CN101745197B - Method of treating refractory pollutants through catalyzing H2O2 oxidation by pyrite cinder - Google Patents
Method of treating refractory pollutants through catalyzing H2O2 oxidation by pyrite cinder Download PDFInfo
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Abstract
A method of treating refractory pollutants utilizes the pyrite cinder as catalyst which forms a heterogeneous Fenton system with H2O2 to catalyze H2O2 to generate hydroxyl radical (.OH) with strong oxidability and degrade the organic pollutants efficiently and quickly. The method comprises the following steps: (1) after the waste water is added in a reactor, a given amount of pyrite cinder original sample or activated and pretreated cinder is added in the waste water; (2) H2O2 solution is added in a mixed liquid of the waste water and the pyrite cinder so as to form an analogous Fenton reagent with the pyrite cinder; (3) stirring is carried out so as to lead the pyrite cinder, the H2O2 solution and the waste water to be mixed for reaction, and the stirring is stopped at the set reaction time; and (4) standing is carried out, the pyrite cinder is quickly precipitated and the supernate is discharged, so that the pyrite cinder can be reused. The invention discovers a novel analogous Fenton oxidation catalyst, extends the resource utilization ways of the pyrite cinder, achieves the purpose of controlling waste by waste and realizes the comprehensive utilization of the waste.
Description
Technical field
The invention belongs to the environment-friendly engineering technical field, relate to the method that a kind of advanced oxidation is removed pollutant, be suitable for reparation water pollution control and polluted water body.
Background technology
The Fenton oxidation technology is the high-level oxidation technology with unique advantage, the required mild conditions such as temperature and pressure of its reaction, is swift in response, and has become one of research focus in the environmental area.The basic principle of Fenton reagent is to pass through Fe
2+And H
2O
2Between chain reaction catalysis generate and to have the very hydroxyl radical free radical OH of high oxidative capacity, its oxidizing potential is only second to fluorine, up to 2.80v.In addition, hydroxyl radical free radical OH also has very high electronegativity and electrophilicity, thereby Fenton reagent can effectively be removed the hardly degraded organic substance that traditional wastewater processing technology can't be removed.
Present Fenton method mainly contains following shortcoming and restricted it and apply: the utilization rate of a. hydrogen peroxide is lower, though by introducing technology such as ultraviolet light, ultrasonic, microwave, can improve the utilization rate of hydrogen peroxide, but it all is in the laboratory research stage, and is unsuitable for large-scale through engineering approaches application; B. reaction needs to carry out under acid condition, and still need regulate the pH value after the reaction to neutral, has increased operating cost; C. catalyst can not reuse, and Fe in the treatment fluid (II) is difficult to reclaim and produce unnecessary sediment and separates and problem such as storE, and excessive Fe ion may produce secondary pollution.
People studies show that, remove Fe
2+Can catalysis H
2O
2Decomposite outside the OH, some other transition metal ions such as Co, Cd, Cu, Ag, Mn, Ni etc. can quicken or alternative Fe
2+Play this effect, the Fenton-like system of utilizing flyash, chromium to cook and stir etc. as catalyst in addition also has the research report.Chinese patent " a kind of method with the flyash degradation of organic waste water " (CN1837076A) discloses a kind of technology of handling organic wastewater with flyash as the Fenton-like of catalyst, this technology has promptly been utilized the adsorption property of flyash, has utilized the transition metal oxides such as di-iron trioxide that contain in the flyash again.Under acid condition, these transition metal oxides are partly dissolved the generation transition metal ions.Transition metal ions can form Fenton-like reagent with hydrogen peroxide, produces the extremely strong hydroxyl radical free radical of oxidisability, and flyash obtained recycling as a kind of discarded object, reaches the effect of the treatment of wastes with processes of wastes against one another.But it needs to regulate the pH value before and after reaction, increased operating cost, and do not solve the recycling problem of catalyst, reacted flyash has increased its intractability owing to it has adsorbed pollutant, and the ferriferous oxide content in the flyash is very low, and effectively the catalyst component deficiency causes catalytic efficiency not high.Improved treatment effect although engage simultaneously microwave technology, it has increased processing cost, and is not suitable for the through engineering approaches application.Chinese patent " Fenton and Fenton-like reaction catalyst regeneration and recycling method " (CN 101491771A) discloses a kind of chemical method regeneration and the new technology that reclaims Fenton and Fenton-like catalysts, this technology is by adding the alkali neutralization precipitation to the waste water after Fenton and the Fenton-like processing, obtain iron containing sludge, and then its dehydration, drying, calcination handled obtain the iron residue, obtain ferrum sulfuricum oxydatum solutum with dilute sulfuric acid dissolved iron residue again, utilize this ferrum sulfuricum oxydatum solutum as the Fenton-like catalyst for reaction.This technology can be removed the organic matter in the iron containing sludge, avoids secondary pollution; The ferrum sulfuricum oxydatum solutum that obtains can be used as the Fenton-like catalyst for reaction and uses.But the recycling process of its catalyst is loaded down with trivial details, and need repeatedly regulate the pH value, and complex process causes cost to improve, and does not solve the key issue of restriction Fenton technical development.
Pyrite cinder is called sulfate slag, pyrite cinder again, is that the chemical plant utilizes pyrite (FeS
2) what is called " waste residue " of discharging when producing sulfuric acid.Behind boiling roaster, most S have been transformed into SO to sulphur ore in the relieving haperacidity process
2, and finally generate H
2SO
4, and whole Fe and be present in other metallic elements in the concentrate originally and all remain in and burn in the slag almost.So main component is Fe in the burning slag, general content also contains other elements such as Si, Ca, Mg, Mn, Cu, Zn in addition 30%～55%.Essential mineral is magnetic iron ore, bloodstone, maghemite, quartz etc.Generally be that it is refined into the smart powder of iron as iron-smelting raw material for the pyrite cinder utilization at present, or produce the products such as ferric oxide red colorant, Polyferric Sulfate coagulant, cement additire.Because the pyrite cinder of China is of poor quality, sorting is difficult, the investment of utilization is big, the high in cost of production problem, and the pyrite cinder comprehensive utilization is unsatisfactory, exists at present or as a kind of solid waste.
Summary of the invention
Deficiency for existing Fenton technology, and the characteristic of pyrite cinder, seminar's research is found, owing to contain the multiple transition metal such as Fe, Mn, Co, Cu, Zn in the slag, and the Fe component mainly exists with the form of the iron-bearing minerals such as magnetic iron ore, its in wider pH scope to H
2O
2All have preferably catalytic activity, and be easy to precipitate and separate.By system research, find pyrite cinder and H
2O
2Combination can form effective Fenton-like oxidation technology, and by slag being carried out can obviously improve behind the activating pretreatment catalytic performance of slag, improves reaction efficiency.Use pyrite cinder to yet there are no bibliographical information as the method for Fenton-like catalyst.
The object of the present invention is to provide that a kind of technology is simple, treatment effeciency is high, as heterogeneous Fenton-like catalyst organic matter is carried out the efficient method of degraded fast with pyrite cinder, can overcome the shortcoming that traditional F enton reaction can only be carried out, catalyst can not reuse under acid condition; And pyrite cinder is a kind of chemical industry discarded object, utilizes its to handle pollutant, can either solve its disposal concerns, reached the purpose of the treatment of wastes with processes of wastes against one another again, realized comprehensive utilization of waste materials.
Solution of the present invention is: utilize pyrite cinder as catalyst, with H
2O
2Consist of heterogeneous Fenton-like system, catalysis H
2O
2Produce the extremely strong hydroxyl radical free radical OH of oxidisability, to pollutant carry out efficiently, fast degradation, and by slag being carried out its reactivity worth of raising after the preliminary treatment.
The concrete steps that realize the inventive method are:
A. after waste water being added reactor, the slag in waste water behind a certain amount of pyrite cinder former state of adding or the process activating pretreatment; Further, the activating pretreatment step of slag is: after pyrite cinder low rate mixing in being added with the dilute hydrochloric acid solution of 0.01～1%NaCl is soaked 1h, take out and with using after clear water flushing, the oven dry.The addition of burning slag is 5g/L～30g/L;
B. in waste water and pyrite cinder mixed liquor, add H
2O
2, form Fenton-like reagent, H with pyrite cinder
2O
2Addition be 0.05mol/L～0.3mol/L;
C. stir, make pyrite cinder and H
2O
2Mix with waste water, react, stop after the reaction time that arrival is set stirring.(at different waste water, the reaction time is different, mainly determines the reaction time according to experimental result, is generally 1～24h.)
D. leave standstill, pyrite cinder precipitates rapidly, discharges supernatant, and the pyrite cinder of precipitation can reuse; Water sample after processing is carried out water analysis, detect the pollutant levels in the waste water, BOD, COD, pH, colourity etc. are with the evaluation process effect.
Advantage of the present invention comprises:
A. the initial pH of reaction pair does not have specific (special) requirements, and applicable pH range is very wide, and initial pH has reaction effect preferably at 1-11, and initially pH is in the 3-11 scope, and reacted pH is at neutral range.Therefore in the ordinary course of things, need not to regulate the pH value before and after the reaction, can greatly simplify technology and save cost.
B. pyrite cinder is a graininess, because density is bigger than water, and stable in properties, be easy to Separation of Solid and Liquid.
C. this heterogeneous Fenton-like reaction is a kind of surface-catalyzed reactions, and catalyst does not consume in course of reaction, and catalytic activity is still very high after reacting, and can reuse.
D. pyrite cinder contains multiple transition metal, has the concerted catalysis effect, has improved H
2O
2Catalytic efficiency is compared as catalyst with the oxide that uses one or both transition metal, because the synergy between the different transition metal, catalytic is obviously accelerated.
E. after pyrite cinder is handled through simple pre-activated, can obviously improve its catalytic perfomance, improve reaction efficiency, save catalyst consumption.
F. course of reaction is simple to operate, and treatment effect is good, is easy to through engineering approaches and applies.
Utilize pyrite cinder as catalyst, expanded the approach of its utilization of resources, reach the purpose of the treatment of wastes with processes of wastes against one another, realized comprehensive utilization of waste materials.
The specific embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1:
The Acid Red B simulated wastewater of getting 5 parts of 500mL places respectively the 1L beaker, and initial concentration is 200mg/L, and regulating the pH value with hydrochloric acid and NaOH successively is 3,5,7,9,11, adds respectively 30% H
2O
2Solution 15mL and pyrite cinder catalyst 15g, open six agitators, in setting-up time point sampling, the concentration of Acid Red B and pH value in the waste water behind the Check processing are as a result shown in the table 1, can find out that this method is very wide to the scope of application of pH, be that treatment effect is unaffected within 3～11 in the pH value, and after processing, the pH value of system is all at neutral range, for all not needing to regulate pH before and after the general waste water reaction.
The different initial pH of table 1 are to the impact of reaction effect
| Initial pH | 3 | 5 | 7 | 9 | 11 |
| PH behind the 4h | 6.74 | 7.36 | 7.42 | 7.45 | 7.9 |
| Concentration behind the 4h (mg/L) | 6.66 | 2.70 | 3.08 | 3.52 | 8.52 |
| 4h clearance (%) | 96.67 | 98.65 | 98.46 | 98.24 | 95.74 |
Embodiment 2:
Get the 500mL initial concentration and be the Acid Red B waste water of 200mg/L and put in the 1L beaker, add pyrite cinder 2.5g as catalyst, and then add 30% H
2O
2Solution 15mL, the initial pH of solution are neutrallty condition (being about 7.3), carry out stirring reaction, in the sampling of setting-up time point, detect the concentration of Acid Red B in the waste water and calculate its clearance, and the result is as shown in table 2:
The treatment effect of table 2 pair waste water from dyestuff
| Reaction time | 1h | 2h | 4h | 6h | 24h |
| Acid Red B concentration (mg/L) | 51.85 | 43.20 | 27.02 | 10.98 | 0 |
| Acid Red B clearance (%) | 74.08 | 78.40 | 86.49 | 94.51 | 100 |
Embodiment 3:
The phenolic waste water of getting 3 parts of 500ml joins respectively in 3 1L beakers, and the initial concentration of phenol is 60mg/L, adds successively pyrite cinder 5g, 10g behind the activating pretreatment, 15g as catalyst, adds respectively 30% H again
2O
2Solution 15mL carries out stirring reaction, in setting-up time point sampling, and the concentration of phenol in wastewater behind the Check processing.The result is as shown in table 3:
Table 3 pyrite cinder activation post processing wastewater containing phenol example
| Catalyst amount | 10g/L | 20g/L | 30g/L |
| Reaction 2h phenol concentration | 2.47 | 1.59 | 0.54 |
| Reaction 4h phenol concentration | Do not detect | Do not detect | Do not detect |
Embodiment 4
The black waste water from dyestuff of two property of getting two parts of 500ml joins in the 1L beaker and (is labeled as A, B difference), and the A sample adds through the slag 10g behind the activating pretreatment, and the B sample adds pyrite cinder former state 10g, adds respectively H then in A, B difference
2O
2, its concentration in waste water is 0.05mol/L, the percent of decolourization of sample analysis waste water behind the stirring reaction 4h, and the result is as shown in table 4.
Table 4 activating pretreatment slag improves the example of reactivity worth
| A (activating pretreatment slag) | B (pyrite cinder former state) | |
| The percent of decolourization of waste water (%) | 85.62 | 67.13 |
Embodiment 5:
Coking, petrochemical industry, the petroleum wastewater of respectively getting 500ml place respectively 3 1L beakers, and adding respectively and adding mass fraction behind the pyrite cinder catalyst 10g again is 30% H
2O
2Solution 15mL, H in the waste water
2O
2Concentration be about 0.3mol/L, open six agitators, sampling detects the indexs such as COD, BOD, pH, colourity of waste water behind the reaction 4h.Can find out that indegradable industrial effluent is through obviously improving the biodegradability of waste water after the catalytic oxidation treatment, the result is as shown in table 5.
Table 5 Industrial Wastewater Treatment example
| Kind of waste water | Coking chemical waste water | Petrochemical wastewater | Petroleum wastewater |
| Initial pH | 9.7 | 8.6 | 8.2 |
| Initial COD | 2360mg/L | 377mg/L | 408mg/L |
| COD after processing | 1452mg/L | 229mg/L | 791mg/L |
| Initial BOD 5/ COD | 0.30 | 0.24 | 0.042 |
| BOD after the reaction 5/ COD | 0.38 | 0.56 | 0.24 |
| Colourity changes | Pitchy → faint yellow | Fully decolouring | Fully decolouring |
Embodiment 6:
The recycling of slag experiment: the reactive light yellow wastewater of getting the 500mL initial concentration and be 200mg/L places the 1L beaker, adds and adds 30% H behind the pyrite cinder 10g again
2O
2Solution 10mL takes a sample the concentration of waste water reactive brilliant yellow after the analyzing and processing behind the low rate mixing reaction 6h.In order to test the recycling performance of slag, behind first set reaction 6h, pour out supernatant, slag is stayed in the beaker, again adds the waste water from dyestuff that concentration is 200mg/L again, again pour out supernatant behind the reaction 6h, slag is continued to employ, and carries out successively the experiment of reusing of slag, can find out that slag is as catalyst recycling 6 times after, still have preferably catalytic treatment effect, the result is as shown in table 6:
The repeated use experiment of table 6 pyrite cinder
| Slag recycling number of times | 1 | 2 | 3 | 4 | 5 | 6 |
| Reactive brilliant yellow clearance (%) | 98.53 | 97.69 | 96.88 | 97.12 | 96.42 | 92.23 |
Above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (7)
1. a method of processing the difficult degradation pollutant is characterized in that: utilize pyrite cinder as catalyst, with H
2O
2Consist of heterogeneous Fenton-like system, catalysis H
2O
2Produce the extremely strong hydroxyl radical free radical OH of oxidisability, to organic pollution carry out efficiently, fast degradation.
2. method according to claim 1, it is characterized in that: before the reaction, handle to improve its reactivity worth by pyrite cinder being carried out pre-activated, described " pre-activated processing " is: pyrite cinder is stirred immersion 1h at a slow speed in being added with the dilute hydrochloric acid solution of 0.01～1%NaCl after, take out also with clear water flushing, the use of oven dry back.
3. method according to claim 1 is characterized in that: comprising:
(1) waste water is added reactor after, slag in waste water behind a certain amount of pyrite cinder former state of adding or the process activating pretreatment, described " activating pretreatment " is: after pyrite cinder low rate mixing in being added with the dilute hydrochloric acid solution of 0.01～1%NaCl is soaked 1h, take out and with using after clear water flushing, the oven dry:
(2) in waste water and pyrite cinder mixed liquor, add H
2O
2Solution is so that itself and pyrite cinder form Fenton-like reagent;
(3) stir, make pyrite cinder and H
2O
2Solution mixes with waste water, reacts, and stops after the reaction time that arrival is set stirring;
(4) leave standstill, pyrite cinder precipitates rapidly, discharges supernatant.
4. method according to claim 3 is characterized in that: in the step (1):
The addition of pyrite cinder is 5g/L～30g/L.
5. method according to claim 3 is characterized in that: in the step (2): H
2O
2Addition be 0.05mol/L～0.3mol/L.
6. method according to claim 3 is characterized in that: in the step (4): the pyrite cinder recycling of precipitation.
7. method according to claim 3 is characterized in that: also comprise step (5): the water sample after handling is carried out water analysis, detect pollutants in waste water concentration, BOD, COD, pH, colourity, biodegradable property of wastewater can improve.
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