CN101811769B - Method for treating parachloronitrobenzene waste water through liquid-liquid two-phase fluidization and ozone oxidation - Google Patents
Method for treating parachloronitrobenzene waste water through liquid-liquid two-phase fluidization and ozone oxidation Download PDFInfo
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Abstract
The invention discloses a method for treating parachloronitrobenzene waste water through liquid/liquid two-phase fluidization and ozone oxidation, which belongs to the field of organic waste water treatment. The method comprises the following steps of: in a common fluidized reactor, forming a two-phase reaction system by using ozone-loaded organic solvent and waste water; and for the waste water containing low-concentration parachloronitrobenzene, using a nontoxic inert perfluoro-solvent as an organic solvent to simultaneously perform extraction concentration and the ozone oxidation to degrade the parachloronitrobenzene in a water body in a water/organic solvent two-phase fluidization state. The organic perfluoro-solvent in the method can be separated from water and is recycled, and under the same condition, compared with the conventional water/gas two-phase reaction system, the method has the advantages that: the adding amount of ozone is reduced by over 1/2, the reaction time is shortened by over 2/3, the total removal rate of toxic organic substances is improved by over 20 percent, and the water quality of yielding water is stable. The method has the advantages of high efficiency and low-consumption treatment of the parachloronitrobenzene waste water containing the low-concentration parachloronitrobenzene, is convenient to operate in practical engineering, is easy to control, and can realize industrial production easily; therefore, the method has a high popularization application value and a very extensive prospect.
Description
Technical field
The present invention relates to a kind of method of handling parachloronitrobenzene waste water, the method for a kind of two-phase fluidization and ozone oxide treatment parachloronitrobenzene waste water of saying so more specifically.
Background technology
Along with the acceleration of Chinese Urbanization and process of industrialization, the pollution of water bodys such as underground water, surface water and domestic water is more and more serious, and water pollution and control have become the important topic of common concern.People adopt eco-friendly and green methods such as chemical synthesis route from source and fundamentally minimizing pollution on the one hand; On the other hand; To water environment pollution under the new situation, how to set up focus efficient, economic, that novel method that clean, remove up hill and dale water pollutant is also becoming domestic and international concern.Through the joint efforts and the practice of scientists, the treatment technology to pollutents such as the heavy metal in the water, suspended solid (SS), bio-degradable organic pollutant (BOD), nitrogen, phosphorus is gradually improved at present.But for being difficult to biological degradation in the polluted-water, being easy to biomagnification and having the lower concentration toxic organic pollutant that " three cause " acts on; Or the processing of some novel organic pollutants; Because of its content in water is low, be difficult to enrichment and degraded, directly restrict the reuse of treating water; Also lack highly effective method and technology at present, so new principle, new technology and the novel method of the more effective specific pollutant control of research and development are extremely urgent problems.
Handle to lower concentration difficult degradation toxic organic pollutant; Advanced oxidation water technology (AOTs) is an oxygenant with oxygen or other green hyperoxia voltinism material (as: molecular oxygen, ozone or ydrogen peroxide 50 etc.); It is one type of very ideal toxic organic pollutant control novel method; In control and elimination water body, demonstrate very tempting application prospect aspect the difficult degradation toxic organic compound, receive people's attention in recent years day by day.
In the advanced oxidation Processing Technology Research, research both at home and abroad focuses mostly on and is (light) chemical oxidization method on basis, (light) chemical oxidization method that ozone is oxygenant etc. at (light) chemical oxidization method that with the molecular oxygen is the basis, activating hydrogen peroxide.In (light) chemical oxidization method water technology that with the molecular oxygen is the basis, having high efficiency photocatalyst and technique for fixing thereof becomes the key that this technical application of restriction is promoted.Activating hydrogen peroxide has bigger advantage for (light) chemical oxidization method on basis is primarily aimed at high density, difficult degradation, poisonous and hazardous organic pollutant processing aspect; But reaction can only be carried out (pH＜3) in acidic medium based on Fenton; For the synthetic organic-fuel that extensively exists in the environment; Then be difficult to degraded with this method, needing to research and develop can activation H
2O
2Catalyzer.Ozone be oxygenant (light) chemical oxidization method because of its ozone the low solubleness of aqueous phase, unstable, organic matter degradation not thoroughly, high limitation consumes energy; Aspect water pollution control, receive very big restriction; Therefore; To the limitation of ozone method in water treatment applications, the water treatment pattern of breaking the normal procedure is researched and developed the focus that heterogeneous ozonization system has become domestic and international concern.
In actual water body, there are many OH suppressor factor, like HCO
3 -, CO
3 2-, SO
3 2-Deng, these materials influence the ozonization activity through the formation that suppresses OH, have to use excessive ozone in order to eliminate the influence of these materials in single-phase (water) reaction system.Therefore, how improving solubleness, stability, the service efficiency of ozone in system, reduce production of by-products, is the critical bottleneck of restriction ozone in water pollution control field large-scale application.
So far; In overwhelming majority's report, all adopt water/organic solvent two phase oxidation reaction systems, and use straight chain perfluoro alkane more (like FC40; FC77 etc.), and use PFD (C10F18) solvent also rarely to report as the research of organic phase as organic phase.PFD (C10F18) is a kind of perfluoro naphthenic hydrocarbon; Have unreactiveness, thermostability, density greatly, at room temperature can dissolve multiple gases in a large number, the boiling spread, nontoxic even as artificial plasm's staple of broad is arranged; Be widely used as environment-friendly material, but also do not appear in the newspapers as the ozone oxidation degraded of carrying the ozone organic solvent and being used for water body lower concentration toxic organic pollutant.
Result of study shows that general water treatment device by ozone oxidation only is applicable to the organic waste water of higher concentration, and the existence that suppressed by the water body radical influences greatlyyer, generally only is used for water body disinfection and handles.Poisonous organic wastewater for the difficult degradation lower concentration adopts conventional ozone or ozone-biological treatment to be difficult to reach processing requirements, feeds a large amount of ozone usually or prolongs oxidization time, has improved working cost so greatly.Single ozone equipment for treating water, energy consumption is bigger, and can only handle the organism (as: phenol etc.) that is prone to degraded or disinfect as the follow-up of other treatment processs.For ozone-bioactive carbon treatment system, can be directed against the degraded of the lower concentration toxic organic compound in the water body, but the activated carbon surface absorption property receives water quality impact bigger; Be easy to fouling, activated carbon regeneration difficulty needs special biological degradation flora for difficult degradation toxic organic compound thing; And it is active affected by environment bigger; Particularly for containing high-salt wastewater, can't use this treatment system, be the major obstacle of restriction practical engineering application at all.Ozone-catalyst (metal) treatment system has the high advantage of ozone oxidation speed, but need to consume a large amount of ozone and expensive catalysts, and catalyst activity receives water quality impact bigger, inactivation easily, regeneration difficulty.Ozone-physical chemistry auxiliary (light, ultrasonic, Fenton, magnetic, energetic ion radiation) is though treatment system ozone oxidation speed is high, and energy consumption height, processing cost are high.Particularly to containing the waste water of lower concentration difficult degradation toxic organic compound, its processing cost is higher.
Therefore, lower concentration difficult degradation toxic organic compound water treatment method and technology that cost of development is low, efficient is high, the development trend and the effective way of also current just solution lower concentration difficult degradation poisonous organic wastewater.
Summary of the invention
1. invent the technical problem that will solve
, poor stability low to ozone solubleness in water (single-phase), lack selective oxidation, problem such as intermediate product is more and ozone utilization rate is on the low side; The present invention proposes the method for a kind of liquid/liquid two-phase ozone Oxidation Treatment parachloronitrobenzene waste water, the method for organic solvent/water two phases of carrying ozone (being called for short liquid/liquid two phases) fluidization treatment parachloronitrobenzene waste water of ability efficient and cost-effective purified industrial organic pollutant, realization industrial applications.
2. technical scheme of the present invention:
Principle: the reaction process of two-phase system mainly is made up of two portions: from liquid phase, extract toxic organic compound; In organic phase, carry out the ozone degradation reaction.Consider from using actual angle; Except that water, require below nonaqueous phase (organic phase) must satisfy: organic solvent is water insoluble, nontoxic, vp is lower, density is high, easily separated, can be recycled, the aqueous phase organic pollutant is had high slective extraction property, higher ozone solution property and stability etc. are arranged.
A kind of liquid/liquid two phase two-phase fluidizations are handled the method for parachloronitrobenzene waste water; In the organic solvent/water two-phase fluidization and ozone water processing reactor of ozone; For concentration less than 500mg/L parachloronitrobenzene waste water; Use the nontoxic inertia perfluorinated cycloalkanes that carries ozone as organic solvent, carry out extracting and enriching-ozone Oxidation Treatment simultaneously.
According to the concentration and the wastewater flow rate of parachloronitrobenzene, select consumption, water intake mode and the fluidized reaction time (or water retention time) of organic solvent in reactor drum.Generally speaking, the waste water saltiness is unrestricted, and parachloronitrobenzene concentration is below 500mg/L, and water and perfluor volume of organic solvent ratio are 1: 1～1: 3 scope.
Can select the kind and the consumption of organic solvent according to toxic organic compound in the concentration of aqueous phase and at the partition ratio of liquid/liquid two in mutually; The perfluor organic solvent is water insoluble; Be easy to water sepn and recycle; In reactor drum, play extraction-inrichment; Parachloronitrobenzene in can the extracting and enriching a large amount of water, and the perfluor organic solvent also is the good ozone solvent that carries, and the solubleness of ozone in organic solvent is about 15 times in the water.Therefore, under liquid/liquid two-phase state, in the perfluoro solvent organic phase, the high density parachloronitrobenzene after ozone with high concentration molecule and the enrichment directly carries out the addition oxidizing reaction, has good selectivity, and speed of reaction is high; At aqueous phase, the ozone molecule of transferring in the water forms offensive radical (as: hydroxyl radical free radical etc.) in decomposition course, can carry out non-selective attack organic molecule, i.e. indirect oxidation reaction; In entire reaction course, because of C-F key bond energy is very high, the perfluor organic solvent is not participated in ozone oxidation reaction; Be good inert organic solvents, in this system, direct addition oxidizing reaction and indirect oxidation reaction are carried out simultaneously; Therefore, in this reaction system, under equal conditions; Traditional water/gas two phase oxidation reaction systems are compared, and the ozone dosage reduces more than 1/2; Reaction times shortens more than 2/3, and the total clearance of toxic organic compound improves more than 20%, and stable effluent quality.
3. beneficial effect
The present invention provides the method for a kind of liquid/liquid two-phase ozone Oxidation Treatment parachloronitrobenzene waste water, has proposed a kind of method of the brand-new ozone PFD organic solvent/quick oxidative degradation parachloronitrobenzene of water two-phase fluidization waste water first.Technology is made simple, and energy consumption is low, and processing cost is low, and is easy to operate in the actual engineering, is easy to control, is easy to realize suitability for industrialized production.
Technology of the present invention has efficiently, the advantage of lower concentration parachloronitrobenzene waste water is handled in low consumption, thereby has bigger application value, and prospect is very wide.The present invention also can be applicable to the ozone oxidation degraded of many phenyl ring aromatics, organophosphorus or organic nitrogen pesticide, microbiotic, estrogens, halogenated aryl hydrocarbon class, phenols (phenol, chlorophenol, p-nitrophenol) etc., and these compounds extensively are present in key industry waste water such as domestic chemical industry, medicine, electronics, food or the city reuse water.
Description of drawings
Fig. 1 is that the present invention handles parachloronitrobenzene waster water process schema.
Embodiment
The present invention can adopt common reactor drum with stirring or fluidization system; In certain volumetrical organic solvent is arranged, can confirm size, organic solvent usage quantity and the extracting and enriching-ozone oxidation reaction time of reactor drum according to handling water yield size and toxic organic compound concentration and the partition ratio of parachloronitrobenzene in water and oil phase thereof.If must carry out when SS concentration is higher than 20mg/L in the treating water (as: micro-filtration processing etc.) after the pre-treatment, reach below the 10mg/L, adopt the inventive method to handle again.Present method is influenced by the saltiness in the waste water hardly.
Embodiment 1
Use the common reactor drum with fluidization system, its device connects ozonizer.The organic waste water that is processed is parachloronitrobenzene waste water, and the water yield is lower than 20m
3/ d, concentration is below the 10mg/L, and ozonizer is 3.0g/h, and the volume ratio of water and PFD is 1: 1 in the two-phase reactor; To perfluoro solvent preaeration, intermittent type advances waste water in fluidized reactor, and carries out fluidisation, and the fluidized reaction time is 20～30min; Stop fluidisation, leave standstill, strain water after PFD and the water sepn; And then aeration and water inlet, getting into next working cycle, the parachloronitrobenzene clearance can reach more than 90%.
Embodiment 2
Use the common reactor drum with fluidization system, its device connects ozonizer.The organic waste water that is processed contains parachloronitrobenzene, and the water yield is lower than 20m
3/ d, parachloronitrobenzene concentration is below the 100mg/L, and ozonizer is 5.0g/h, and the volume ratio of water and PFD is 1: 2 in the two-phase reactor; To perfluoro solvent preaeration, intermittent type advances waste water in fluidized reactor, and carries out fluidisation; The fluidized reaction time is 20～30min, stops fluidisation, leaves standstill; Strain water after PFD and the water sepn, and then the water inlet and get into next working cycle, the parachloronitrobenzene clearance can reach more than 90%.
Embodiment 3
Use the common reactor drum with fluidization system, its device connects ozonizer.The organic waste water that is processed contains parachloronitrobenzene waste water, and the water yield is greater than 20m
3/ d, concentration is below the 100mg/L, ozonizer is 8.0g/h; The volume ratio of water and PFD solvent is 1: 2 in the two-phase reactor, and to perfluoro solvent preaeration, intermittent type advances waste water in fluidized reactor; And carry out fluidisation, the fluidized reaction time is 20～30min, water outlet then; Get into water/PFD separation cell, the PFD after the separation recycles, and the parachloronitrobenzene clearance can reach more than 90%.
Embodiment 4
Use the common reactor drum with fluidization system, its device connects ozonizer.The organic waste water that is processed is for mainly containing parachloronitrobenzene waste water, and the water yield is lower than 20m
3/ d, parachloronitrobenzene concentration is below the 500mg/L, and ozonizer is 10g/h, and the volume ratio of water and PFD solvent is 1: 3 in the two-phase reactor; To PFD preaeration, intermittent type advances waste water in fluidized reactor, and carries out fluidisation; The fluidized reaction time is 20～30min, stops fluidisation, leaves standstill; Strain water after PFD and the water sepn, and then the water inlet and get into next working cycle, the parachloronitrobenzene clearance can reach more than 90%.
Claims (4)
1. the method for liquid/liquid two-phase ozone Oxidation Treatment parachloronitrobenzene waste water; It is characterized in that in common fluidized reactor; Use the nontoxic inertia perfluorinated cycloalkanes that carries ozone as organic solvent, form two-phase system with containing parachloronitrobenzene waste water, under fluidized state; Less than 500mg/L parachloronitrobenzene waste water, carry out extracting and enriching-ozone Oxidation Treatment for concentration simultaneously.
2. the method for processing parachloronitrobenzene waste water according to claim 1 is characterized in that the waste water saltiness is unrestricted, and parachloronitrobenzene concentration is below 500mg/L, and water and perfluor cycloalkanes volume of organic solvent ratio are 1: 1～1: 3.
3. the method for processing parachloronitrobenzene waste water according to claim 2 is characterized in that perfluor cycloalkanes organic solvent is the PFD organic solvent.
4. according to the method for each described processing parachloronitrobenzene waste water in the claim 1～3; It is characterized in that carrier gas ozone at first carries out aeration to the perfluor organic solvent and reaches capacity; General aeration time 20～30min; The perfluoro solvent that contains saturated ozone gets into common fluidized reactor, and carries out fluidisation, and fluidisation time or reaction times are 10～30min.
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| CN2010101395077A CN101811769B (en) | 2010-04-02 | 2010-04-02 | Method for treating parachloronitrobenzene waste water through liquid-liquid two-phase fluidization and ozone oxidation |
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| CN110713249A (en) * | 2019-11-01 | 2020-01-21 | 云南大学 | Method for treating hardly biodegradable organic wastewater |
| CN111054306A (en) * | 2019-11-19 | 2020-04-24 | 南京师范大学 | Modified biochar and preparation method and application method thereof |
| CN115594357B (en) * | 2022-11-08 | 2024-04-19 | 煤炭科学技术研究院有限公司 | Fractional treatment method for acylated wastewater |
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|---|---|---|---|---|
| US4793931A (en) * | 1987-09-10 | 1988-12-27 | Solarchem Research, A Division Of Brolor Investments Limited | Process for treatment of organic contaminants in solid or liquid phase wastes |
| CN101514044A (en) * | 2009-03-17 | 2009-08-26 | 南京师范大学 | Method for treating low-concentration nitrobenzene waste water by means of three-phase fluidization |
| CN201347378Y (en) * | 2009-01-07 | 2009-11-18 | 南京师范大学 | Batch-type three-phase-fluidization ozone oxidation reactor |
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| US7547388B2 (en) * | 2004-07-20 | 2009-06-16 | Think Village-Kerfoot, Llc | Superoxidant poiser for groundwater and soil treatment with in-situ oxidation-reduction and acidity-basicity adjustment |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4793931A (en) * | 1987-09-10 | 1988-12-27 | Solarchem Research, A Division Of Brolor Investments Limited | Process for treatment of organic contaminants in solid or liquid phase wastes |
| CN201347378Y (en) * | 2009-01-07 | 2009-11-18 | 南京师范大学 | Batch-type three-phase-fluidization ozone oxidation reactor |
| CN101514044A (en) * | 2009-03-17 | 2009-08-26 | 南京师范大学 | Method for treating low-concentration nitrobenzene waste water by means of three-phase fluidization |
Non-Patent Citations (1)
| Title |
|---|
| 徐腾娇等.臭氧氧化降解水中对硝基氯苯的效能与机制.《水处理技术》.2007,第33卷(第1期),第27-30页. * |
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