CN109626591B - Method for synergistically reducing hexavalent chromium by utilizing microorganisms and hematite under illumination condition - Google Patents
Method for synergistically reducing hexavalent chromium by utilizing microorganisms and hematite under illumination condition Download PDFInfo
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Abstract
The invention discloses a method for synergistically reducing hexavalent chromium by utilizing microorganisms and hematite under the illumination condition, which is characterized in that the hexavalent chromium is synergistically reduced by adding the hematite and iron reducing bacteria capable of carrying out extracellular electron transfer into wastewater containing the hexavalent chromium under the illumination condition. The method utilizes hematite minerals and extracellular breathing iron reducing bacteria which widely exist in the natural environment to realize the high-efficiency treatment of chromium pollution by synergistically utilizing light energy and chemical energy, solves the problems of low treatment efficiency, complex synthesis of photocatalytic materials, poor environmental compatibility, intolerance of microorganisms, high treatment cost and the like of the existing method, and simultaneously avoids the problem of secondary pollution in the treatment process.
Description
Technical Field
The invention relates to a treatment technology of hexavalent chromium in wastewater, in particular to a method for reducing hexavalent chromium by utilizing environmental microorganisms and hematite minerals in a synergetic photocatalytic manner, and belongs to the field of environmental engineering water treatment.
Background
Chromium and its compounds have wide industrial application, but are easy to produce harmful chromium-containing waste slag and waste water in the course of production and use. With the economic development, the use amount of chromium salt in industrial production is more and more, and the chromium pollution is more and more serious. The toxicity of chromium is related to the valence state of chromium, and hexavalent chromium is 100 times more toxic than trivalent chromium and is easily absorbed by the human body and accumulated in the body. Hexavalent chromium is a persistent hazard to the environment and can invade the body through the digestive, respiratory, skin and mucous membranes. It has been reported that there are different degrees of hoarseness and atrophy of nasal mucosa when the respiratory air contains chromic anhydride with different concentrations, and perforation of nasal septum and bronchiectasis when the respiratory air is serious; vomiting and abdominal pain may occur when entering through the digestive tract; dermatitis and eczema can be produced when the skin is invaded; there is a carcinogenic risk of long or short term exposure or inhalation. Trivalent chromium in the water is mainly adsorbed on solid matters and exists in sediments, and hexavalent chromium is mostly dissolved in water and is stable. How to convert hexavalent chromium in wastewater into trivalent chromium which is easy to precipitate and less harmful is the key point of chromium pollution treatment of wastewater at present.
Xu et al TiO coated with alginic acid2As a photocatalytic material, ferric ions are added, and the good effect on reducing hexavalent chromium is found. But TiO 22Has a very narrow absorption band and is expensive to synthesize, and does not have the ability to continuously reduce and maintain the original form due to consumption of alginic acid (Xu S C, Pan S, Xu Y, et al. effective removal of Cr (VI) from water under bright by Fe (II) -doped TiO2sphericalshell.[J].Journal of Hazardous Materials,2015,283(283):7-13.)。
Middleton et al used Shewanella oneidensis MR-1 to reduce hexavalent chromium, and found that at low concentrations of chromium, chromic acid can be added continuously for multiple reductions, but at high concentrations there is some metabolic inhibition on the microorganism and the rate of biological reduction of hexavalent chromium is slower (Middleton S S, L atmani R B, Mackey M R, et al, Commetalism of Cr (VI) by Shewanella oneidensis MR-1 process l-assisted reduced chromium and inhibition growth [ J ]. Biotechnology & Bioengineering,2003,83(6): 627-37.).
Ye and the like can excite the organic complex of Fe (III) by ultraviolet under the acidic condition to degrade the organic complex and reduce Fe (III); the resulting Fe (II) converts Cr (VI) to Cr (III). However, this method requires a large amount of energy consumption, not only ultraviolet conditions, but also a large amount of organic complexes as electron donors (Ye Y, Jiang Z, Xu Z, equivalent. effective removal of Cr (III) -organic complexes from Water using UV/Fe (III) system: New gligible Cr (VI) accumulation and mechanism [ J ]. Water Research,2017,126: 172.).
The microorganism-assisted photocatalytic reduction reaction is a process in which after a semiconductor material is excited by illumination, some microorganisms capable of transferring extracellular electrons or extracellular secretions released by the microorganisms are used as hole capture agents of the semiconductor material, and reduction of other substances is carried out by utilizing the reducibility of photo-generated electrons, so that biomass energy and light energy are converted into chemical energy.
Disclosure of Invention
The invention aims to provide a method for efficiently reducing hexavalent chromium by coupling the extracellular respiration electricity generation function of microorganisms and the photocatalysis of natural minerals, which is used for solving the problems of low treatment efficiency, complex synthesis of photocatalytic materials, poor environmental compatibility, intolerance of microorganisms, high treatment cost and the like in the conventional method.
Semiconductor minerals generate oxidative photogenerated holes and reductive photogenerated electrons after being excited by light with a certain wavelength, and the oxidative photogenerated holes and the reductive photogenerated electrons are often paired and greatly recombined. The microorganisms such as Shewanella and Geobacillus can fill the holes generated by photoexcitation of semiconductor minerals with extracellular electrons, and some hole trapping agents can react with the holes, so that the photoproduction electrons can reduce hexavalent chromium into trivalent chromium. The trivalent chromium forms hydroxide precipitate at pH above 8, thereby achieving separation of chromium from the liquid phase.
The method for reducing hexavalent chromium provided by the invention is characterized in that hematite and iron reducing bacteria capable of carrying out extracellular electron transfer are added into the wastewater containing hexavalent chromium, and the hematite and the iron reducing bacteria synergistically reduce the hexavalent chromium under the illumination condition.
The hematite used in the method for reducing hexavalent chromium can be natural hematite or synthetic hematite. Preferably, the hematite has a particle size of the order of nanometers or microns, i.e., a hematite having an average particle size of 1nm to 10 μm.
The desired synthesis can be carried out by the following methodHematite of (a): (1) weighing Fe (NO)3)3·9H2Dissolving O solid in water to obtain Fe (NO) with concentration of 0.8-1.2M3)3·9H2O solution; (2) heating a volume of water to boiling, and adding Fe (NO) under stirring3)3·9H2Dropwise adding the O solution into continuously boiling water, and then standing and cooling to room temperature; (3) and (3) filling the suspension obtained in the step (2) into a dialysis bag, putting into ultrapure water for dialysis, periodically changing water until the conductivity of the dialysis water is similar to that of pure water, bottling, sealing and storing in dark place.
The above iron-reducing bacteria capable of extracellular electron transfer include Shewanella, Pseudomonas aeruginosa, Alcaligenes faecalis, Geobacillus, etc., preferably Shewanella inelloides MR-1(Shewanella oniedensisi MR-1) (accession number ATCC 700550).
The strain can be preserved by various preservation methods, such as freeze-drying preservation method, deep low-temperature preservation method, liquid nitrogen preservation method, mineral oil sealing preservation method, solid yeast preservation method, sand and soil tube preservation method, agar puncture preservation method, and the like. Before use, the preserved bacteria are activated in culture solution, the activated or transfer-cultured bacteria liquid is subcultured, when the bacteria liquid is cultured to a stationary phase, the iron reducing bacteria and the culture solution are separated by methods such as centrifugation, the culture solution is discarded, and the bacteria liquid is resuspended by isotonic solution. If the influence of extracellular secretion of the iron reducing bacteria on reduction of hexavalent chromium is avoided, the washing effect can be achieved by centrifuging for many times, discarding supernatant and resuspending.
In the method for reducing hexavalent chromium, the adding amount of the iron reducing bacteria is used for controlling the final bacterial amount OD600Preferably 0.1-1.0, preferably 0.2-1.0, and the concentration of hematite is controlled to 15 mg/L-300 mg/L.
In the method for reducing hexavalent chromium of the present invention, it is preferable to adjust the pH of the hexavalent chromium-containing wastewater to 6.5 to 7.5 before adding hematite and iron-reducing bacteria. If the pH value of the wastewater is lower than 6, trivalent chromium generated by reduction of the iron reducing bacteria has toxicity to microorganisms, so under an acidic condition, a complexing agent of the trivalent chromium, such as EDTA (ethylene diamine tetraacetic acid), TEOA (triethanolamine) and the like, can be added while hematite and the iron reducing bacteria are added, and the toxicity to the microorganisms is reduced by complexing the trivalent chromium. The amount of complexing agent added depends on the amount of trivalent chromium produced.
If the hexavalent chromium-containing wastewater lacks nutrients for the growth of iron-reducing bacteria, lactate may be added at a concentration of 10mM to 45 mM.
In the method for reducing hexavalent chromium, the illumination condition can be that the illumination intensity is 10mW/cm when the method is placed under a xenon lamp simulating sunlight or other artificial light source with visible light wave band2-100mW/cm2Or under natural sunlight, maintaining the temperature within the range of 25-35 ℃, and continuously reducing the hexavalent chromium.
By the method for synergistically reducing hexavalent chromium under the illumination condition of hematite and iron reducing bacteria, the tolerance of microorganisms to hexavalent chromium is improved, the reduction capability of microorganisms to hexavalent chromium is accelerated, and the cost of artificially synthesized semiconductors for catalytic reduction is saved.
Drawings
Figure 1 is an identification of the XRD pattern (upper) of the hematite sample synthesized in example 1 in comparison to the standard hematite pattern (lower).
FIG. 2 is a graph showing the synergistic reduction of hexavalent chromium between iron-reducing bacteria and minerals in a neutral environment, under light or dark conditions in example 1.
FIG. 3 is a graph of the photocatalytic reduction of hexavalent chromium by iron-reducing bacteria in example 2 in wastewater at pH 5.5, in light or darkness, with or without hematite.
FIG. 4 is a graph showing the reduction of hexavalent chromium by iron-reducing bacteria in dark conditions in example 3, with or without addition of EDTA complexing agent to the wastewater having a pH of 5.5.
FIG. 5 is a graph showing the reduction of hexavalent chromium in example 3 under the conditions of light or dark with or without iron-reducing bacteria, in which EDTA is added to the wastewater having a pH of 5.5.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments, but the present invention is not limited thereto.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1:
32.32g Fe (NO) were weighed out3)3·9H2O solid, dissolved in 80M L water to make 1M Fe (NO)3)3·9H2O solution, 1L ultrapure water was put in a conical flask, magnetons were added, and the flask was heated to boiling on a magnetic heating stirrer, and Fe (NO) was added dropwise at 0.5m L/min with a peristaltic pump while stirring the solution3)3·9H2The O solution was added to continuously boiling water. Stopping heating after the solution is added, and standing to naturally cool to room temperature.
Soaking dialysis bag (3.5-5KD, Spectrapor) with ultrapure water for 1h before use, cutting into multiple sections (about 30 cm), placing cooled suspension into dialysis bag, fastening two ends, dialyzing in ultrapure water, changing water every 12h until the conductivity of dialysis water is similar to that of pure water, taking out synthetic solution, bottling, sealing, and storing in 4 deg.C refrigerator in dark place.
Fig. 1 is an XRD pattern of hematite synthesized by the hydrothermal method, and compared with a standard XRD pattern of hematite, it can be considered that the material synthesized by the hydrothermal method is actually hematite.
The bacterial liquid of the normal transfer of the Shewanella onaedensisi (Shewanella niedrensisi MR-1, preservation number ATCC 700550) is mixed with 50% of glycerol according to the volume ratio of 1:1 in a container and is preserved at-80 ℃, the preserved bacterial liquid is added into L B culture medium according to the volume ratio of 1:20 in use, the transfer is carried out in the same ratio after activation.
Adding the synthesized hematite, re-suspended bacteria solution and lactate into chromium-containing (5 mg/L) neutral wastewater (pH equal to 7) to make OD of the mixed solution after addition600The value was 0.2, lactate concentration was 30mM, and hematite concentration was 150 mg/L, and the mixture was placed under a simulated sunlight xenon lamp with an irradiation intensity of 45mW/cm2Or irradiating under natural sunlight, and maintaining the temperature within 25-35 deg.C. The illumination time is 6hThe treatment efficiency of 50% is achieved, and as shown in fig. 2, it can be seen that the reduction of Cr and Cr in the system under neutral condition by light has a significant promoting effect in terms of both reaction speed and reaction degree.
Example 2:
the hematite synthesis method and the bacteria culture method in example 1 were used, and the synthesized hematite, the bacteria solution, and the lactate were added to chromium-containing (10 mg/L) acidic wastewater (pH 5.5) so that OD of the mixture was adjusted600The value is about 0.2, the lactate concentration is 30mM, and the hematite concentration is 150 mg/L. then the mixed solution is irradiated under the illumination condition (the illumination condition is the same as that of example 1), the hexavalent chromium reduction efficiency of more than 85% can be achieved within 25h, as shown in a dynamic curve of 'the presence of hematite by illumination bacteria' in figure 3, it can be seen from figure 3 that the hexavalent chromium is reduced by iron reducing bacteria in the dark, whether the hexavalent chromium is hematite or not is achieved, the chromium reduction dynamic curve is basically the same, but under the condition that the hematite is illuminated, the reduction effect is obviously improved, and the treatment efficiency of more than 80% can be achieved within 20 h.
Example 3:
the hematite synthesis method and the bacteria culture method in example 1 were adopted, since trivalent chromium reduced from the acidic wastewater is in an ionic state and has a certain toxicity to microorganisms, EDTA was used as a trivalent chromium complexing agent, synthesized hematite, a bacterial solution, a lactate and EDTA were added to acidic wastewater (pH 5.5) containing chromium (10 mg/L), and OD of the added mixed solution was made to be equal to OD of the acidic wastewater600The value is about 0.2, the lactate concentration is 30mM, the hematite concentration is 150 mg/L concentration is 0.66 mM., then the mixed solution is irradiated under the illumination condition (the irradiation condition is the same as that of example 1), the hexavalent chromium reduction efficiency of 80% can be achieved within 5h, as shown in a dynamic curve of 'the existence of bacteria and hematite under illumination' in figure 5, comparing figure 4 and figure 5, it can be seen that, compared with the condition without EDTA, the photoreduction effect of the iron reducing bacteria and the hematite is obviously improved by adding EDTA, the EDTA complexing agent is complexed with trivalent chromium, so the toxicity to microorganisms is reduced, and experiments prove that EDTA has the promotion effect on the reduction of hexavalent chromium by the iron reducing bacteria under the acid condition, in addition, the addition of EDTA promotes the high-efficiency reduction of hexavalent chromium by the iron reducing bacteria under the acid condition, namely 3h is achievedThe treatment efficiency is more than 80%.
Finally, it should be noted that the above examples are only for further understanding of the present invention and are not to be construed as limiting the same. But those skilled in the art will understand that: various substitutions and modifications are possible without departing from the spirit and scope of the invention and the appended claims. Therefore, the invention should not be limited to the embodiments disclosed, but the scope of the invention is defined by the appended claims.
Claims (11)
1. A method for reducing hexavalent chromium comprises adding hematite and iron reducing bacteria capable of performing extracellular electron transfer into wastewater containing hexavalent chromium, and synergistically reducing hexavalent chromium under illumination condition.
2. The method of claim 1, wherein the hematite is natural hematite or synthetic hematite having a particle size of the order of nanometers or microns.
3. The method of claim 2, wherein the hematite has an average particle size of from 1nm to 10 μ ι η.
4. The method of claim 1, wherein the hematite is prepared by:
1) weighing Fe (NO)3)3·9H2Dissolving O solid in water to prepare Fe (NO) with the concentration of 0.8-1.2M3)3·9H2O solution;
2) heating a volume of water to boiling, and adding Fe (NO) under stirring3)3·9H2Dropwise adding the O solution into continuously boiling water, and then standing and cooling to room temperature;
3) filling the turbid liquid obtained in the step 2) into a dialysis bag, putting the dialyzed turbid liquid into ultrapure water for dialysis, periodically changing water until the conductivity of the dialyzed water is similar to that of the pure water, and then bottling, sealing and storing in dark place.
5. The method of claim 1, wherein the iron-reducing bacteria capable of extracellular electron transfer are shewanella, pseudomonas aeruginosa, alcaligenes faecalis, and/or geobacillus.
6. The method of claim 5, wherein the Shewanella is Shewanella inekensis MR-1(Shewanella niedensis MR-1).
7. The method of claim 1, wherein the iron-reducing bacteria are added in an amount to control the final bacteria amount OD6000.1-1.0, and the hematite concentration is 15-300 mg/L.
8. The method of claim 1 wherein the pH of the hexavalent chromium-containing wastewater is adjusted to a pH of 6.5 to 7.5 prior to the addition of the hematite and the iron reducing bacteria.
9. The method of claim 1 wherein when the hexavalent chromium-containing wastewater is acidic, the complexing agent for trivalent chromium is added simultaneously with the hematite and the iron-reducing bacteria.
10. The method of claim 1 wherein a quantity of lactate salt is added for the growth of iron-reducing bacteria when the hexavalent chromium-containing wastewater is depleted of nutrients for the growth of iron-reducing bacteria.
11. The method according to claim 1, wherein the illumination condition is that the illumination intensity is 10-100 mW/cm when the artificial light source simulating sunlight is placed under the illumination condition2Or in natural sunlight, maintaining the temperature in the range of 25-35 ℃.
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| CN110699296B (en) * | 2019-11-12 | 2021-06-25 | 黑龙江八一农垦大学 | Iron reduction complex microbial inoculant and application thereof |
| CN111659729A (en) * | 2020-05-27 | 2020-09-15 | 北京化工大学 | Method for restoring chromium-polluted soil by Shewanella |
| CN115340194B (en) * | 2022-08-09 | 2023-12-26 | 华中科技大学 | Method for cooperatively removing hexavalent chromium by sludge iron-rich biochar and pseudomonas aeruginosa |
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