CN1576244A - Reactor for efficient removing organic pollutanti in water by catalysis and ozonization - Google Patents
Reactor for efficient removing organic pollutanti in water by catalysis and ozonization Download PDFInfo
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- CN1576244A CN1576244A CN 03150149 CN03150149A CN1576244A CN 1576244 A CN1576244 A CN 1576244A CN 03150149 CN03150149 CN 03150149 CN 03150149 A CN03150149 A CN 03150149A CN 1576244 A CN1576244 A CN 1576244A
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Abstract
The reactor includes reaction glass column, ozone inlet pipe, porous quartzite ozone distributing system, catalyst column and constant temperature control system. Ozone gas in certain concentration is introduced into reaction column with organic pollutant in certain concentration loaded in advance, and mineralization and elimination of the organic pollutant may be completed in the efficiency higher than that using ozone only. When herbicide alachlor as target organic pollutant is eliminated, the catalytic ozonizing treatment can reach elimination rate as high as 98 % in 30 min and TOC eliminating rate of 90 % may reach in 180 min. The reactor has controllable catalytic ozonizing time, regenerateable catalyst, metal leaching rate less than 2 ppb and no secondary pollution to the treated water.
Description
The present invention relates to a kind of O3 catalytic oxidation and remove the reactor of organic pollutant in the water, specifically is certain density ozone gas to be evenly distributed to one by a porous air distribution plate water-filled loaded Cu/Al arranged
2O
3In the reactor that the honeycomb ceramic body of catalyzer exists, at Cu/Al
2O
3Organism under the catalysis in the oxidizing water.
In source water, underground water, surface water and trade effluent, all contain various Persistent organic pollutants to some extent, as various Insecticides (tech) ﹠ Herbicides (tech)s, sterilant and macromole soil ulmin, small molecules organic carboxyl acid etc., utilize existing water technology to be difficult to they thorough removals.In addition, Cl
2, ClO
2Deng forming a series of by products that still have toxicity and internal secretion interferon activity after the method for oxidation processing, the water after handling is caused secondary pollution; Because O
3Have stronger oxidisability, instability, become oxygen after the decomposition, so ozonize is a kind of water technology of safety.Studies have shown that independent ozone oxidation can effectively remove multiple Persistent organic pollutants, but under different pH conditions O
3Oxidizing reaction has extremely strong selectivity, and can not be CO with the thorough mineralising of most of material
2And H
2O, these materials still exist with the form that contains aromatic ring organism or small molecules organic carboxyl acid, can not thoroughly eliminate its pollution to water.The UV/O that developed recently gets up
3Method and TiO
2Persistent organic pollutants in the photocatalysis method treating water have been proved to be good effect, but because it has relatively high expectations powder TiO to reactor
2The separation difficulty of catalyzer in the water after the photocatalysis treatment, and processing cost is higher, therefore is difficult to be applied to actual water technology.Therefore, simple, efficiently, treatment process is the key that ozonize contains Persistent organic pollutants water cheaply.Studies have shown that and adopt a kind of Cu/Al
2O
3The process of catalyst ozonize Persistent organic pollutants can obtain higher TOC clearance, the organic intermediate product that produces in the ozone oxidation process can both be removed largely as containing phenyl ring organism and small molecules organic carboxyl acid (oxalic acid, acetate, propionic acid etc.) etc. separately, makes the ozone oxidation of Persistent organic pollutants in the water remove thorough more, complete.
The objective of the invention is: solve the problem that independent ozone oxidation can not be removed some organism permineralization in the water, overcome existing powder TiO
2The defective of heterogeneous catalysis ozonize cost height, separation difficulty is invented the reactor that Persistent organic pollutants in the water are removed in a kind of efficient catalytic ozonize, improves the utilization ratio of ozone in water, reaches higher mineralization of organic material efficient.
Structure of reactor of the present invention as shown in drawings.Loaded Cu/Al
2O
3Ceramic honeycomb catalyst 4, ozone reaction post 5 in recirculated water constant temperature system 6; The ozone gas that ozonizer produces is uniformly distributed in the reaction column by quartz sand porous air distribution plate 3 through inlet pipe 1, and tolerance is by intake valve 2 controls; Organism in ozone gas and the water fully reacts; Remaining ozone gas enters device for absorbing tail gas through escape pipe 9, can control air output by the adjusting of intake valve 2 and air outlet valve 8 as required; Sample is regularly taken out by thief hole 7 and analyzes alachlor concentration and TOC.
The ozone reaction post of this reactor is a diameter 30mm, the glass column of high 200mm, and the bottom is fixed with quartz sand porous air distribution plate (aperture 10 μ m), then is that load has Cu/Al on the air distribution plate
2O
3The honeycomb ceramic body of catalyzer (diameter 29mm, high 100mm).Ozone fully contacts with organism and catalyzer in the slit of honeycomb ceramic body by the porous air distribution plate, finishes the catalytic ozonation reaction.
Because the solubleness of ozone gas in water is subjected to Temperature Influence bigger, variation of temperature also can influence O greatly
3Mass transfer in water, and then can influence O largely
3The organic reaction process of oxidative degradation.Therefore, in the present invention, considered the influence of temperature to the catalytic ozonation reaction.The present invention adopts a thermostatic circulation bath to keep homo(io)thermism in the treating processes, makes processing can reach the stable treated effect within the predetermined time under identical condition of water quality.
This reactor also can be selected stainless steel for use, and distribution device uses titanium porous air distribution plate (aperture 10 μ m) to replace thereupon, tightly is fixed in the bottom of reactor with flange.Can make the ozone gas physical efficiency more even, soluble in water more expeditiously, and then ozone gas, water and catalyzer are contacted more fully, improve the efficient of catalytic ozonation reaction.Reactor diameter 70mm, high 300mm, reactor loam cake also are connected with the reactor cylinder with flange, make to be reflected under the airtight condition and carry out.Remaining ozone gas enters device for absorbing tail gas by the air outlet and carries out the tail gas absorption.
The operating process of reactor of the present invention is as follows: with ultrapure water reactor is washed several times continuously, and continue logical O in empty reactor
3About 10 minutes, remove the organic or inorganic impurity that remains on the reactor with oxidation, in order to avoid in the process of catalytic ozonation, consume O
3With alachlor is that representative target organic pollutant carries out the catalytic ozonation removal, preparing certain density alachlor solution joins in the reaction column, reactor is airtight, the reactor air valve is adjusted to required size, open ozonizer, control certain ozone flow and concentration, this moment is constantly zero as the catalytic ozonation reaction, takes a sample constantly in different reactions and analyzes.Catalytic ozonation reaction after 30 minutes alachlor can remove after about 98%, 180 minute the alachlor more than 90% and can be removed by permineralization.
Remain O in the treating processes in the water
3The measuring method of concentration is as follows: extract in an amount of reactor from the thief hole place with the syringe that finite concentration Indigo reagent is housed in advance and be dissolved with O
3Water, mix immediately, in the colorimetric estimation of 600nm place.
Characteristics of the present invention are as follows:
1, adopts quartz sand porous air distribution plate, both do not had the organism stripping, ozone gas evenly is distributed in the solution effectively, improved the utilization ratio of ozone.
2, working method is simple, facility compact, easy handling.
3, various parameters are controlled easily, can be as required conditioned reaction parameter at any time, and can be by the required tolerance of several different methods control reaction.
4, the catalytic effect of catalytic ozonation process is remarkable, can realize that the permineralization of Persistent organic pollutants in the water is removed.
5, Cu/Al
2O
3The metal stripping of solid catalyst is minimum, can not cause secondary pollution to processed water.
6, Cu/Al
2O
3Can use for several times continuously behind the solid catalyst high temperature regeneration and do not reduce catalytic effect.
7, the simple and easy investment of reactor is low, handles rear catalyst and processed water natural separation.
8, this reactor is treated the no particular restriction of pH value for the treatment of water, can be acidity, neutrality or alkaline, and the gained treatment effect all is better than the independent ozone Oxidation Treatment under the same condition of water quality.
9, this reactor also can be selected stainless steel for use, distribution device uses titanium porous air distribution plate (aperture 10 μ m) to replace thereupon, can make the ozone gas physical efficiency more even, soluble in water more expeditiously, and then ozone gas, water and catalyzer are contacted more fully, improve the efficient of catalytic ozonation reaction.
Embodiment:
Embodiment 1:
In glass reactor, add alachlor solution 75ml, adjust O
3Each parameter of producer is to set(ting)value, with the flow velocity generation O of 40ml/min
3, treat that steady air current inserts the gas reactor inlet after 2 minutes, pick up counting, the airtight oxidizing reaction of carrying out, this moment is as 0 constantly.Carrying out catalytic ozonation under the following conditions handles:
Reaction target solution volume: 75ml
Reaction target solution concentration: alachlor: 100mg/L, TOC:60mg/L
Reaction target solution temperature: 20 ℃
Reaction soln system: 0.001M phosphate buffer soln
Solution initial pH value: 7.00
O
3Concentration: 12.2mg/L/min takes place
Catalytic material: catalyst fines is carried on the cylindric material that the ceramic honey comb surface forms
Alachlor and corresponding TOC clearance are as shown in table 1 after sampling time point: 10min, 30min, 60min, 120min, 180min, the processing.
Table 1 embodiment 1 handles back alachlor and TOC clearance
Time (min) | ??10 | ??30 | ??60 | ??120 | ??180 | |
Alachlor clearance (%) | On-catalytic | ??52.3 | ??85.6 | ??90.5 | ??91.4 | ??92.8 |
Catalysis | ??68.5 | ??97.6 | ??98.5 | ??99.0 | ??99.3 | |
TOC clearance (%) | On-catalytic | ??4.61 | ??21.4 | ??31.4 | ??38.6 | ??49.3 |
Catalysis | ??5.22 | ??36.9 | ??56.4 | ??82.2 | ??87.3 |
Embodiment 2:
In glass reactor, add alachlor solution 75ml, adjust O
3Each parameter of producer is to set(ting)value, with the flow velocity generation O of 40ml/min
3, treat that steady air current inserts the gas reactor inlet after 2 minutes, pick up counting, the airtight oxidizing reaction of carrying out, this moment is as 0 constantly.Carrying out catalytic ozonation under the following conditions handles:
Reaction target solution volume: 75ml
Reaction target solution concentration: alachlor: 100mg/L, TOC:60mg/L
Reaction target solution temperature: 20 ℃
Reaction soln system: 0.001M phosphate buffer soln
Solution initial pH value: 4.30
O
3Concentration: 12.2mg/L/min takes place
Catalytic material: catalyst fines is carried on the cylindric material that the ceramic honey comb surface forms
Alachlor and corresponding TOC clearance are as shown in table 2 after sampling time point: 10min, 30min, 60min, 120min, 180min, the processing.
Table 2 embodiment 2 handles back alachlor and TOC clearance
Time (min) | ??10 | ??30 | ??60 | ????120 | ??180 | |
Alachlor clearance (%) | On-catalytic | ??45.3 | ??75.6 | ??84.9 | ????87.3 | ??89.9 |
Catalysis | ??59.4 | ??85.7 | ??93.8 | ????95.6 | ??95.8 | |
TOC clearance (%) | On-catalytic | ??1.52 | ??21.2 | ??26.2 | ????38.0 | ??48.1 |
Catalysis | ??3.93 | ??28.7 | ??47.2 | ????74.1 | ??80.8 |
Embodiment 3:
In glass reactor, add alachlor solution 75ml, adjust O
3Each parameter of producer is to set(ting)value, with the flow velocity generation O of 40ml/min
3, treat that steady air current inserts the gas reactor inlet after 2 minutes, pick up counting, the airtight oxidizing reaction of carrying out, this moment is as 0 constantly.Carrying out catalytic ozonation under the following conditions handles:
Reaction target solution volume: 75ml
Reaction target solution concentration: alachlor: 100mg/L, TOC:60mg/L
Reaction target solution temperature: 20 ℃
Reaction soln system: 0.001M phosphate buffer soln
Solution initial pH value: 9.10
O
3Concentration: 12.2mg/L/min takes place
Catalytic material: catalyst fines is carried on the cylindric material that the ceramic honey comb surface forms
Alachlor and corresponding TOC clearance are as shown in table 3 after sampling time point: 10min, 30min, 60min, 120min, 180min, the processing.
Table 3 embodiment 3 handles back alachlor and TOC clearance
Time (min) | ??10 | ??30 | ??60 | ??120 | ??180 | |
Alachlor clearance (%) | On-catalytic | ??63.7 | ??89.5 | ??92.5 | ??94.1 | ??95.3 |
Catalysis | ??70.5 | ??98.2 | ??98.7 | ??99.2 | ??99.5 | |
TOC clearance (%) | On-catalytic | ??5.05 | ??23.2 | ??37.7 | ??48.9 | ??58.4 |
Catalysis | ??10.3 | ??40.6 | ??66.9 | ??86.8 | ??89.7 |
By table 1-3 as can be known, no matter under acid, alkaline or neutrallty condition, at Cu/Al
2O
3Catalytic ozonation process under the catalyst action can both show than independent O
3Make better alachlor of time spent and TOC removal effect.
Embodiment 4:
In glass reactor, add alachlor solution 75ml, adjust O
3Each parameter of producer is to set(ting)value, with the flow velocity generation O of 40ml/min
3, treat that steady air current inserts the gas reactor inlet after 2 minutes, pick up counting, the airtight oxidizing reaction of carrying out, this moment is as 0 constantly.Carry out catalytic ozonation under the following conditions and handle (catalyzer is reused after using 500 ℃ of high temperature regenerations of several times continuously):
Reaction target solution volume: 75ml
Reaction target solution concentration: alachlor: 100mg/L, TOC:60mg/L
Reaction target solution temperature: 20 ℃
Reaction soln system: 0.001M phosphate buffer soln
Solution initial pH value: 7.00
O
3Concentration: 12.2mg/L/min takes place
Catalytic material: catalyst fines is carried on the cylindric material that the ceramic honey comb surface forms
Alachlor and corresponding TOC clearance are as shown in table 4 after sampling time point: 10min, 30min, 60min, 120min, 180min, the processing.
Table 4 embodiment 4 handles back alachlor and TOC clearance
Time (min) | ????10 | ????30 | ????60 | ????120 | ????180 |
Alachlor clearance (%) | ????68.3 | ????97.2 | ????98.3 | ????89.8 | ????99.0 |
TOC clearance (%) | ????5.03 | ????35.4 | ????55.9 | ????81.7 | ????87.1 |
As can be seen from Table 4, work as Cu/Al
2O
3Behind continuous use of catalyzer and the high temperature regeneration several times, still can show very strong katalysis.In addition from the metal stripping result that measures catalyzer this Cu/Al as can be known
2O
3Catalyzer metal stripping in use very little (less than 2ppb) illustrates catalyzer by the very firm carrier surface that is fixed in, and this has explained its lasting catalysis efficiency dry straightly.
Embodiment 5:
In glass reactor, add humic acids, oxalic acid, acetic acid mixed solution 75ml, adjust O
3Each parameter of producer is to set(ting)value, with the flow velocity generation O of 40ml/min
3, treat that steady air current inserts the gas reactor inlet after 2 minutes, pick up counting, the airtight oxidizing reaction of carrying out, this moment is as 0 constantly.Carrying out catalytic ozonation under the following conditions handles:
Reaction target solution volume: 75ml
Reaction target solution concentration: humic acids 20mg/L (DOC), oxalic acid and each 20mg/L of acetate
Reaction target solution temperature: 20 ℃
O
3Concentration: 12.2mg/L/min takes place
Catalytic material: catalyst fines is carried on the cylindric material that the ceramic honey comb surface forms
Corresponding TOC clearance is as shown in table 5 after sampling time point: 10min, 30min, 60min, 120min, 180min, the processing.
Table 5 embodiment 5 handles back TOC clearance
Time (min) | ????10 | ????30 | ????60 | ????120 | ????180 | |
TOC clearance (%) | On-catalytic | ????2.3 | ????4.8 | ????10.6 | ????15.9 | ????16.2 |
Catalysis | ????11.0 | ????31.9 | ????43.6 | ????52.8 | ????65.7 |
From the result of table 5 as can be seen: for extremely difficult humic acids, oxalic acid and the acetate of being removed by various method for oxidation mineralisings the water, this Cu/Al
2O
3The catalytic ozonation method shows remarkable advantages, the mixing TOC clearance of several materials can be improved approximately 50%, if through the sufficiently long catalytic ozonation time, TOC all should be able to be removed, reaches permineralization.
Embodiment 6:
In volume is the glass reactor of 100ml, add alachlor solution 75ml, adjust O
3Each parameter of producer is to set(ting)value, with the flow velocity generation O of 40ml/min
3, treat that steady air current inserts the gas reactor inlet after 2 minutes, pick up counting, the airtight oxidizing reaction of carrying out, this moment is as 0 constantly.Carrying out catalytic ozonation under the following conditions handles:
Reaction target solution volume: 75ml
Reaction target solution concentration: alachlor: 100mg/L, TOC:60mg/L
Reaction target solution temperature: 20 ℃
Reaction soln system: 0.001M phosphate buffer soln
Solution initial pH value: 7.00
O
3Concentration: 12.2mg/L/min takes place
Catalytic material: granules of catalyst (dosage: 250mg/L)
Alachlor and corresponding TOC clearance are as shown in table 6 after sampling time point: 10min, 30min, 60min, 120min, 180min, the processing.
Table 6 embodiment 6 handles back alachlor and TOC clearance
Time (min) | 10 | ?30 | ?60 | ?120 | ?180 | |
Alachlor clearance (%) | On-catalytic | 52.3 | ?85.6 | ?90.5 | ?91.4 | ?92.8 |
Catalysis | 66.5 | ?96.7 | ?96.9 | ?97.8 | ?98.0 | |
TOC clearance (%) | On-catalytic | 4.61 | ?21.4 | ?31.4 | ?38.6 | ?49.3 |
Catalysis | 4.91 | ?30.8 | ?45.2 | ?68.3 | ?72.4 |
As can be known from the results of Table 6, when catalyzer adds with graininess, also can obtain relatively significantly catalytic effect, but than will hanging down slightly that supported solid state is used.The shortcoming that particle adds is that the catalyst separating after handling is difficult.
Embodiment 7:
In volume is the stainless steel reactor of 1400ml, add alachlor solution 1200ml, adjust O
3Each parameter of producer is to set(ting)value, with the flow velocity generation O of 40ml/min
3, treat that steady air current inserts the gas reactor inlet after 2 minutes, pick up counting, the airtight oxidizing reaction of carrying out, this moment is as 0 constantly.Carrying out catalytic ozonation under the following conditions handles:
Reaction target solution volume: 1200ml
Reaction target solution concentration: alachlor: 100mg/L, TOC:60mg/L
Reaction target solution temperature: 20 ℃
Reaction soln system: 0.001M phosphate buffer soln
Solution initial pH value: 7.00
O
3Concentration: 12.2mg/L/min takes place
Catalytic material: catalyst fines is carried on the cylindric material that the ceramic honey comb surface forms
Alachlor and corresponding TOC clearance are as shown in table 7 after sampling time point: 10min, 30min, 60min, 120min, 180min, the processing.
Table 7 embodiment 7 handles back alachlor and TOC clearance
Time (min) | ??10 | ??30 | ??60 | ??120 | ??180 | |
Alachlor clearance (%) | On-catalytic | ??50.1 | ??82.3 | ??88.2 | ??92.5 | ??93.7 |
Catalysis | ??73.5 | ??98.2 | ??98.8 | ??99.3 | ??99.5 | |
TOC clearance (%) | On-catalytic | ??5.45 | ??23.8 | ??35.2 | ??40.0 | ??50.7 |
Catalysis | ??10.4 | ??40.1 | ??58.9 | ??84.2 | ??89.0 |
As can be known from the results of Table 7, in the reactor of stainless steel and amplification slightly, can obtain good catalytic ozonation treatment effect equally, and alachlor and TOC clearance be higher slightly than glass reactor also, this may be because titanium porous gas distribution system can obtain than littler, more even, the more stable bubble of quartz sand porous air distribution plate, and the gas-to-liquid contact area has been increased, improved processing efficiency.
Claims (4)
1. the reactor of organic pollutant in the water is removed in an efficient catalytic ozonize, it is characterized in that a kind of Cu/Al
2O
3Catalyzer is carried on the ceramic honey comb surface equably, and as the core of catalytic ozonation reaction, the catalytic ozonation that is carried out in reactor reaction can make the thorough mineralising of organic pollutant in the water.
2. according to the described reactor of claim 1, solid Cu/Al
2O
3But the catalyst fines single or multiple lift evenly is coated on honeycomb ceramic body or other porous solid carrier surface, and dissolving is few, does not come off, and ozonization is had strong katalysis.
3. according to the described reactor of claim 1, it is characterized in that used loaded Cu/Al
2O
3Catalyzer still can keep original catalytic effect through high temperature regeneration after using repeatedly.
4. according to the described reactor of claim 1, it is characterized in that, the quartz sand porous gas distribution system of reactor bottom or titanium porous air distribution plate are distributed in the reaction soln ozone gas more equably, have improved the utilization ratio and the gas-to-liquid contact area of ozone, have accelerated speed of response.
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CN100357193C (en) * | 2006-06-16 | 2007-12-26 | 中钢集团鞍山热能研究院 | Deep technique for treating charking wastewater |
CN102267756A (en) * | 2010-06-04 | 2011-12-07 | 中国科学院过程工程研究所 | Waste water deep treatment method through heterogeneous catalysis and ozone oxidation, and apparatus thereof |
CN103159316A (en) * | 2013-04-01 | 2013-06-19 | 北京科技大学 | Method for removing organic matters from water by photocatalytic ozonization |
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CN100357193C (en) * | 2006-06-16 | 2007-12-26 | 中钢集团鞍山热能研究院 | Deep technique for treating charking wastewater |
CN102267756A (en) * | 2010-06-04 | 2011-12-07 | 中国科学院过程工程研究所 | Waste water deep treatment method through heterogeneous catalysis and ozone oxidation, and apparatus thereof |
CN102267756B (en) * | 2010-06-04 | 2013-08-21 | 中国科学院过程工程研究所 | Waste water deep treatment method through heterogeneous catalysis and ozone oxidation, and apparatus thereof |
CN103159316A (en) * | 2013-04-01 | 2013-06-19 | 北京科技大学 | Method for removing organic matters from water by photocatalytic ozonization |
CN103159316B (en) * | 2013-04-01 | 2014-09-03 | 北京科技大学 | Method for removing organic matters from water by photocatalytic ozonization |
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CN104071888A (en) * | 2014-06-10 | 2014-10-01 | 南京德磊科技有限公司 | Tilting plate catalytic reaction tower |
CN104071888B (en) * | 2014-06-10 | 2015-12-09 | 南京德磊科技有限公司 | A kind of swash plate catalytic tower |
CN108423795A (en) * | 2018-03-29 | 2018-08-21 | 中国矿业大学(北京) | Efficiently catalyzing and oxidizing device |
CN113104950A (en) * | 2020-07-15 | 2021-07-13 | 昆山中环科本科技发展有限公司 | External catalyst ozone catalytic reactor and process thereof |
CN113788504A (en) * | 2021-09-30 | 2021-12-14 | 中国矿业大学 | Bismuth tungstate-based photocatalytic reactor and mineral processing wastewater degradation system |
CN113788504B (en) * | 2021-09-30 | 2022-10-04 | 中国矿业大学 | Bismuth tungstate-based photocatalytic reactor and mineral processing wastewater degradation system |
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