CN108314208B - Method for oxidizing and flocculating phenanthrene and coal particles in coking wastewater by using Fe (VI)/Fenton system - Google Patents
Method for oxidizing and flocculating phenanthrene and coal particles in coking wastewater by using Fe (VI)/Fenton system Download PDFInfo
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Abstract
The invention relates to the field of wastewater treatment, in particular to the field of treatment of phenanthrene and coal particles in coking wastewater. A method for oxidizing and flocculating phenanthrene and coal particles in coking wastewater by using an Fe (VI)/Fenton system comprises the steps of controlling the temperature of the coking wastewater to be treated to be 25-30 ℃, adjusting the pH value of the coking wastewater to be treated to be 5 by using sodium hydroxide or sulfuric acid, and measuring the content of the phenanthrene and coal particles in the coking wastewater to be treated; and (3) adding potassium ferrate into the coking wastewater to be treated in the first step, reacting for 40s, adding a Fenton reagent, reacting for 15min, adding sodium sulfite to terminate the reaction, standing for 60min, and filtering with a filter membrane of 0.22 mu m.
Description
Technical Field
The invention relates to the field of wastewater treatment, in particular to the field of treatment of phenanthrene and coal particles in coking wastewater.
Background
The pollutants in the coking wastewater mainly comprise organic compounds with high concentration, complex composition, toxicity and difficult degradation and carbon particles with high concentration, small particle size, light specific gravity and little negative charge. The existing various treatment processes are difficult to effectively remove the substances, reach the national first-level standard and restrict the development of enterprises. In addition, the existing coking wastewater treatment process has complex combination, more troublesome flow and longer hydraulic retention time, so that the construction cost and the operation cost are high and the management is difficult. Therefore, the technology for treating the coking wastewater and the optimization upgrading of the system are still to be further improved. The main attack direction of coking wastewater treatment is to find a new wastewater treatment technology which is high in efficiency, low in consumption, free of secondary pollution and strong in controllability.
The ferrate oxidation method utilizes the strong oxidizing property of Fe (VI) to effectively oxidize and degrade organic matters with rich electron groups in the wastewater, and simultaneously, a reduction product Fe (III) can be used as a flocculating agent to further remove pollutants in the wastewater. Research shows that ferrate can obtain higher removal rate of COD, BOD and SS under the condition of less dosage compared with ferric sulfate. According to the current research, ferrate oxidation treatment wastewater hardly generates toxic and harmful byproducts, and has wide application prospect without adverse effect on the environment. Ferrate, however, does not work well for organic materials that do not have electron rich groups in the wastewater.
The Fenton oxidation method uses OH to oxidize and remove various pollutants in the wastewater, OH can react with the pollutants without selectivity and can oxidize almost all organic pollutants in the wastewater, however, just because of the non-selectivity, a part of OH is likely to be consumed by other pollutants before reacting with target pollutants, thereby increasing the treatment cost, and in addition, the Fenton oxidation method has strict requirements on the pH value, and if Fe is used, the Fenton oxidation method has strict requirements2+Excessive COD concentration of the effluent is increased, and the wide application of the Fenton oxidation method in the actual production is restricted.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to overcome the defects of the prior art that the ferrate oxidation method and the Fenton oxidation method treat the coking wastewater.
The technical scheme adopted by the invention is as follows: a method for oxidizing and flocculating phenanthrene and coal particles in coking wastewater by using an Fe (VI)/Fenton system comprises the following steps
Controlling the temperature of coking wastewater to be treated to be 25-30 ℃, adjusting the pH value of the coking wastewater to be treated to be 5 by adopting sodium hydroxide or sulfuric acid, and simultaneously measuring the content of phenanthrene and coal particles in the coking wastewater to be treated;
and step two, adding potassium ferrate into the coking wastewater to be treated in the step one, reacting for 40s, adding a Fenton reagent, reacting for 15min, adding sodium sulfite to stop the reaction, standing for 60min, and filtering by using a filter membrane with the diameter of 0.22 mu m.
As a preferred mode: in the second step, the molar ratio of the potassium ferrate to the phenanthrene in the coking wastewater is 1:3, and the molar ratio of the hydrogen peroxide in the Fenton reagent to the phenanthrene in the coking wastewater is 2: 1.
As a preferred mode: and step two, adding sodium sulfite and sodium hydroxide to enhance the flocculation of Fe (III), wherein the molar concentration of the sodium sulfite in the solution is more than 1Mmol/L when the sodium sulfite is added, and the molar concentration of the sodium hydroxide in the solution is more than 0.1Mmol/L when the sodium hydroxide is added.
As a preferred mode: and in the second step, adding a borax-hydrochloric acid solution as a buffer solution when the potassium ferrate is added to prevent the pH from changing too fast, wherein the molar ratio of borax to hydrochloric acid in the borax-hydrochloric acid buffer solution is 5:2, and the molar ratio of potassium ferrate to borax is 1: 12.5.
The invention has the beneficial effects that: the invention constructs an Fe (VI)/Fenton system, effectively combines a ferrate oxidation method and a Fenton oxidation method, firstly adopts the ferrate oxidation method to oxidize and degrade a part of organic pollutants in the wastewater (OH in the subsequent Fenton oxidation process can be prevented from being consumed by non-target pollutants to a certain extent), and then adopts the Fenton advanced oxidation method to degrade pollutants which can not be oxidized by Fe (VI) in the earlier stage. In addition, Fe (II) is generated in the process of oxidizing pollutants by Fe (VI) in the early stage and can be used as a part of catalyst of a subsequent Fenton advanced oxidation method, so that part of water treatment cost is saved, and the subsequent Fenton oxidation process improves the removal effect of the pollutants so as to achieve the purpose of oxidizing and flocculating phenanthrene and coal particles in coking wastewater at high efficiency and low price.
Drawings
FIG. 1 shows Zeta potential on the surface of coal particles with potassium ferrate K2FeO4A schematic diagram of variation of the dosage;
FIG. 2 Zeta potential on the surface of coal particle with H2O2A schematic diagram of variation of the dosage;
FIG. 3 is a schematic diagram showing the relationship between PHE degradation rate and time in three oxidation methods ([ PHE ]]: the concentration of PHE at the reaction time t; [ PHE0]: initial concentration of PHE).
Detailed Description
Modified A of Shanxi coke-oven plant2The production wastewater is treated by the O process, the plant adds HSBEMBM microbial preparation in anaerobic, anoxic and aerobic reaction units, and adds an MBR membrane system behind the aerobic reaction unit to replace a secondary sedimentation tank behind the aerobic reaction unit, on one hand, the HSBEMBM microbial system contains a large amount of nitrobacteria and nitrosobacteria population, and compared with the traditional A process2The treatment effect of the/O process is enhanced, and on the other hand, the MBR membrane system enables the effluent quality to be more excellent and the property to be stable. However, most organic pollutants in the coking wastewater have high biological toxicity and are difficult to be degraded by microorganisms.
The Fe (VI)/Fenton system has good removal effect on phenanthrene which is a typical organic pollutant in coking wastewater, and can improve the settling property of coal particles in the coking wastewater to a certain extent and promote the flocculation and settling of the coal particles. The ferrate-Fenton combined oxidation method is used for treating raw coking wastewater of certain coking plants in Shanxi province, so that the treatment effect of the Fe (VI)/Fenton system on coking wastewater is tested.
The treatment method comprises the following steps: adding 6mmol/L potassium ferrate reagent (3mmol) into 500ml coking wastewater for pre-oxidation treatment, stirring for 40s, adding Fenton reagent, Fenton reagent hydrogen peroxide H2O2With potassium ferrate K2FeO4The molar ratio of (1) to (6) is 15min, standing for 1h after the reaction is finished, and taking supernatant to measure the water quality index.
The raw water of coking wastewater and the Chemical Oxygen Demand (COD), Suspended Solids (SS), ammonia Nitrogen (NH) after treatment by Fe (VI)/Fenton system are listed in Table 13-N) an index value. Thus, after being treated by the Fe (VI)/Fenton system,the quality of the coking wastewater is obviously improved, and the removal rates of COD, ammonia nitrogen and SS in the experiment reach 69.27%, 75.95% and 89.81% respectively. In addition, the color of the water sample treated by the Fe (VI)/Fenton system becomes obviously lighter, which shows that the Fe (VI)/Fenton system has good decolorizing effect.
TABLE 1 treatment of Focus wastewater in Fe (VI)/Fenton system
Analytical study
Optimal reaction condition of Fe (VI)/Fenton system for removing Phenanthrene (PHE)
Taking 2mL of PHE stock solution (0.0053 g of PHE is weighed and dissolved in 100mL of acetonitrile, wherein the content of acetonitrile is 2%), and diluting to 100mL by using phosphate buffer solution to obtain 6 mu mol/L PHE solution. The resulting PHE solution (containing 6. mu. mol of PHE) was placed in a 200mL beaker and washed with NaOH and H sulfuric acid2SO4After the pH value of the water sample is adjusted, a certain amount of high potassium ferrate K is added2FeO4Stock solution (weighing 0.0198g K)2FeO4100mL borax-hydrochloric acid buffer solution (0.0125M Na) dissolved at pH 92B4O7·10H2O/0.005M HCl), stirring quickly, reacting for a while, adding a certain amount of Fenton reagent (H)2O2And FeSO4·7H2O), continuing the reaction, adding excessive sodium sulfite to stop the reaction after a period of time, simultaneously adding excessive NaOH to enhance the flocculation of Fe (III), standing for 60min, filtering through a filter membrane of 0.22 mu m, and determining the PHE concentration.
Orthogonal experiments were used to explore the optimal conditions for oxidative degradation of Phenanthrene (PHE) by the fe (vi)/Fenton system. Orthogonal experiment, controlling reaction temperature at 30 deg.C, selecting pH and potassium ferrate K2FeO4Adding amount of potassium ferrate K2FeO4Reaction time, hydrogen peroxide H2O2Dosage and hydrogen peroxide H2O2Reaction time five factors, five-factor four-level orthogonal experiments were performed. TABLE 2 five factors of orthogonal experiment andfour levels. In this orthogonal experiment, FeSO was generated because Fe (VI) may be generated during reduction and excessive Fe (II) may inhibit the Fenton reaction4The dosage is zero.
Table 2 orthogonal experimental tables
The results of the orthogonality experiment are shown in table 3. The optimal reaction conditions for the ferrate-Fenton combined oxidation process can be found in the table: pH 5, potassium ferrate K in the early stage2FeO4The reaction time is 40s, and the adding ratio of the reagent is PHE to K2FeO4(n/n) ═ 3:1, the later Fenton reaction time is 15min, and the adding proportion of the reagent is PHE: H2O2，(n/n)＝1:2。
TABLE 3 results of orthogonal experiments
Influence of Fe (VI)/Fenton system on coal particle settling performance
The Zeta potential on the surface of the coal particles is selected as an index of the sedimentation performance of the coal particles, and the influence of an Fe (VI)/Fenton system on the sedimentation performance of the coal particles under different environmental factors is researched through the measurement of the Zeta potential under different conditions.
Firstly determining potassium ferrate K2FeO4The influence of the adding amount on the Zeta potential on the surface of the coal particles is determined, and then the influence of the hydrogen peroxide on the Zeta potential on the surface of the coal particles is determined.
Phosphate buffer solution is used as a solvent, the concentration of coal particles is 50g/L, the pH value is adjusted to 5, the temperature is controlled to be 25 ℃, and potassium ferrate K is added2FeO4(the adding amount is 0, 0.3, 0.5, 1, 2 and 3mmol/L respectively), standing for 1h, and collecting supernatantThe Zeta potential of the coal particles was measured by a Zeta potentiometer, and the experiment was repeated 3 times, and the results are shown in FIG. 1. It can be seen that in potassium ferrate K2FeO4When the adding amount is 0.5mmol/L, the Zeta potential absolute value on the surface of the coal particles reaches the minimum.
Phosphate buffer solution is used as a solvent, the concentration of coal particles is 50g/L, the pH value is adjusted to 5, the temperature is controlled to be 25 ℃, potassium ferrate K2FeO4 (the adding amount is 0.5mmol/L) and H2O2 (the adding amounts are 0, 1, 2, 3 and 4mmol/L respectively) are added, then the mixture is kept stand for 1H, supernate is taken, the Zeta potential of the coal particles is measured by a Zeta potentiometer, the experiment is repeated for 3 times, and the result is shown in figure 2. It can be seen that with the increase of the adding amount of H2O2, the Zeta potential on the surface of the coal particles is closer to zero, and the settling property of the coal particles is better.
Claims (3)
1. A method for oxidizing and flocculating phenanthrene and coal particles in coking wastewater by using an Fe (VI)/Fenton system is characterized by comprising the following steps: the method comprises the following steps:
controlling the temperature of coking wastewater to be treated to be 25-30 ℃, then adjusting the pH value of the coking wastewater to be treated to be 5 by adopting sodium hydroxide or sulfuric acid, and simultaneously measuring the content of phenanthrene and coal particles in the coking wastewater to be treated;
step two, adding potassium ferrate into the coking wastewater to be treated in the step one, reacting for 40s, adding a Fenton reagent, and adding FeSO in the Fenton reagent4The adding amount is zero, sodium sulfite is added after the reaction is carried out for 15min to stop the reaction, and after the reaction is kept stand for 60min, the phenanthrene concentration is measured after the filtration by using a filter membrane of 0.22 mu m;
in the second step, the molar ratio of hydrogen peroxide to potassium ferrate in the Fenton reagent is 6:1, according to the adding ratio, when the molar ratio of the added potassium ferrate to phenanthrene is 1:3, and the molar ratio of the hydrogen peroxide to phenanthrene is 2:1, the removal rate of the phenanthrene can be the highest and reaches 92.29%, when the influence of an Fe (VI)/Fenton system on the sedimentation performance of coal particles is measured, the surface Zeta potential of the coal particles is selected as an index of the sedimentation performance of the coal particles, the influence of the Fe (VI)/Fenton system on the sedimentation performance of the coal particles under different environmental factors is analyzed through the measurement of the Zeta potential under different conditions, the influence of the adding amount of the potassium ferrate on the surface Zeta potential of the coal particles is firstly determined, then the influence of hydrogen peroxide on the surface Zeta potential of the coal particles is determined, when the concentration of the coal particles is 50g/L, the adding amount of the potassium ferrate is 0.5mmol/L, the Zeta potential absolute value on the surface of the coal particles can be minimized, the Zeta potential on the surface of the coal particles is closer to zero along with the increase of the adding amount of the hydrogen peroxide, the adding amount of the hydrogen peroxide in the Fenton reagent is 3mmol/L according to the molar ratio of 6:1 of the hydrogen peroxide to the potassium ferrate, the settling property of the coal particles is good, and the purpose of cooperatively treating phenanthrene and coal particles in coking wastewater can be achieved.
2. The method for oxidizing and flocculating phenanthrene and coal particles in coking wastewater by using an Fe (VI)/Fenton system according to claim 1, wherein the method comprises the following steps: in the second step, the flocculation of Fe (III) is enhanced by adding sodium hydroxide simultaneously with the addition of sodium sulfite, wherein Fe (III) is obtained by pre-oxidation of potassium ferrate, the molar concentration of sodium sulfite in the solution is more than 1mmol/L when sodium sulfite is added, and the molar concentration of sodium hydroxide in the solution is more than 0.1mmol/L when sodium hydroxide is added.
3. The method for oxidizing and flocculating phenanthrene and coal particles in coking wastewater by using an Fe (VI)/Fenton system according to claim 1, wherein the method comprises the following steps: and in the second step, adding a borax-hydrochloric acid solution as a buffer solution when the potassium ferrate is added to prevent the pH from changing too fast, wherein the molar ratio of borax to hydrochloric acid in the borax-hydrochloric acid buffer solution is 5:2, and the molar ratio of potassium ferrate to borax is 1: 12.5.
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| CN101088926A (en) * | 2006-06-12 | 2007-12-19 | 深圳职业技术学院 | Combined water-treating farrate-fenton reagent process |
| CN202322541U (en) * | 2011-11-18 | 2012-07-11 | 谢志建 | Leachate sewage treatment equipment for municipal solid waste transfer station |
| CN102863069A (en) * | 2012-10-12 | 2013-01-09 | 中国地质大学（北京） | Composite Fenton treatment method for herbicide pesticide wastewater |
| CN104891779A (en) * | 2015-06-29 | 2015-09-09 | 北京工业大学 | Combination type efficient sludge dewatering conditioning method |
| CN106430714A (en) * | 2016-10-26 | 2017-02-22 | 上海纳旭实业有限公司 | Method for deep treatment of pesticide wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101088926A (en) * | 2006-06-12 | 2007-12-19 | 深圳职业技术学院 | Combined water-treating farrate-fenton reagent process |
| CN202322541U (en) * | 2011-11-18 | 2012-07-11 | 谢志建 | Leachate sewage treatment equipment for municipal solid waste transfer station |
| CN102863069A (en) * | 2012-10-12 | 2013-01-09 | 中国地质大学（北京） | Composite Fenton treatment method for herbicide pesticide wastewater |
| CN104891779A (en) * | 2015-06-29 | 2015-09-09 | 北京工业大学 | Combination type efficient sludge dewatering conditioning method |
| CN106430714A (en) * | 2016-10-26 | 2017-02-22 | 上海纳旭实业有限公司 | Method for deep treatment of pesticide wastewater |
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