CN104229972A - Method for removing carbamazepine in sewage by virtue of strong oxidation of Fenton technology - Google Patents
Method for removing carbamazepine in sewage by virtue of strong oxidation of Fenton technology Download PDFInfo
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- CN104229972A CN104229972A CN201310487708.XA CN201310487708A CN104229972A CN 104229972 A CN104229972 A CN 104229972A CN 201310487708 A CN201310487708 A CN 201310487708A CN 104229972 A CN104229972 A CN 104229972A
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Abstract
The invention relates to a method for removing carbamazepine in sewage by virtue of strong oxidation of a Fenton technology. The method comprises the following steps: under the condition that the pH value is 3-7, simultaneously adding nano-sized zero-valent iron and hydrogen peroxide into the carbamazepine-containing sewage, adding citric acid serving as a chelating agent, reacting for 5-40 minutes and removing carbamazepine in the sewage by virtue of oxidation, wherein the mass concentration of carbamazepine in the sewage is 1-20 mg per liter, the addition of nano-sized zero-valent iron is 0.1-1 gram per liter of the sewage, the addition of hydrogen peroxide is 100-300mg per liter of the sewage and the addition of citric acid is 5-40 mg per liter of the sewage. Compared with the prior art, the method disclosed by the invention has the advantages of simple conditions required for the reaction, mild reaction, short treatment time, high removal rate of carbamazepine and no secondary pollution and the method is suitable for treatment of carbamazepine-containing sewage and other pharmaceutical wastewater and is conductive to the resource utilization of the sewage.
Description
Technical field
The present invention relates to a kind of wastewater efficient treatment process containing Carbamzepine, especially relate to a kind of method utilizing Fenton technology Strong oxdiative to remove Carbamzepine in sewage, be specially to add in nano zero valence iron Fenton system chelator acid citrate to sewage in Carbamzepine carry out the method for efficient Strong oxdiative process.
Background technology
Medicine and Personal hygiene nursing materials are ubiquitous organic micro-pollutants in sewage, its waste water has complicated component, organic content is high, toxicity is large, the features such as the dark and biodegradability of color is poor, biological treatment difficulty is large, and it has caused extensive concern both domestic and external to the impact that environment causes.These pollutents can be transformed into polarity, deliquescent meta-bolites and acid in human body, and enter in municipal effluent along with urine and ight soil.There are some researches show, most drug pollutent is difficult to biological degradation, and most of sewage work generally only adopts two stages for the treatment of technique, seldom adopts tertiary treatment process or advanced oxidation treatment technology.Therefore, if fail to remove completely at Sewage Plant Chinese traditional medicine pollutent, the drug contamination thing remained will be caused to enter in surface water, underground water or seawater, thus the mankind are had an impact and aquatic environment is damaged.
In daily life, Carbamzepine (also known as carbadipimidine) is widely used, and it often makes for treatment epileptics and trigeminal neuralgia etc. together with other drug.Therefore, the parent of Carbamzepine and metabolite are often detected in sewage.There are some researches show, Carbamzepine well can not be removed by traditional sewage work, and finds that its clearance in sewage work is lower than 10% by inquiry.For being difficult to biodegradable drug contamination thing, in order to improve its removal effect, high-level oxidation technology is widely used, and mainly comprises: ultraviolet, ultraviolet/hydrogen peroxide, ozone, ozone/hydrogen peroxide solution etc.Previous investigator to utilizing ozone, ultraviolet and remove typical medicaments pollutent with hydrogen peroxide coupling and carried out large quantity research, but it is expensive.Relative to other high-level oxidation technology, Fenton technical price is relatively cheap, and the hydroxyl radical free radical that Fenton system produces has strong oxidizing property, does not have a selectivity, can react with the organism of 95% organic degraded.If Fe (II) is different with hydrogen peroxide concentration, the radical pair organism that also can form other form is effectively degraded, such as: perhydroxyl radical free radical, ultra-oxygen anion free radical, perhydroxy anion and organic free radical.Along with the rise of nano material in recent years, also have and nano material is introduced Fenton system, because nano material has huge specific surface area and high reactivity, speed of reaction is improved, more and more comes into one's own, and wherein popular to the research of nano zero valence iron.In traditional Fenton system, often need the pH of reaction to control at about 3-4, otherwise molysite is separated out with ferric hydroxide precipitate, thus reduce catalytic effect.In order to make reaction to carry out in neutral conditions, someone proposes, with the sequestrant of iron for catalyzer, to improve organic removal efficiency.Using maximum in traditional sequestrant is EDTA, but the biological degradability of EDTA is poor, can exist in sewage after sewage disposal, along with tail water entered environment, thus produces accumulation in the environment.There are some researches show citric acid recently as the effective sequestrant of one, have good biological degradability, can well be removed in Sewage treatment systems, can not to environmental effects.Inner complex can be formed with Fe (II) or Fe (III) in neutral conditions, thus avoid iron and separate out with precipitation forms, produce the hydroxyl radical free radical of very high density in neutral conditions, thus effectively remove organic pollutant.
At present, also citric acid is not introduced the report in nano zero valence iron Fenton system, the Carbamzepine in sewage removed, be necessary to carry out relevant research work.
Summary of the invention
Object of the present invention is exactly the defect needing reaction pH to control at 3 ~ 4 such acidic conditionss in sewage disposal application process to overcome traditional Fenton system, thus providing that a kind of reaction conditions is simple to operation, the treatment time is short, non-secondary pollution, removing the method for Carbamzepine in sewage to general sewage without the need to regulating the Fenton technology Strong oxdiative that utilizes of pH.The method can make pollutent also have good removal effect under slightly acidic or neutrallty condition, and improves speed of reaction, and industrial applications prospect is large.
Object of the present invention can be achieved through the following technical solutions:
Utilize Fenton technology Strong oxdiative to remove a method for Carbamzepine in sewage, to containing in the sewage of Carbamzepine, add nano zero valence iron and hydrogen peroxide simultaneously, and add citric acid as sequestrant, stir, reaction times 5-40 minute, the Carbamzepine in oxidation removal sewage.In Fenton system, add citric acid sequestrant to the mechanism of action of Carbamzepine is: citric acid and nano zero valence iron form the inner complex of iron, under neutrality or solutions of weak acidity, Carbamzepine is oxidized to hydroxylated Carbamzepine, and the biodegradability of hydroxylated Carbamzepine improves greatly, can well be removed in follow-up biological treatment process.
Further, in described sewage, the mass concentration of Carbamzepine is 1 ~ 20 milligrams per liter, the input amount of described nano zero valence iron adds 0.1 ~ 1 gram in often liter of sewage, the input amount of described hydrogen peroxide adds 100 ~ 300 milligrams in often liter of sewage, and the input amount of described citric acid is for adding 5 ~ 40 milligrams in often liter of sewage.
Further, before adding nano zero valence iron and hydrogen peroxide, the pH value regulating sewage is 3 ~ 7.
Further, before adding nano zero valence iron and hydrogen peroxide, the pH value regulating sewage is 6 ~ 7.
Again further, before adding nano zero valence iron and hydrogen peroxide, the pH value regulating sewage is 6..
Further, the grain diameter of described nano zero valence iron is 50 ~ 70 nanometers.
Further, in sewage, add nano zero valence iron, hydrogen peroxide and citric acid simultaneously.
Compared with prior art, the present invention has the following advantages and beneficial effect:
1, applied widely, reaction conditions is simple.The present invention adds nano zero valence iron and hydrogen peroxide to containing in the sewage of Carbamzepine, and adds citric acid as sequestrant, and sewage can not regulate pH, can reach good removal effect under normal temperature and pressure.
2, speed of reaction is fast.Because nano zero valence iron particle diameter has huge specific surface area and high reactivity, therefore speed of reaction is very fast.Just good removal effect can be had to the sewage containing mass concentration being the Carbamzepine of 1 ~ 20 milligrams per liter in 5 ~ 40 minutes.
3, processing cost is low.The present invention's oxidant hydrogen peroxide used is more cheap for other oxygenants, and consumption is few, easy and simple to handle, has a good application prospect.
4, environmental friendliness.The sequestrant that the present invention adds is can be biodegradable, for the sequestrant of other difficult degradations (as EDTA), can not cause secondary pollution to environment.
5, target compound scope is suitable for wide.The present invention, except being applicable to the sewage disposal containing Carbamzepine, is also applicable to the sewage disposal containing other drug pollutent.
Accompanying drawing explanation
Fig. 1 is that the pH value of sewage and reaction times are on the impact of Carbamzepine clearance;
Fig. 2 is that the concentration of Carbamzepine in sewage and reaction times are on the impact of Carbamzepine clearance.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
In following examples, in water sample, the analysis of Carbamzepine measures and adopts Agilent1200 high performance liquid chromatography (HPLC), and separator column adopts C18 post (250 millimeters × 4.6 millimeters, packing material size 5 microns, Supelco).Moving phase is water (adding the potassium primary phosphate that 20 mmoles often rise) and acetonitrile, and flow velocity is 1 milliliter of per minute, sample size 50 microlitre, column temperature 20 degrees Celsius, determined wavelength 280 nanometer.Eluent gradient changes, and start acetonitrile concentration and be 4096 and keep 3 minutes, in 5 minutes, acetonitrile concentration is raised to 10096 subsequently, and keep 3 minutes, last acetonitrile concentration returned 40% in 5 minutes.
Embodiment 1
Adopt in nano zero valence iron Fenton system and add the sewage that citric acid as the Strong oxdiative minimizing technology process Carbamzepine mass concentration of sequestrant to Carbamzepine in sewage is 10 milligrams per liter.
The initial pH value regulating sewage is 3, and in system, add hydrogen peroxide 200 milligrams per liter of sewage, add nano zero valence iron 0.5 gram of often liter of sewage, citric acid 20 milligrams per liter of sewage, stir, and wherein, the grain diameter of nano zero valence iron is 50 ~ 70 nanometers simultaneously.The clearance of Carbamzepine in sewage is detected when the differential responses time.
Embodiment 2
Difference from Example 1 is, the initial pH value of sewage be regulated to be 4.
Embodiment 3
Difference from Example 1 is, the initial pH value of sewage be regulated to be 5.
Embodiment 4
Difference from Example 1 is, the initial pH value of sewage be regulated to be 6.
Embodiment 5
Difference from Example 1 is, the initial pH value of sewage be regulated to be 7.
In embodiment 1 ~ 5, will detect the clearance of Carbamzepine in sewage when each embodiment is carried out when the differential responses time, result as shown in Figure 1.As seen from Figure 1, in reaction 20 minutes, under five pH conditions, Carbamzepine is higher at the clearance of the condition of pH=6 and pH=7, is greater than 94%.After adding citric acid, nano zero valence iron Fenton system has good removal effect to the Carbamzepine in sewage under slightly acidic and neutrallty condition; On the contrary under strongly acidic conditions, its removal effect is poor, is different from traditional Fenton system.
Embodiment 6
Adopt in nano zero valence iron Fenton system and add the sewage that citric acid as the Strong oxdiative minimizing technology process Carbamzepine mass concentration of sequestrant to Carbamzepine in sewage is 1 milligrams per liter.
The initial pH value regulating sewage is 6, and in system, add hydrogen peroxide 200 milligrams per liter of sewage, add nano zero valence iron 0.5 gram of often liter of sewage, citric acid 20 milligrams per liter of sewage, stir, and wherein, the grain diameter of nano zero valence iron is 50 ~ 70 nanometers simultaneously.The clearance of Carbamzepine in sewage is detected when the differential responses time.
Embodiment 7
Difference from Example 6 is, in pending sewage, Carbamzepine mass concentration is 5 milligrams per liter.
Embodiment 8
Difference from Example 6 is, in pending sewage, Carbamzepine mass concentration is 10 milligrams per liter.
Embodiment 9
Difference from Example 6 is, in pending sewage, Carbamzepine mass concentration is 15 milligrams per liter.
Embodiment 10
Difference from Example 6 is, in pending sewage, Carbamzepine mass concentration is 20 milligrams per liter.
In embodiment 6 ~ 10, will detect the clearance of Carbamzepine in sewage when each embodiment is carried out when the differential responses time, result as shown in Figure 2.As seen from Figure 2, in reaction 40 minutes, under five initial Carbamzepine concentration conditions of difference, its clearance all can reach more than 95%.The reaction times needing more to grow that just in initial sewage, Carbamazepine is high just can make its clearance reach more than 95%, and the needs that in initial sewage, Carbamazepine is low shorter reaction times can make its clearance reach more than 95%.
Embodiment 11
A kind of method utilizing Fenton technology Strong oxdiative to remove Carbamzepine in sewage, the pH value regulating sewage is 3, mass concentration to Carbamzepine is in the sewage of 1 milligrams per liter, add nano zero valence iron and hydrogen peroxide simultaneously, and add citric acid as sequestrant, the input amount of nano zero valence iron adds 0.1 gram in often liter of sewage, the input amount of hydrogen peroxide adds 100 milligrams in often liter of sewage, the input amount of citric acid adds 5 milligrams in often liter of sewage, stir, 5 minutes reaction times, the Carbamzepine in oxidation removal sewage.Wherein, the grain diameter of nano zero valence iron is 50 ~ 70 nanometers.
Embodiment 12
A kind of method utilizing Fenton technology Strong oxdiative to remove Carbamzepine in sewage, the pH value regulating sewage is 7, mass concentration to Carbamzepine is in the sewage of 20 milligrams per liter, add nano zero valence iron, hydrogen peroxide and citric acid simultaneously, the input amount of nano zero valence iron adds 1 gram in often liter of sewage, the input amount of hydrogen peroxide adds 300 milligrams in often liter of sewage, the input amount of citric acid adds 40 milligrams in often liter of sewage, stir, 40 minutes reaction times, the Carbamzepine in oxidation removal sewage.Wherein, the grain diameter of nano zero valence iron is 50 ~ 70 nanometers.
Claims (7)
1. utilize Fenton technology Strong oxdiative to remove a method for Carbamzepine in sewage, it is characterized in that, in the sewage containing Carbamzepine, add nano zero valence iron and hydrogen peroxide simultaneously, and add citric acid as sequestrant, reaction times 5-40 minute, the Carbamzepine in oxidation removal sewage.
2. a kind of method utilizing Fenton technology Strong oxdiative to remove Carbamzepine in sewage according to claim 1, it is characterized in that, in described sewage, the mass concentration of Carbamzepine is 1 ~ 20 milligrams per liter, the input amount of described nano zero valence iron adds 0.1 ~ 1 gram in often liter of sewage, the input amount of described hydrogen peroxide adds 100 ~ 300 milligrams in often liter of sewage, and the input amount of described citric acid is for adding 5 ~ 40 milligrams in often liter of sewage.
3. a kind of method utilizing Fenton technology Strong oxdiative to remove Carbamzepine in sewage according to claim 1, it is characterized in that, before adding nano zero valence iron and hydrogen peroxide, the pH value regulating sewage is 3 ~ 7.
4. a kind of method utilizing Fenton technology Strong oxdiative to remove Carbamzepine in sewage according to claim 3, it is characterized in that, before adding nano zero valence iron and hydrogen peroxide, the pH value regulating sewage is 6 ~ 7.
5. a kind of method utilizing Fenton technology Strong oxdiative to remove Carbamzepine in sewage according to claim 4, it is characterized in that, before adding nano zero valence iron and hydrogen peroxide, the pH value regulating sewage is 6.
6. a kind of method utilizing Fenton technology Strong oxdiative to remove Carbamzepine in sewage according to claim 1, it is characterized in that, the grain diameter of described nano zero valence iron is 50 ~ 70 nanometers.
7. a kind of method utilizing Fenton technology Strong oxdiative to remove Carbamzepine in sewage according to claim 1, is characterized in that, add nano zero valence iron, hydrogen peroxide and citric acid simultaneously in sewage.
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Cited By (11)
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| CN104692515A (en) * | 2015-02-04 | 2015-06-10 | 华东理工大学 | Method for removing chloro-olefin in water through strengthening activating calcium peroxide |
| CN105399281A (en) * | 2015-12-22 | 2016-03-16 | 潘豪杰 | Treatment method for removing carbamazepine in wastewater |
| CN105417786A (en) * | 2015-12-14 | 2016-03-23 | 山东凯盛新材料有限公司 | Treatment method of wastewater containing 2-chloroethyl propyl ether |
| CN105481173A (en) * | 2015-12-22 | 2016-04-13 | 潘豪杰 | Treatment system for removing carbamazepine in wastewater |
| CN106914483A (en) * | 2016-12-22 | 2017-07-04 | 常州大学 | A kind of chelating agent aids in nZVI/Na2CO4The method for cooperateing with rehabilitating soil organo-chlorine pesticide |
| CN108059228A (en) * | 2017-12-20 | 2018-05-22 | 苏州科技大学 | A kind of method of sulfamido antiseptic in removal livestock breeding wastewater |
| CN108772101A (en) * | 2018-08-16 | 2018-11-09 | 南京工业大学 | A kind of efficient metal complex molecule catalyst and its preparation and application |
| CN110773559A (en) * | 2019-11-08 | 2020-02-11 | 华中师范大学 | Method for restoring organic pollutant soil in ectopic mode through micromolecule acid coupling reduction-oxidation integration |
| CN111943347A (en) * | 2020-07-16 | 2020-11-17 | 同济大学 | Method for removing carbamazepine in wastewater by activating peracetic acid through copper ions |
| CN112661472A (en) * | 2020-12-29 | 2021-04-16 | 鄂尔多斯市固邦环保科技有限公司 | Solidification stabilizing material for water-based drill chip landfill and solidification method of water-based drill chips |
| CN112811566A (en) * | 2021-01-14 | 2021-05-18 | 昆明理工大学 | photo-Fenton reaction system and application |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104692515A (en) * | 2015-02-04 | 2015-06-10 | 华东理工大学 | Method for removing chloro-olefin in water through strengthening activating calcium peroxide |
| CN105417786B (en) * | 2015-12-14 | 2018-03-16 | 山东凯盛新材料股份有限公司 | Processing method containing 2 chloroethyl propyl ether waste water |
| CN105417786A (en) * | 2015-12-14 | 2016-03-23 | 山东凯盛新材料有限公司 | Treatment method of wastewater containing 2-chloroethyl propyl ether |
| CN105481173B (en) * | 2015-12-22 | 2017-11-24 | 吕涛 | The processing system of carbamazepine in a kind of removal waste water |
| CN107285577A (en) * | 2015-12-22 | 2017-10-24 | 潘豪杰 | The processing system of carbamazepine in a kind of removal waste water |
| CN105481173A (en) * | 2015-12-22 | 2016-04-13 | 潘豪杰 | Treatment system for removing carbamazepine in wastewater |
| CN107285577B (en) * | 2015-12-22 | 2018-03-02 | 林权豪 | The processing system of carbamazepine in a kind of removal waste water |
| CN105399281A (en) * | 2015-12-22 | 2016-03-16 | 潘豪杰 | Treatment method for removing carbamazepine in wastewater |
| CN106914483A (en) * | 2016-12-22 | 2017-07-04 | 常州大学 | A kind of chelating agent aids in nZVI/Na2CO4The method for cooperateing with rehabilitating soil organo-chlorine pesticide |
| CN108059228A (en) * | 2017-12-20 | 2018-05-22 | 苏州科技大学 | A kind of method of sulfamido antiseptic in removal livestock breeding wastewater |
| CN108772101A (en) * | 2018-08-16 | 2018-11-09 | 南京工业大学 | A kind of efficient metal complex molecule catalyst and its preparation and application |
| CN110773559A (en) * | 2019-11-08 | 2020-02-11 | 华中师范大学 | Method for restoring organic pollutant soil in ectopic mode through micromolecule acid coupling reduction-oxidation integration |
| CN111943347A (en) * | 2020-07-16 | 2020-11-17 | 同济大学 | Method for removing carbamazepine in wastewater by activating peracetic acid through copper ions |
| CN112661472A (en) * | 2020-12-29 | 2021-04-16 | 鄂尔多斯市固邦环保科技有限公司 | Solidification stabilizing material for water-based drill chip landfill and solidification method of water-based drill chips |
| CN112811566A (en) * | 2021-01-14 | 2021-05-18 | 昆明理工大学 | photo-Fenton reaction system and application |
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Application publication date: 20141224 |