfate wastewater of coal tar processing that relates to except phenol method, the method comprises the following steps:
A sodium sulfate wastewater and extraction agent add in static mixer and also fully mix by (), make the phenol in sodium sulfate wastewater be extracted in organic phase;
B () will extract the mixture that obtains and send into coalescer, carry out that breakdown of emulsion is coalescent wherein, strengthening extraction and oily water separation;
C () enters downstream be for further processing extracting the lower floor's sodium sulfate wastewater obtained in coalescer;
D upper strata extraction agent in coalescer is sent into another static mixer by () together with the third phase flocculence material produced because of two-phase extraction in the middle part of coalescer, to carry out reextraction process after mixing with alkali lye;
E mixture that () obtains stripping is sent in another coalescer and is carried out oily water separation, and wherein storage tank recycling sent back to by extraction agent; And
F the sodium phenolate solution obtained after reextraction is sent into sulfuric acid decomposition technique by ().
Preferably, the blending ratio of described sodium sulfate wastewater and extraction agent is 1:5 to 5:1.
Preferably, described extraction agent is selected from lower group: benzene, toluene, light oil, tributyl phosphate (TBP), n-Octanol or its mixture.
Preferably, described sodium sulfate wastewater and the extraction agent time of hybrid extraction in static mixer is no more than 5 minutes.
In the present invention, described coalescer is gathering de-oiling type high efficiency oil/water separator, is made up of shell and internals, and wherein, internals comprise coalescing layer, flap separator layer and oleophobic medium layer, and internals can be changed.Described coalescer compact construction, volume is little, oil removal efficiency is high, movement-less part, long service life, effectively can process two-phase density difference and be not less than 0.01g/cm
3suspension or emulsion.Coalescing layer fibrous reticulum block coils in an annular manner, coils shaping rear net block diameter D and is larger than barrel diameter, by net block elastic network(s) block and cylinder inboard wall compact siro spinning technology, prevent gap.
In the present invention, the coalescing layer fibrous reticulum block axis in described coalescer aligns with cylindrical tube housing axis, and longitudinally can be consistent with layer of fibers during Flow of Goods and Materials, reduce resistance drop, reduce energy consumption, enlarge active surface, is easy to coarse separation.Coalescing layer fibrous reticulum block is discontinuous placement two pieces in cylindrical shell, can realize the coalescent strengthening extraction separating treatment of secondary.Coalescer adopts horizontal being placed on supporting beam.
In the present invention, the coalescing layer in described coalescer is hydrophilic oleophobic material or oleophilic drainage material.Hydrophilic oleophobic material is metal or pottery etc., and oleophilic drainage material is polypropylene or polyvinyl chloride etc.
In the present invention; described breakdown of emulsion is coalescent, oil water separation process, utilizes water different with surface tension to the wetting angle on micro-surface of selected coarse material with oil; make small particle can depart from its surface after the surface aggregate of material is grown up float or sink, thus realize being separated object.When liquid at the uniform velocity flows through oleophylic fiber, in oil-in-water/water-in-oil emulsion, oil droplet is in the wetting attachment of oleophilic drainage fiber, constantly coalescently to grow up, when water droplet flows through, little oil droplet in water is extracted by the organic extractant phase agent on oleophylic fiber, improves mass-transfer efficiency, strengthening extraction effect, oily water separation is efficiently rapid, and demulsification is obvious.
In the present invention, described upper strata extraction agent carries out the static mixer of reextraction process simultaneously for alkali cleaning third phase material.Owing to also can there are other oily substances in sodium sulfate wastewater, generate other extracted species during extraction, multiple different extracted species can generate third phase flocculence material, affects the carrying out of breakdown of emulsion agglomeration process below.In the middle part of coalescer, arrange a blowdown line, third phase is introduced the static mixer being used for alkali cleaning, after alkali cleaning, third phase is thoroughly eliminated.
In the present invention, in described coalescer, liquid stream is out-of-date, and the pressure-losses is 0.01-0.3MPa.
Preferably, extraction agent alkali lye used when static mixer is stripped in described upper strata is NaOH solution, and its massfraction is 10-20%.Described alkali lye is simultaneously for alkali cleaning third phase material.
In the present invention, described upper strata extraction agent, after stripping, can realize it and recycle; Sodium phenolate adopts sulfuric acid decomposition technique to extract meal, and can reduce the loss of phenol and sulfuric acid, cost is low, good economy performance.
In the present invention, sodium sulfate wastewater after treatment, it reduces greatly containing phenol amount, and except phenol efficiency can reach more than 95%, other oily substance is also removed in the lump, can qualified discharge, reduces waste water downstream processing pressure.
Below referring to accompanying drawing.
Fig. 1 removes phenol method process flow sheet according to the sodium sulfate wastewater of an embodiment of the invention.As shown in Figure 1, sodium sulfate wastewater and extraction agent are added in static mixer 1 and fully mixes, make the phenol in sodium sulfate wastewater be extracted in organic phase; Then coalescer 2 is sent extracting the mixture obtained into, carry out that breakdown of emulsion is coalescent wherein, strengthening extraction and oily water separation, wherein, extract the lower floor's sodium sulfate wastewater obtained in coalescer 2 to enter downstream and be for further processing, and upper strata extraction agent in coalescer 2 sends into another static mixer 3 together with the third phase flocculence material produced because of two-phase extraction in the middle part of coalescer 2, processes to carry out reextraction after mixing with the alkali lye adding static mixer 3; Then sent in another coalescer 4 by the mixture that obtains of stripping and carry out oily water separation, wherein extraction agent is sent storage tank 5 back to and is reused, and namely again mixed with sodium sulfate wastewater by pump 6 pumping, the sodium phenolate solution obtained after reextraction enters sulfuric acid decomposition technique.
Fig. 2 is the breakdown of emulsion coalescence principle schematic diagram according to an embodiment of the invention.As shown in Figure 2, water droplet is the waste water water droplet containing denier sodium sulfate after extraction, the medium and small oil droplet of oil-in-water emulsion is sodium sulfate, and on oleophilic drainage fiber, oil droplet is the little oil droplet of organic phase of extraction sodium sulfate, and oleophilic drainage fiber is polypropylene or thermovyl; When liquid at the uniform velocity flows through oleophilic drainage fiber, the little oil droplet of organic phase, in the wetting attachment of oleophilic drainage fiber, constantly coalescently to be grown up, when contains sodium sulfate waste water water droplet flows through, the little oil droplet of sodium sulfate in water can be extracted by the organic extractant phase agent on oleophilic drainage fiber, thus it is coalescent to realize breakdown of emulsion.
Fig. 3 is the coalescer schematic diagram according to an embodiment of the invention.As shown in Figure 3, described coalescer comprises: opening for feed a, inlet distributor b, rectifier c, coalescing layer medium d, a multilayer flap separator e, secondary coalescing layer medium f, hydrophobic dielectric layer g, oil collecting zone h, light phase export i and heavy out j.
The major advantage of method of the present invention is:
Easy to operate, clear process is feasible, continuously-running, and process elasticity is large; Device is simple, and do not need main equipment, floor space is little; Thoroughly can abolish emulsion, oily water separation is efficiently rapid; Oleophylic fiber has the effect of strengthening extraction, can reduce the usage quantity of extraction agent, improves mass-transfer efficiency and separation efficiency; Third phase is eliminated in alkali cleaning, ensures that extraction process carries out smoothly; Extraction agent after back extraction can realize recycle, does not cause any pollution, decrease cost for wastewater treatment to waste water water body; Phenol can be recovered utilization, turns waste into wealth, green high-efficient, economical convenient.
embodiment
The present invention is set forth further below in conjunction with specific embodiment.But, should be understood that these embodiments only do not form limitation of the scope of the invention for illustration of the present invention.The test method of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.Except as otherwise noted, all per-cent and number are by weight.
embodiment 1:
Being 40t/h containing phenol sodium sulfate wastewater flow, is 9408.5mg/L containing phenol value.Adopt benzene as extraction agent, the blending ratio of sodium sulfate wastewater and benzene is 3:1.Process of stripping is 15% with alkali cleaning third phase NaOH solution massfraction used.
Adopt the inventive method to process it, technical process as shown in Figure 1.Metabisulfite solution water quality clarification after treatment, recording it containing phenol value through bromination volumetry survey volatile phenol is 310.4mg/L.It is 96.7% that extraction removes phenol efficiency.After reextraction, can record reextraction efficiency is 95.5%.
embodiment 2:
Being 40t/h containing phenol sodium sulfate wastewater flow, is 9408.5mg/L containing phenol value.Adopt light oil as extraction agent, the blending ratio of sodium sulfate wastewater and benzene is 3:1.Process of stripping is 20% with alkali cleaning third phase NaOH solution massfraction used.
Adopt the inventive method to process it, technical process as shown in Figure 1.Metabisulfite solution water quality clarification after treatment, recording containing phenol value through bromination volumetry survey volatile phenol is 366.9mg/L.It is 96.1% that extraction removes phenol efficiency.After reextraction, can record reextraction efficiency is 96.2%.
embodiment 3:
Being 40t/h containing phenol sodium sulfate wastewater flow, is 9408.5mg/L containing phenol value.Adopt benzene+15%TBP as extraction agent, the blending ratio of sodium sulfate wastewater and benzene is 5:1.Process of stripping is 15% with alkali cleaning third phase NaOH solution massfraction used.
Adopt the inventive method to process it, technical process as shown in Figure 1.Metabisulfite solution water quality clarification after treatment, recording containing phenol value through bromination volumetry survey volatile phenol is 461.1mg/L.It is 95.1% that extraction removes phenol efficiency.After reextraction, can record reextraction efficiency is 95.3%.
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read above-mentioned teachings of the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (10)
1. relate to the sodium sulfate wastewater of coal tar processing except a phenol method, the method comprises the following steps:
A sodium sulfate wastewater and extraction agent add in static mixer (1) and also fully mix by (), make the phenol in sodium sulfate wastewater be extracted in organic phase;
B () will extract the mixture that obtains and send into coalescer (2), carry out that breakdown of emulsion is coalescent wherein, strengthening extraction and oily water separation;
C lower floor's sodium sulfate wastewater that extraction in coalescer (2) obtains is entered downstream and is for further processing by ();
Send into another static mixer (3) together with d third phase flocculence material that upper strata extraction agent in coalescer (2) and coalescer (2) middle part produces because of two-phase extraction by (), process to carry out reextraction after mixing with alkali lye;
E mixture that () obtains stripping is sent in another coalescer (4) and is carried out oily water separation, and wherein storage tank (5) recycling sent back to by extraction agent; And
F the sodium phenolate solution obtained after reextraction is sent into sulfuric acid decomposition technique by ().
2. the method for claim 1, is characterized in that, in step (a), the blending ratio of described sodium sulfate wastewater and extraction agent is 1:5 to 5:1.
3. method as claimed in claim 1 or 2, it is characterized in that, in step (a), described extraction agent is selected from lower group: benzene, toluene, light oil, tributyl phosphate, n-Octanol or its mixture.
4. method as claimed in claim 1 or 2, is characterized in that, in step (a), the time of described sodium sulfate wastewater and extraction agent hybrid extraction in static mixer (1) is no more than 5 minutes.
5. method as claimed in claim 1 or 2, it is characterized in that, described coalescer is gathering de-oiling type high efficiency oil/water separator, is made up of shell and internals, and wherein said internals comprise coalescing layer, flap separator layer and oleophobic medium layer, and replaceable.
6. method as claimed in claim 5, it is characterized in that, the coalescing layer in described coalescer is hydrophilic oleophobic material or oleophilic drainage material.
7. method as claimed in claim 1 or 2, is characterized in that, in step (b), described oily water separation adopts Agglomeration methods, and utilize oleophilic drainage material by oil droplet absorption thereon, strengthening phase Contact and mass transfer, to improve percentage extraction.
8. method as claimed in claim 1 or 2, is characterized in that, in step (d), uses upper strata extraction agent to carry out the static mixer (3) of reextraction process simultaneously for alkali cleaning third phase flocculence material.
9. method as claimed in claim 1 or 2, it is characterized in that, in step (d), described third phase flocculence material is that other oily substances owing to also existing in sodium sulfate wastewater generate other extracted species, the third phase that multiple different extracted species jointly exists and generates when extracting.
10. method as claimed in claim 1 or 2, it is characterized in that, in step (d), described alkali lye is NaOH solution, and its massfraction is 10-30%, and described alkali lye is simultaneously for alkali cleaning third phase flocculence material.
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| CN105797427A (en) * | 2016-04-25 | 2016-07-27 | 江苏德林环保技术有限公司 | Automatic liquid separating system for liquid-liquid extraction |
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Application publication date: 20150930 |