CN114804374B - Fenton dye degradation system and degradation method and application thereof - Google Patents
Fenton dye degradation system and degradation method and application thereof Download PDFInfo
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Abstract
The invention provides a Fenton dye degradation system and a degradation method and application thereof, belonging to the technical field of sewage treatment; in the present invention, by controlling the electrically active bacteriaShewanella oneidensis A novel biologically-driven Fenton degradation system is constructed under the oxygen environment condition of MR-1 (MR-1 for short) growth, and under the aerobic and anaerobic environment conditions, the MR-1 respectively converts O into oxygen 2 And Fe 3+ Reduction to H 2 O 2 And Fe 2+ The method not only realizes the high-efficiency degradation of the organic pollutants difficult to degrade, but also achieves the purpose of reducing the operation cost.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a Fenton dye degradation system, a degradation method and application thereof.
Background
Industrial wastewater is an important source for causing water environment pollution, wherein the printing and dyeing wastewater accounts for about 35 percent of the discharge amount of the whole industrial wastewater. The printing and dyeing wastewater has large discharge amount, complex components, strong environmental stability and difficult biodegradation, most of contained dye pollutants have the 'three-cause' effect, and the ecological environment and the health safety of human beings are seriously threatened. Therefore, efficient and low-consumption green treatment of dye wastewater is imperative. At present, the treatment method of dye wastewater mainly comprises three types, namely a physical method, a biological method and a chemical method. Wherein, the physical method has simple operation and management, but limited effect, high cost and easy generation of secondary pollution; the biological method has low cost and is environment-friendly, but has low efficiency and poor environmental adaptability; although the conventional chemical method has a good effect, the operation cost is high, the environmental friendliness is poor, and a high-efficiency pollution-free green chemical oxidation technology is favored, particularly, the Fenton oxidation method is concerned in the field of dye wastewater treatment because the Fenton oxidation method is environment-friendly, high in reaction speed and high in degradation efficiency, and can treat organic matters which are difficult to degrade.
Fe for Fenton oxidation 2+ Catalysis H 2 O 2 The decomposition produces hydroxyl radicals (. OH) which attack the organic contaminants by this highly reactive. OH, thereby mineralizing them into carbon dioxide, water and inorganic ions. Since OH has high oxidation-reduction potential and strong electronegativity, it can remove refractory organic pollutants in water without selective oxidation. Compared with other oxidation methods, the Fenton method can destroy organic matters in the dark, and has the advantages of high degradation efficiency, high reaction speed, capability of treating organic matters difficult to degrade and the like. However, the conventional Fenton method requires constant replenishment of Fenton's reagent (H) 2 O 2 And Fe 2+ ) And pH adjustment, and other disadvantages, such as high operation cost, generation of a large amount of iron sludge, easy secondary pollution, high requirement on corrosion resistance of equipment, high equipment investment cost, and the like. These disadvantages have largely restricted the practical application of the Fenton process to contaminant degradation. Therefore, if the Fenton reagent self-supply (the system is automatically generated without being added) can be realized, the running cost of the Fenton method is greatly reduced, and the application potential of the Fenton method in the field of organic pollutant degradation is enhanced.
In the prior art, fe is used 3+ To replace Fe 2+ Maintenance of Fe required in Fenton reaction by iron cycling 2+ A catalyst. However, this method overcomes the additional supplement of Fe 2+ But requires a continuous supply of H 2 O 2 And photo-assisted Fe 2+ Regeneration due to difficulty in obtaining light and H in underground aquifers 2 O 2 The supply of (2) has the problems of high operation cost, difficult in-situ remediation for groundwater pollution and the like. Therefore, the Fenton method driven by the development system is of great significance.
Disclosure of Invention
Aiming at some defects in the prior art, the invention provides a Fenton dye degradation system, a degradation method and application thereof. In the present invention, by controlling the electrically active bacteriaShewanella oneidensis A novel biologically-driven Fenton degradation system is constructed under the oxygen environment condition of MR-1 (MR-1 for short) growth, and the MR-1 respectively converts O into oxygen under the aerobic and anaerobic environment conditions 2 And Fe 3+ Reduction to H 2 O 2 And Fe 2+ The method not only realizes the high-efficiency degradation of the organic pollutants difficult to degrade, but also achieves the purpose of reducing the operation cost.
The invention firstly provides an electroactive microorganism driven Fenton dye degradation system, which comprises free electroactive bacteria and co-immobilized electroactive bacteria;
the co-immobilized electroactive bacteria comprise electroactive bacteria and Fe 3+ The co-immobilized pellet of (1), the co-immobilized pellet has a particle size of 4.5 to 5.5mm, wherein the inoculation amount of the electroactive bacteria in the co-immobilized pellet is 30 to 40% (v/v);
the free electroactive bacteria and the co-immobilized electroactive bacteria are MR-1.
Further, in the Fenton dye degradation system driven by the electroactive microorganisms, the number ratio of free electroactive bacteria to living bacteria contained in co-immobilized electroactive bacteria is 0.2 to 0.6:1.
further, the preparation method of the co-immobilized electroactive bacteria comprises the following steps:
adding Fe to a mineral salt solution containing sodium alginate 3+ Compound (I)Ultrasonically stirring the mixture to be uniform, adding MR-1 bacterial liquid, uniformly mixing the mixture to obtain a mixed solution, dropwise adding the mixed solution into 3.5% anhydrous calcium chloride solution, standing the mixture, taking out the pellets after forming the pellets, washing the pellets, and placing the pellets in mineral salt solution for later use.
Wherein the concentration of the sodium alginate in the mixed solution is 2-3g/L;
said Fe 3+ The compound being Fe 2 O 3 Any one of ferric hydroxide and ferric chloride, the final concentration of which is 0.4 to 0.6g/L;
the concentration of the MR-1 is 4 to 6 multiplied by 10 7 CFU/mL, and the inoculum size is 30 to 40% (v/v).
The invention also provides application of the Fenton dye degradation system driven by the electroactive microorganisms in degradation of dye pollutants. Wherein the dye contaminants comprise anthraquinone dyes, metal complex dyes, or azo dyes of different polarities.
The invention also provides a degradation method of dye pollutants, which comprises the following steps:
(1) Activating the electroactive bacteria MR-1, inoculating the activated electroactive bacteria MR-1 into a liquid LB culture medium, performing shake culture to the late logarithmic phase, centrifugally collecting thalli, and then re-suspending the thalli by using a mineral salt solution to obtain free electroactive bacteria MR-1 for later use;
(2) Mixing sodium alginate, free electroactive bacteria MR-1 and Fe 3+ The compounds are mixed and then dropped into an anhydrous calcium chloride solution to prepare the co-immobilized electroactive bacteria MR-1 for later use;
(3) Inoculating the free electroactive bacteria and the co-immobilized electroactive bacteria into a mineral salt solution containing the dye pollutants or wastewater containing the dye pollutants for reaction.
Further, in the step (1), the concentration of the free electroactive bacteria is 4 to 6 multiplied by 10 7 CFU/mL。
Further, in the step (3), the volume ratio of the total inoculation amount of the free electroactive bacteria and the co-immobilized electroactive bacteria to the mineral salt solution containing the dye pollutants or the wastewater containing the dye pollutants is 8 to 18; the ratio of the number of viable bacteria contained in the free electroactive bacteria to the number of viable bacteria contained in the co-immobilized electroactive bacteria is 0.2 to 0.6:1;
the reaction is carried out at 29.5 to 30.5 ℃ under a stirring condition of 195 to 205rpm.
Further, in the step (3), the dye contaminant includes anthraquinone dye, metal complex dye or azo dye with different polarity.
Compared with the prior art, the invention has the following beneficial effects:
in the invention, the O in the environment can be reduced by utilizing the release of electrons to the environment in the process of old metabolism of the electroactive bacteria 2 Or Fe 3+ The microbial technology is combined with the Fenton technology, and the MR-1 continuously releases O in the air by controlling the environmental condition of the growth of the MR-1 2 And Fe 3+ Respectively converted into H 2 O 2 And Fe 2+ Thereby obtaining the Fenton reagent, forming a Fenton reaction system, and continuously generating OH to degrade organic pollutants. Specifically, the invention provides anaerobic environment condition by utilizing immobilized microorganism technology, so that the electroactive bacteria MR-1 carries out anaerobic respiration, and solid Fe is obtained 3+ Reduction to Fe 2+ (ii) a Reduction of molecular oxygen in wastewater to H using suspended MR-1 2 O 2 And on the solid phase surface of the pellet, fe 2+ Catalysis H 2 O 2 Decomposing to generate high-activity hydroxyl free radicals, thereby efficiently degrading dye pollutants.
Compared with the Fenton technology in the prior art, the Fenton dye degradation system driven by the electroactive microorganisms has the following obvious advantages: (1) H 2 O 2 The MR-1 is used for reducing the molecular oxygen in the water without adding, so that the operation cost is greatly reduced; (2) The Fenton reaction is carried out under the condition of neutral pH, the requirement on the corrosion resistance of equipment is low, and the investment cost of the equipment is reduced; (3) Catalyst Fe 2+ From solid phase Fe 2 O 3 Anaerobic formation by MR-1 and formation of Fe in the reaction 2+ And Fe 3+ The iron sludge is not generated in the process of circulation; (4) The anaerobic environment condition required by MR-1 is provided by the immobilized pellet, and the closed environment required by the conventional microorganism anaerobic is not required, so the operation is simple and convenient, and the management is easy; (5) Immobilized MR-1 and suspended MR-1 in the same reactor, and synchronously carrying out anaerobic Fe production 3+ And aerobic production of H 2 O 2 The reagent has high utilization rate, simple flow and easy realization of engineering application. The invention relates to a biological Fenton system driven by electroactive microorganisms, wherein a Fenton reagent H is not added 2 O 2 Without supplementing Fenton reagent Fe 2+ Under the condition, the Fenton reagent is generated by electroactive microorganisms, so that the effective degradation of dye pollutants is successfully realized, the degradation rate of the degradation system to different types of dyes reaches 49.0-95.4% within a short degradation time (6-12 hours), the application value and the application prospect of a Fenton method are improved, and the application range of electroactive bacteria in environmental pollution remediation is widened.
Drawings
FIG. 1 is a diagram of MR-1 driven biological Fenton contaminant degradation mechanism.
FIG. 2 shows MR-1 and Fe 2 O 3 A manufacturing flow chart of the co-immobilized pellet.
FIG. 3 is a graph showing the degradation effect of the MR-1 driven bio-Fenton system on anthraquinone dye disperse blue 56.
FIG. 4 is a graph showing the degradation effect of a biological Fenton system driven by MR-1 on metal complex dye naphthol green B.
FIG. 5 is a graph showing the degradation effect of MR-1 driven bio-Fenton system on methyl orange, a strongly polar azo dye.
FIG. 6 is a graph showing the degradation effect of MR-1 driven biological Fenton system on m-aniline yellow, a low polarity azo dye.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, but the scope of the invention is not limited thereto. The strain MR-1 of the present invention is a model electrogenic microorganism, which is given by professor Nielsen, university of California, USA; the strain is deposited in American Type Collection Center (ATCC) and has strain number of ATCC700500 TM . The LB medium and mineral salt solutions presented in the examples are conventional in the art and are either commercially available or formulated on their own as described below.
Solid LB medium: contains yeast extract 5g/L, tryptone 10g/L, sodium chloride 10g/L, and agar 2%.
Liquid LB medium: contains yeast extract 5g/L, tryptone 10g/L, and sodium chloride 10g/L.
Mineral salt solution: the solution contained 7.5 mmol NaOH and 28 mmol NH per liter 4 Cl、1.3 mmol KCl、4.3 mmol NaH 2 PO 4 100 mmol NaCl, 1 mL vitamin mother liquor, 1 mL amino acid mother liquor and 1 mL microelement mother liquor. Wherein the vitamin mother liquor: each liter of the mother liquor contains 2.0mg of biotin, 2.0mg of folic acid, 10.0mg of pyridoxine hydrochloride, 5.0mg of riboflavin, 5.0mg of vitamin B, 5.0mg of nicotinic acid, 5.0mg of pantothenic acid, and 0.1mg of vitamin B 12 5.0mg p-aminobenzoic acid and 5.0mg lipoic acid;
amino acid mother liquor: each liter of mother liquor contains 2g of L-glutamic acid, 2g of L-arginine and 2g of DL-serine;
and (3) a microelement mother solution: the mother liquor contains 78.49 mu mol C per liter 6 H 9 NO 3 、121.71 μmol MgSO 4 ·7H 2 O、29.58 μmol MnSO 4 ·H 2 O、 171.12 μmol NaCl、3.60 μmol FeSO 4 ·7H 2 O、6.80 μmol CaCl 2 ·2H 2 O、4.20 μmol CoCl 2 ·6H 2 O、9.54 μmol ZnCl 2 、0.40 μmol CuSO 4 ·5H 2 O、0.21 μmol AlK(SO 4 ) 2 ·12H 2 O、1.62 μmol H 3 BO 3 、1.03 μmol Na 2 MoO 4 ·2H 2 O、1.01 μmol NiCl 2 ·6H 2 O and 0.76. Mu. Mol Na 2 WO 4 ·2H 2 O。
The degradation mechanism of the Fenton dye degradation system driven by the electroactive microorganisms is shown in figure 1, and specifically, anaerobic environment conditions are provided by utilizing the immobilized microorganism technology, so that electroactive bacteria MR-1 carry out anaerobic respiration, and solid Fe is obtained 3+ Reduction to Fe 2+ (ii) a Reduction of molecular oxygen in wastewater to H using suspended MR-1 2 O 2 . On the solid phase surface of the pellet, fe 2+ Catalysis H 2 O 2 Decompose to generate high-activity hydroxyl free radicals, thereby efficiently degrading the dyeA contaminant.
Example 1:
(1) MR-1 stored in glycerol was streaked onto solid plate LB medium and activated for culture at 30 ℃.
(2) And (3) sucking the activated single colony by using a pipette gun, inoculating the single colony into 50mL of liquid LB culture medium, performing shake culture at (30 +/-0.5) DEG C and (200 +/-5) rpm for 10h to the late logarithmic phase, centrifuging the late logarithmic phase bacterial liquid at 7000 rpm for 15 min, and collecting thalli. The bacterial precipitation is resuspended by mineral salt solution, and the concentration of the bacterial suspension is adjusted to 4 to 6 × 10 by spectrophotometry 7 CFU/mL, spare.
(3) The preparation process of the co-immobilized electroactive bacteria pellet is shown in figure 2, and comprises the following specific steps:
preparing a sodium alginate solution of 2g/L, and adding Fe into the sodium alginate solution 2 O 3 And (3) enabling the iron concentration to be 0.6g/L, uniformly stirring by ultrasonic, adding the prepared MR-1 bacterial liquid, and uniformly mixing. Dripping the mixed solution into 3.5% anhydrous calcium chloride solution for complexing to form small balls, standing for 2h, taking out, washing with pure water for 2 times, and adding into mineral salt solution for later use.
(4) Mixing the co-immobilized electroactive bacteria pellets (80 particles) with a free electroactive bacteria MR-1 solution (50 mL) to obtain the Fenton dye degradation system driven by the electroactive microorganisms.
Example 2:
in this example, the degradation effect of the electroactive microorganism-driven Fenton dye degradation system of the present invention on dye pollutants of different structural types was examined by using only co-immobilized electroactive bacteria as a control group a, only free electroactive bacteria MR-1 as a control group B, and the electroactive microorganism-driven Fenton dye degradation system obtained in example 1 as an experimental group. The examination steps are as follows:
0.005 g of dye pollutants (anthraquinone dye disperse blue 56, metal complex dye naphthol green B, strong polar azo dye methyl orange and low polar azo dye m-aniline yellow) with different structure types is weighed and respectively dissolved in 50mL of the Fenton dye degradation system driven by the electroactive microorganism in the embodiment 1, and then a ventilating sealing film is used for sealing to obtain the dye pollutant reaction system. The reaction system is put into a shaking table, shaking culture is carried out at the temperature of (30 +/-0.5) DEG C and the rpm of (200 +/-5), each group is provided with three parallels, timed sampling is carried out on an experimental group and a control group, and after centrifugation, the absorbance value of supernatant is measured. From the absorbance values, the degradation rate of the dye was calculated according to the following formula.
In the formula (I), the compound is shown in the specification,A 0 is the initial absorbance of the dye solution;A t the absorbance of the dye solution at the time t of decolorization.
The degradation effects of the Fenton degradation system driven by the electroactive microorganism MR-1 on different types of dye pollutants including anthraquinone dye disperse blue 56, metal composite dye naphthol green B, strong polar azo dye methyl orange and low polar azo dye m-aniline yellow are respectively shown in the figures 3, 4, 5 and 6.
As can be seen from FIG. 3, in the degradation time of 6h, the degradation rate of the MR-1 driven Fenton degradation system on disperse blue 56 can reach 66.3%, while the degradation rate of the control group A is only 32.4% and the degradation rate of the control group B is only 6.7%.
As can be seen from FIG. 4, in the degradation time of 12h, the degradation rate of the MR-1 driven Fenton degradation system on naphthol green B can reach 49.0%, while the degradation rate of the control group A is only 42.4%, and the degradation rate of the control group B is only 14.0%.
As can be seen from FIG. 5, the degradation rate of the MR-1 driven Fenton degradation system on methyl orange can reach 95.4% in the degradation time of 12h, while the control group A is only 87.3% and the control group B cannot degrade.
As can be seen from FIG. 6, the degradation rate of the MR-1 driven Fenton degradation system on m-aniline yellow can reach 91.9% within 10h of degradation time, while the control group A only has 87.4% and the control group B cannot degrade.
In summary, the results of FIGS. 3-6 show that the bioactive microorganism MR-1 driven biological Fenton system does not add Fenton reagent H 2 O 2 Without supplementing Fenton reagent Fe 2+ In the case of (1), fe is produced by an electroactive microorganismThe nton reagent successfully realizes the effective degradation of dye pollutants, and the degradation rate of the degradation system to different types of dyes reaches 49.0 to 95.4 percent within a short degradation time (6 to 12 hours). Wherein, the anthraquinone dye which is difficult to be biodegraded is degraded by 66.3 percent within 6 hours, and is particularly effective; for azo dyes, the degradation effect is best whether strong polarity or weak polarity, the degradation rate in 10 hours reaches more than 90%, and complete degradation can be realized quickly; the metal complex dye can release heavy metal ions in the degradation process, possibly inhibit the metabolism of microorganisms, but can also be effectively degraded.
Therefore, the Fenton degradation system driven by the electrically active microorganism MR-1 can effectively degrade anthraquinone dye, metal composite dye wastewater or azo dye wastewater with different polarities. Therefore, the system is a high-efficiency and low-consumption dye degradation system, and the high efficiency is reflected in that the dye degradation rate is high, the degradation speed is high, and the system is suitable for different types of dyes; the low consumption is realized by not adding Fenton reagent, the operation cost is low, and meanwhile, the equipment investment cost is low because the system operates in a neutral environment, so that the cost for restoring environmental pollution by a Fenton method can be greatly reduced, secondary pollutants such as iron mud and the like are not generated, and the application prospect is good.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (6)
1. A Fenton dye degradation system is characterized by comprising free electroactive bacteria and co-immobilized electroactive bacteria;
the co-immobilized electroactive bacteria comprise electroactive bacteria and Fe 3+ The co-immobilized bead of (1), wherein the particle size of the co-immobilized bead is 4.5 to 5.5mm;
the free electroactive bacteria and the co-immobilized electroactive bacteria are all electroactive bacteriaShewanella oneidensis MR-1；
In the Fenton dye degradation system driven by the electroactive microorganisms, the number ratio of viable bacteria contained in free electroactive bacteria to co-immobilized electroactive bacteria is 0.2 to 0.6:1;
the preparation method of the co-immobilized electroactive bacteria comprises the following steps:
adding Fe to mineral salt solution containing sodium alginate 3+ The compound is ultrasonically stirred until uniform and then addedShewanella oneidensis Uniformly mixing the MR-1 bacterial liquid to obtain a mixed solution, dropwise adding the mixed solution into a 3.5% anhydrous calcium chloride solution, standing, taking out the pellets after forming into pellets, washing, and placing in a mineral salt solution for later use;
the above-mentionedShewanella oneidensis The concentration of the MR-1 bacterial liquid is 4 to 6 multiplied by 10 7 CFU/mL, saidShewanella oneidensis The bacterial load of MR-1 was 30 to 40% (v/v).
2. The Fenton dye degradation system according to claim 1, wherein the concentration of sodium alginate in the mixed solution is 2-3 g/L;
said Fe 3+ The compound being Fe 2 O 3 And (3) any one of ferric hydroxide and ferric chloride, wherein the final concentration of the ferric hydroxide and the ferric chloride in the mixed solution is 0.4-0.6 g/L.
3. Use of the Fenton dye degradation system of claim 1 to degrade dye contaminants.
4. Use according to claim 3, wherein the dye contaminants comprise anthraquinone dyes, metal complex dyes or azo dyes of different polarity.
5. A method for degrading dye contaminants, the method comprising:
(1) Electrically active bacteriaShewanella oneidensis Inoculating the activated MR-1 into a liquid LB culture medium to shake culture to the late logarithmic phase, centrifugally collecting thalli, and then re-suspending with a mineral salt solution to obtain free electroactive bacteriaShewanella oneidensis MR-1, spare; the concentration of the free electroactive bacteria is 4 to 6 multiplied by 10 7 CFU/mL；
(2) Mixing sodium alginate and free electroactive bacteriaShewanella oneidensis MR-1 and Fe 3+ The compounds are mixed and dropped into an anhydrous calcium chloride solution to prepare the co-immobilized electroactive bacteriaShewanella oneidensis MR-1, spare;
(3) Inoculating free electroactive bacteria and co-immobilized electroactive bacteria into wastewater containing dye pollutants for reaction; the volume ratio of the total inoculum size of the free electroactive bacteria and the co-immobilized electroactive bacteria to the wastewater containing the dye pollutants is 8 to 18; the ratio of the number of viable bacteria contained in the free electroactive bacteria to the number of viable bacteria contained in the co-immobilized electroactive bacteria is 0.2 to 0.6:1;
the reaction is carried out at 29.5 to 30.5 ℃ under stirring conditions of 195 to 205rpm.
6. The method of degrading dye contaminants of claim 5, wherein in step (3), the dye contaminants comprise anthraquinone dyes, metal complex dyes, or azo dyes of different polarity.
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