CN104591426B - Zero-valent Iron reduction-Fenton oxidation integrated reacting device and the method utilizing its process nitro-aromatic compound waste water - Google Patents
Zero-valent Iron reduction-Fenton oxidation integrated reacting device and the method utilizing its process nitro-aromatic compound waste water Download PDFInfo
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Abstract
The invention discloses a kind of Zero-valent Iron reduction-Fenton oxidation integrated reacting device.This reaction unit includes the reactor body in hollow cylindrical configuration, iron cement collecting region, Zero-valent Iron reducing zone, Zero-valent Iron Fenton oxidation district and the reaction of four, settling zone it is divided into from bottom to top inside reactor body, described four reaction areas is connected with each other logical, and has been abound with iron plane flower in Zero-valent Iron reducing zone and Zero-valent Iron Fenton oxidation district.The present invention, by Zero-valent Iron reduction technique and Zero-valent Iron Fenton oxidation technology coupling, maximally utilises the useful space of reactor, simplifies sewage treatment technology process, reduce operating cost；Zero-valent Iron reduction technique and Fenton oxidation technology are coupled by the present invention, and Fenton oxidation workshop section can make full use of Zero-valent Iron and reduce iron ion produced by workshop section as catalyst, improves the treatment effeciency of Fenton oxidation workshop section.
Description
Technical field
The invention belongs to technical field of sewage, be specifically related to Zero-valent Iron reduction-Fenton oxidation integrated apparatus and utilize its method processing nitro-aromatic compound waste water.
Background technology
Zero-valent Iron reduction technique and Fenton oxidation technology are two kinds of typical wastewater from chemical industry preconditioning techniques, often separately or concurrently adopt in waste water treatment process designs, can treatment effect preferably.Adopt simultaneously and generally Zero-valent Iron reduction reaction device and Fenton oxidation reaction unit are successively connected when Zero-valent Iron reduction technique and Fenton oxidation technology, reduce wastewater biological toxicity and improve the purpose of wastewater biodegradability, thus creating good condition for subsequent biochemical technique.But the design that this series connection uses needs the flow process according to setting that each independent Zero-valent Iron reduction reactor and Fenton oxidation reaction unit are coupled together, and configure a series of subsidiary conduit and facility, the connected mode of this simple superposition not only operating cost is high, processing technological flow is tediously long numerous and diverse, to controlling to require height, it is difficult to make Zero-valent Iron reduction reactor and Fenton oxidation reaction unit be simultaneously in optimal operating condition.Additionally, tradition Fenton process itself exists some defects, such as iron cement generation amount is big, and iron ion runs off serious, and iron ion utilization ratio is low；Fenton iron cement produced by Fenton technology belongs to dangerous solid waste, and subsequent treatment cost is high, and enterprise is difficult to bear.
Nitro-aromatic compound is important chemicals, is widely used in the production of the products such as explosive wastewater, pesticide, Insecticides (tech) & Herbicides (tech), dyestuff, medicine.The feature of such waste water is that salt is high, toxicity is big, complicated component, biodegradability are poor, has very big intractability, and conventional biological treatment cannot individually be worked, and there is the shortcoming such as inefficiency, poor stability.It is thus desirable to a kind of efficient pretreating process of novel economizer of exploitation, reduce the toxicity of this type of waste water and improve biodegradability, creating good treatment conditions for follow-up biochemical process.Research in recent years has shown that Zero-valent Iron-Fenton coupling technique is to realize the feasible way that nitro-aromatic compound pollutant effluents is efficiently administered.But, the shortcomings such as Fenton workshop section processing cost is high, secondary pollution is big seriously limit the practical engineering application of Zero-valent Iron-Fenton coupling technique.How to reduce additional hydrogen peroxide and the consumption of catalyst (such as ferrous iron), reduce iron cement and produce, be the technical barrier that have to overcome of Zero-valent Iron-Fenton coupling technique.
Summary of the invention
The invention provides a kind of Zero-valent Iron reduction-Fenton oxidation integrated apparatus, the redox preprocessing process of nitro-aromatic compound is realized in same reactor, and utilize ferrous original position generation effect to improve iron unilization, thus reducing iron cement growing amount.
Realizing the object of the invention technical solution is:
Zero-valent Iron reduction-Fenton oxidation integrated reacting the device of the present invention, described reaction unit includes the reactor body in hollow cylindrical configuration, iron cement collecting region, Zero-valent Iron reducing zone, Zero-valent Iron Fenton oxidation district and the reaction of four, settling zone it is divided into from bottom to top inside reactor body, described four reaction areas is connected with each other logical, and has been abound with iron plane flower in Zero-valent Iron reducing zone and Zero-valent Iron Fenton oxidation district.
Described reactor body material adopts lucite.
Being provided with aerator and spoil disposal valve in described iron cement collecting region, described spoil disposal valve is positioned at the bottom of iron cement collecting region.
Being provided with water-locator and the first dividing plate in described Zero-valent Iron reducing zone, the first dividing plate is positioned at the bottom of water-locator.
Being provided with second partition and drug feeding device in described Zero-valent Iron Fenton oxidation district, second partition is positioned at the top of drug feeding device.
Described settling zone is provided with downflow weir.
Described reaction unit is also provided with connector, is used for connecting Zero-valent Iron reducing zone and Zero-valent Iron Fenton oxidation district.
The method utilizing above-mentioned Zero-valent Iron reduction-Fenton oxidation integrated reacting device pretreatment nitro-aromatic compound waste water is: fill up iron plane flower respectively to reactor Zero-valent Iron reducing zone and Zero-valent Iron Fenton oxidation district；Nitro-aromatic compound waste water through water-locator even into reactor body, flow in the Zero-valent Iron reduction reaction district of reactor body, and move along the axis direction of reactor body, waste water is 6-10h in the water conservancy time of staying in this district, in the process, nitro-aromatic compound in waste water and Zero-valent Iron react, it may be achieved high efficiency reduction converts, and generate the amino aromatic compound being easily oxidised degraded and polymerization；When the axis direction of amino aromatic compound waste water adjustment pH value to 2.5-3.5 tailing edge reactor body continues to ascend into Zero-valent Iron Fenton oxidation district, it is 8-12h in the water conservancy time of staying in this district, the target contaminant that fraction is not reduced can continue thoroughly to be reduced, hydrogen peroxide enters Zero-valent Iron Fenton oxidation district through drug feeding device, hydrogen peroxide spends reaction to generate hydroxyl radical free radical with the iron plane of setting in Zero-valent Iron Fenton oxidation district, then reduzate obtains oxidation removal under the effect of hydroxyl radical free radical, waste water after the process of Zero-valent Iron Fenton continues to rise along the axis direction of reactor body, overflow through downflow weir, enter settling zone, reactor is discharged after stopping 4-8h.
Compared with prior art, present invention have the advantage that
(1) present invention is by Zero-valent Iron reduction technique and Zero-valent Iron Fenton oxidation technology coupling, maximally utilises the useful space of reactor, simplifies sewage treatment technology process, reduces operating cost.
(2) the Zero-valent Iron reduction-Fenton oxidation integrated apparatus of present invention design, Zero-valent Iron reduction technique and Fenton oxidation technology are coupled, Fenton oxidation workshop section can make full use of Zero-valent Iron and reduce iron ion produced by workshop section as catalyst, improves the treatment effeciency of Fenton oxidation workshop section.
(3) use of this reaction unit Fenton workshop section iron plane flower packing material, original position can produce ferrous iron, promote that ferric iron is to ferrous converted in-situ, can improve ferrous utilization ratio, reduce iron cement in Fenton's reaction process to produce, thus reducing follow-up Fenton iron cement processing cost.
Accompanying drawing explanation
Fig. 1 is the front view of integrated reacting device of the present invention, wherein, 1-iron cement collecting region, 2-aerator, 3-water-locator, 4-the first dividing plate, 5-Zero-valent Iron reducing zone, 6-connector, 7-drug feeding device, 8-second partition, 9-Zero-valent Iron Fenton oxidation district, 10-settling zone, 11-downflow weir, 12-spoil disposal valve.
Fig. 2 is the sectional view of integrated reacting device of the present invention, and wherein, A-A figure is the direction view of Fig. 1 drug feeding device 7；B-B figure is the direction view of Fig. 1 the first dividing plate 4；C-C figure is the direction view of Fig. 1 water-locator 3；D-D figure is the direction view of Fig. 1 aerator 2.
Fig. 3 is the changing trend diagram of each reaction zone target contaminant clearance in embodiment 1.
Fig. 4 is each reaction zone UV in embodiment 1254Changing trend diagram.
Fig. 5 is the changing trend diagram of each reaction zone TOC clearance in embodiment 1.
Fig. 6 is each reaction zone UV under the different hydrogen peroxide concentrations in embodiment 2254Changing trend diagram.
Fig. 7 is the changing trend diagram of each reaction zone TOC clearance under the different hydrogen peroxide concentrations in embodiment 2.
Fig. 8 is Fenton oxidation district UV under the different pH condition in embodiment 3254Changing trend diagram.
Fig. 9 is the changing trend diagram of Fenton oxidation district TOC clearance under the different pH condition in embodiment 3.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is further illustrated.
Embodiment 1: Zero-valent Iron reduction-Fenton oxidation Fourier Series expansion technique processes 2,4-dinitroanisol washes
Zero-valent Iron reduction-Fenton oxidation integrated apparatus of the present invention is as shown in Figure 1, this reaction unit includes the reactor body in hollow cylindrical configuration, reactor body adopts lucite to make, it is divided into iron cement collecting region 1, Zero-valent Iron reducing zone 5, Zero-valent Iron Fenton oxidation district 9 and the reaction of 10 4, settling zone inside reactor body from bottom to top, and is abound with iron plane flower in Zero-valent Iron reducing zone 5 and Zero-valent Iron Fenton oxidation district 9；Iron cement collecting region 1 includes spoil disposal valve 12 and aerator 2；Zero-valent Iron reducing zone 5 by the first dividing plate 4 and water-locator 3, the first dividing plate 4 is for carrying the iron plane flower of Zero-valent Iron reducing zone 5, and water-locator 3 can make waste water evenly into reactor body；Zero-valent Iron Fenton oxidation district 9 includes drug feeding device 7 and second partition 8, and drug feeding device 7 can make the acid solution of hydrogen peroxide and adjustment pH even into Zero-valent Iron Fenton oxidation district 9, and second partition 8 is for carrying the iron plane in Zero-valent Iron Fenton oxidation district 9 flower；Being provided with connector 6 between Zero-valent Iron reducing zone 5 and Zero-valent Iron Fenton oxidation district 9, this connector 6 is the filling of the dismounting for the ease of reactor body and iron plane flower；Settling zone 10 is provided with downflow weir 11.Nitro-aromatic compound wastewater biological toxicity through Zero-valent Iron reduction-Fenton oxidation pretreatment significantly reduces, and enters follow-up biochemical treatment apparatus, finally realizes process up to standard.
The present embodiment is with 2,4-dinitroanisol washes is object of study, its main polluted factors be 3% salinity (being mainly sodium chloride), methanol, 2,2, 4-dinitrophenol (DNP), 2,4-dinitroanisol (DNAN), DNFB (DNCB) etc., pH value is 7.2；This waste water CODcrUp to 34000 ± 985mg/L, DNP, DNAN, DNCB concentration respectively 110.4 ± 4.2mg/L, 123.1 ± 3.8mg/L, 249.3 ± 6.9mg/L, main difficult for biological degradation composition is DNP, DNCB and DNAN.2,4-dinitroanisol washess are entered reactor body with the flow velocity of 0.21L/h by water-locator 3, flow in Zero-valent Iron reduction reaction district 5, and move along the axis direction of reactor body, and hydraulic detention time is 8h.In the process, in waste water 2,2, 4-dinitrophenol (DNP), 2,4-dinitroanisol (DNAN), 2,4-dinitrochlorobenzene (DNCB) and Zero-valent Iron react, it may be achieved high efficiency reduction converts, and generate the amino aromatic compound being easily oxidised degraded and polymerization；When amino aromatic compound waste water continues to ascend into Zero-valent Iron Fenton oxidation district 9 along the axis direction of reactor body, the target contaminant that small part is not reduced can continue thoroughly to be reduced, and then reduzate obtains oxidation removal under the effect of hydroxyl radical free radical.The waste water hydraulic detention time in Zero-valent Iron Fenton oxidation district 9 is 10h, and hydrogen peroxide enters this district with the flow velocity of 2.1mL/h from drug feeding device 7.Fenton processed waste water continues to rise along the axis direction of reactor body, overflows through downflow weir 11, enters settling zone 10 and processes further, is discharged by outlet by the tail water after processing.
Periodically turning on aerator 2, rinsed the iron plane flower in reactor body by aeration, remove precipitate and passivation in reactor body, keep Zero-valent Iron activity, improve its utilization ratio, it is at least weekly for rinsing frequency, and aeration time is 1 minute；Rinse complete precipitation more than 30 minutes, open spoil disposal valve 12 and carry out spoil disposal.Zero-valent Iron reducing zone 5 iron plane flower replacement frequency is 2 months, and iron plane flower replacement frequency in Zero-valent Iron Fenton oxidation district is 1 month, need to take connector 6 apart, open Zero-valent Iron reducing zone and be replaced when changing Zero-valent Iron reducing zone iron plane flower.
Process 2,4-dinitroanisols (DNAN) washes by this reaction unit and can not only obtain good treatment effect, and the dosage of medicament and the generation amount of Fenton process iron cement can also be reduced.Adopt traditional Zero-valent Iron reduce-homogeneous Fenton oxidation group technology is when processing, the generation amount processing waste water iron cement per ton is 12kg, and the dosage of hydrogen peroxide (concentration by 30%) is 21.6L；Adopting Zero-valent Iron reduction-Fenton oxidation integral process described in the invention, the generation amount processing waste water iron cement per ton reduces to 3kg, and the dosage of hydrogen peroxide (concentration by 30%) is down to 10L.Visible, adopt Zero-valent Iron reduction-Fenton oxidation integral process, reagent cost and subsequent treatment cost all can significantly reduce.
At HRT=24h, it is 10mL/L that hydrogen peroxide adds concentration, and Zero-valent Iron Fenton oxidation district pH is under the reaction condition of 6, and this patent determines the clearance of DNP, DNAN, DNCB, UV in reaction system254The change of value, TOC the index such as clearance, weigh the removal effect of nitro-aromatic compound in Fourier Series expansion technique.
As seen from Figure 3, three kinds of target contaminants are behind Zero-valent Iron reducing zone, DNP, DNAN and DNCB clearance respectively 79.8%, 78.3%, 89.8%, show that Zero-valent Iron reducing zone has stronger reduction effect, nitro-aromatic compound can be reduced to amino aromatic compound expeditiously.Zero-valent Iron Fenton oxidation district is mainly used in the removal of amino aromatic compound, in addition, also removing, by continuing reduction, the target contaminant that small part is not reduced, therefore three kinds of target contaminants essentially yield after experiencing this region and remove completely, clearance is above 90%.The flocculation of settling zone or sweep effect, removes the pollutant in waste water further, DNP, DNCB and DNAN pollutant can be made all to be removed completely.
This patent adopts UV254Variation tendency weigh the overall removal effect of aromatic compound (i.e. nitro-aromatic compound and reduzate thereof).From fig. 4, it can be seen that the UV of original water sample254Value is 0.83, UV after the reaction treatment of Zero-valent Iron reducing zone254It is down to 0.55, Zero-valent Iron Fenton oxidation district's water outlet UV254Value is reduced to 0.17, settling zone water outlet UV254Value is further reduced to 0.13.Visible, through Zero-valent Iron reduction-Fenton oxidation coupling technique, the target contaminant such as DNP, DNCB and DNAN and reduzate thereof can effectively be removed.
As seen from Figure 5, waste water TOC clearance after Zero-valent Iron reducing zone processes is 12.3%, and the clearance of Zero-valent Iron Fenton oxidation district TOC of yielding water is 23.1%, and settling zone TOC of yielding water clearance is only promoted to 26.1%.Visible, Zero-valent Iron reduction-Fenton oxidation Fourier Series expansion technique is limited to waste water TOC removal effect, it primarily serves the purpose of the nitro-aromatic compounds such as removal DNAN, DNCB and DNP, and the coupling of Zero-valent Iron reduction-Fenton oxidation can realize the selectively removing of the nitro-aromatic compounds such as DNAN, DNCB and DNP.
Embodiment 2: the hydrogen peroxide concentration impact on nitro-aromatic compound removal effect
Arranging HRT=24h, Zero-valent Iron Fenton oxidation district pH is the reaction condition of 6, regulates the amount of pumping into of hydrogen peroxide in drug feeding device 7, explores different hydrogen peroxide and adds concentration to UV254The impact of the change of value and the change of TOC clearance.
As seen from Figure 6, at the UV through each reaction zone processed waste water254Value is gradually lowered, particularly in hydrogen peroxide add concentration be 10mL/L time, UV254The change of value is the most obvious, the UV of final waste water254Value is 0.14, represents and adds under concentration conditions at this hydrogen peroxide, and the removal effect of target contaminant and reduzate thereof is best.It is shown that hydrogen peroxide add concentration relatively low time, Fenton DeGrain；When hydrogen peroxide concentration is higher, Fenton oxidation effect is also suppressed.
As seen from Figure 7, the TOC clearance of each reaction zone water outlet gradually steps up, when hydrogen peroxide add concentration be 10mL/L time, the final clearance of TOC is the highest, is 26.1%, it was shown that when this hydrogen peroxide concentration, and the overall remineralization efficacy of waste water is best.
Embodiment 3: the Zero-valent Iron Fenton oxidation district pH value impact on nitro-aromatic compound removal effect
At HRT=24h, hydrogen peroxide adds under the reaction condition that concentration is 10mL/L, controls the pH value in Zero-valent Iron Fenton oxidation district by regulating the amount of pumping into of sulfuric acid solution in drug feeding device 7, explores Zero-valent Iron Fenton oxidation district pH value to this district UV254The impact of value change and the change of TOC clearance.
As seen from Figure 8, the UV of water inlet254Value is 0.84, after the process in Zero-valent Iron Fenton oxidation district, and UV254Value significantly decreases.When Zero-valent Iron Fenton oxidation district pH value is 3, the UV of water outlet254It is worth minimum, is 0.10, along with the rising of Fenton oxidation district pH value, the UV of water outlet254Value increases to some extent, when pH value rises to 6, and UV254Value increases to 0.18.Illustrate that when Zero-valent Iron Fenton oxidation district pH value is 3, the clearance of target contaminant and reduzate thereof is the highest, and the rising of pH value is unfavorable for that Fenton oxidation reacts.
As seen from Figure 9, along with the continuous rising of Zero-valent Iron Fenton oxidation district pH value, the clearance of TOC is gradually lowered.When pH value is 3, TOC clearance is the highest, is 27.8%；When pH rises to 6, the clearance of Zero-valent Iron Fenton oxidation district TOC is reduced to 23.1%.
Claims (7)
1. a Zero-valent Iron reduction-Fenton oxidation integrated reacting device, it is characterized in that, described reaction unit includes the reactor body in hollow cylindrical configuration, iron cement collecting region (1) it is divided into from bottom to top inside reactor body, Zero-valent Iron reducing zone (5), Zero-valent Iron Fenton oxidation district (9) and settling zone (10) four reaction areas, described four reaction areas is connected with each other logical, and in Zero-valent Iron reducing zone (5) and Zero-valent Iron Fenton oxidation district (9), it has been abound with iron plane flower, aerator (2) and spoil disposal valve (12) it is provided with in described iron cement collecting region (1), described spoil disposal valve (12) is positioned at the bottom of iron cement collecting region (1).
2. Zero-valent Iron reduction-Fenton oxidation integrated reacting device as claimed in claim 1, it is characterised in that the material of described reactor body adopts lucite.
3. Zero-valent Iron reduction-Fenton oxidation integrated reacting device as claimed in claim 1, it is characterized in that, being provided with water-locator (3) and the first dividing plate (4) in described Zero-valent Iron reducing zone (5), the first dividing plate (4) is positioned at the bottom of water-locator (3).
4. Zero-valent Iron reduction-Fenton oxidation integrated reacting device as claimed in claim 1, it is characterized in that, being provided with second partition (8) and drug feeding device (7) in described Zero-valent Iron Fenton oxidation district (9), second partition (8) is positioned at the top of drug feeding device (7).
5. Zero-valent Iron reduction-Fenton oxidation integrated reacting device as claimed in claim 1, it is characterised in that be provided with downflow weir (11) in described settling zone (10).
6. the Zero-valent Iron reduction-Fenton oxidation integrated reacting device as described in as arbitrary in claim 1-5, it is characterized in that, described reaction unit is also provided with connector (6), is used for connecting Zero-valent Iron reducing zone (5) and Zero-valent Iron Fenton oxidation district (9).
7. the method for the Zero-valent Iron reduction-Fenton oxidation integrated reacting device pretreatment nitro-aromatic compound waste water as described in as arbitrary in claim 1-5, it is characterized in that, fill up iron plane flower to reactor Zero-valent Iron reducing zone (5) and Zero-valent Iron Fenton oxidation district (9) respectively；Nitro-aromatic compound waste water through water-locator (3) even into reactor body, flow in the Zero-valent Iron reducing zone (5) of reactor body, and move along the axis direction of reactor body, the nitro-aromatic compound waste water water conservancy time of staying in Zero-valent Iron reducing zone (5) is 6-10h, in the process, nitro-aromatic compound in waste water and Zero-valent Iron react, and generate the amino aromatic compound being easily oxidised degraded and polymerization；When the axis direction of amino aromatic compound waste water adjustment pH value to 2.5-3.5 tailing edge reactor body continues to ascend into Zero-valent Iron Fenton oxidation district (9), the water conservancy time of staying in Zero-valent Iron Fenton oxidation district (9) is 8-12h, the target contaminant that fraction is not reduced can continue thoroughly to be reduced, hydrogen peroxide enters Zero-valent Iron Fenton oxidation district (9) through drug feeding device (7), hydrogen peroxide spends reaction to generate hydroxyl radical free radical with the iron plane of setting in Zero-valent Iron Fenton oxidation district (9), then reduzate obtains oxidation removal under the effect of hydroxyl radical free radical, waste water after the process of Zero-valent Iron Fenton continues to rise along the axis direction of reactor body, overflow through downflow weir (11), enter settling zone (10), reactor body is discharged after stopping 4-8h.
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| CN102276023A (en) * | 2011-06-21 | 2011-12-14 | 舒振华 | Method for treating organic dyestuff in wastewater |
| CN103626277B (en) * | 2013-09-13 | 2016-04-13 | 上海市环境科学研究院 | Be applicable to the Ex-situ remediation method of chloronitrobenzene class polluted underground water |
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Inventor after: Shen Jinyou Inventor after: Han Weiqing Inventor after: Zhang Hui Inventor after: Liu Jianguo Inventor after: Wang Lianjun Inventor after: Ou Changjin Inventor after: Zhang Shuai Inventor after: Sun Xiuyun Inventor after: Li Jiansheng Inventor after: Liu Xiaodong Inventor before: Shen Jinyou Inventor before: Wang Lianjun Inventor before: Liu Jianguo Inventor before: Ou Changjin Inventor before: Zhang Shuai Inventor before: Sun Xiuyun Inventor before: Li Jiansheng Inventor before: Liu Xiaodong Inventor before: Han Weiqing |
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| COR | Change of bibliographic data |