CN117185479B - Bacteria-carrying slow-release carbon source and preparation method and application thereof - Google Patents
Bacteria-carrying slow-release carbon source and preparation method and application thereof Download PDFInfo
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- CN117185479B CN117185479B CN202311306406.8A CN202311306406A CN117185479B CN 117185479 B CN117185479 B CN 117185479B CN 202311306406 A CN202311306406 A CN 202311306406A CN 117185479 B CN117185479 B CN 117185479B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical group [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 62
- 239000000945 filler Substances 0.000 claims abstract description 45
- 239000002351 wastewater Substances 0.000 claims abstract description 44
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 36
- 230000000813 microbial effect Effects 0.000 claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 claims abstract description 29
- 241001057811 Paracoccus <mealybug> Species 0.000 claims abstract description 16
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 12
- 241000316848 Rhodococcus <scale insect> Species 0.000 claims abstract description 8
- -1 succinate compound Chemical class 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 16
- 230000000593 degrading effect Effects 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 235000013399 edible fruits Nutrition 0.000 claims description 14
- 238000007710 freezing Methods 0.000 claims description 13
- 230000008014 freezing Effects 0.000 claims description 13
- 239000003431 cross linking reagent Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 241000894006 Bacteria Species 0.000 claims description 11
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 241000158504 Rhodococcus hoagii Species 0.000 claims description 8
- 238000004132 cross linking Methods 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 claims description 8
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 235000010413 sodium alginate Nutrition 0.000 claims description 5
- 239000000661 sodium alginate Substances 0.000 claims description 5
- 229940005550 sodium alginate Drugs 0.000 claims description 5
- SFAYBQDGCKZKMH-UHFFFAOYSA-N BNCC Chemical group BNCC SFAYBQDGCKZKMH-UHFFFAOYSA-N 0.000 claims description 4
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 3
- 244000105624 Arachis hypogaea Species 0.000 claims description 3
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 3
- 235000018262 Arachis monticola Nutrition 0.000 claims description 3
- 240000007049 Juglans regia Species 0.000 claims description 3
- 235000009496 Juglans regia Nutrition 0.000 claims description 3
- 235000020232 peanut Nutrition 0.000 claims description 3
- 235000020234 walnut Nutrition 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 2
- 238000006731 degradation reaction Methods 0.000 abstract description 15
- 230000015556 catabolic process Effects 0.000 abstract description 14
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052744 lithium Inorganic materials 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 5
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 15
- 239000001963 growth medium Substances 0.000 description 13
- 230000001580 bacterial effect Effects 0.000 description 11
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 238000000855 fermentation Methods 0.000 description 7
- 230000004151 fermentation Effects 0.000 description 7
- 239000002609 medium Substances 0.000 description 7
- 235000015097 nutrients Nutrition 0.000 description 7
- 238000011218 seed culture Methods 0.000 description 7
- 238000009631 Broth culture Methods 0.000 description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000010257 thawing Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 241000520272 Pantoea Species 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 244000005700 microbiome Species 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 240000008042 Zea mays Species 0.000 description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
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- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
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- 238000005119 centrifugation Methods 0.000 description 2
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- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 239000007836 KH2PO4 Substances 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
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- 238000007865 diluting Methods 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- 229910000396 dipotassium phosphate Inorganic materials 0.000 description 1
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- 238000000227 grinding Methods 0.000 description 1
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- 229920005610 lignin Polymers 0.000 description 1
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- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
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Abstract
The invention relates to the field of wastewater treatment materials, and particularly discloses a bacteria-carrying slow-release carbon source, a preparation method and application thereof. The bacteria-carrying slow-release carbon source provided by the invention comprises slow-release carbon source filler and microbial liquid loaded on the surface of the slow-release carbon source filler, wherein the slow-release carbon source filler is a tetramethyl ammonium hydroxide modified shell/polyethylene glycol succinate compound; the microbial liquid is mixed liquid of paracoccus and rhodococcus. The invention utilizes the combination of the slow-release carbon source filler and the microbial liquid, and effectively solves the technical problems of high treatment cost and low degradation efficiency caused by a large amount of carbon source consumption in the biochemical treatment of the waste water of the lithium battery production containing N-methyl pyrrolidone in the prior art. The bacteria-carrying slow-release carbon source has remarkable effect of treating the waste water of the lithium battery production containing the N-methylpyrrolidone, is low in cost and simple and convenient to operate, and greatly relieves the treatment pressure of the waste water of the lithium battery production.
Description
Technical Field
The invention relates to the field of wastewater treatment materials, and particularly discloses a bacteria-carrying slow-release carbon source, a preparation method and application thereof.
Background
N-methylpyrrolidone (NMP) is one of the most important production raw materials for lithium batteries, mainly for dissolving binders and diluting slurries. As new energy industries are rising, the capacity of power batteries is continuously increased, and the production wastewater containing N-methyl pyrrolidone is increasingly produced. Because the N-methyl pyrrolidone has stable structure, is not easy to hydrolyze and has high degradation difficulty, the treatment of the production wastewater containing the N-methyl pyrrolidone has become one of important research directions in the field of current environmental treatment.
In the prior art, the treatment method for the waste water of the lithium battery production containing N-methyl pyrrolidone comprises a high-grade oxidation method, a membrane treatment method, a biochemical treatment method and the like. However, the advanced oxidation method and the membrane treatment method have high treatment cost, unsatisfactory treatment effect and serious secondary pollution, and the biochemical treatment method has the advantages of lower cost, better treatment effect, small secondary pollution and the like, so that the biochemical treatment method becomes the most widely used method for treating the production wastewater containing the N-methylpyrrolidone.
Although the biochemical treatment method can degrade the waste water of the lithium battery production containing the N-methyl pyrrolidone, the total nitrogen and ammonia nitrogen content is high and the waste water has certain toxicity due to the serious unbalance of the nutrition ratio in the waste water, a large amount of carbon sources can be consumed in the process of degrading the waste water, and when the carbon content is insufficient, the degradation efficiency can be greatly reduced, so that the treatment cost is increased and the treatment effect of the waste water of the lithium battery production containing the N-methyl pyrrolidone is poor. Therefore, developing a degradation material which can effectively supplement carbon sources and has low cost plays an important role in relieving the pressure of the treatment of the waste water of the lithium battery production containing N-methyl pyrrolidone.
Disclosure of Invention
Aiming at the technical problems of high treatment cost and low degradation efficiency caused by a large amount of carbon source consumed in the biochemical treatment of the waste water of the lithium battery production containing N-methyl pyrrolidone in the prior art. The invention provides a bacteria-carrying slow-release carbon source and a preparation method and application thereof. According to the invention, the slow-release carbon source loaded with the microbial inoculum capable of degrading the N-methylpyrrolidone is utilized to carry out denitrification treatment on the wastewater, so that not only is the N-methylpyrrolidone difficult to treat degraded, but also nitrate nitrogen in the wastewater is effectively degraded, the cost of the slow-release carbon source loaded with the bacteria is low, and a new thought is provided for treating the production wastewater containing the N-methylpyrrolidone.
In order to achieve the above purpose, the present invention provides the following technical solutions:
The invention provides a bacteria-carrying slow-release carbon source, which comprises slow-release carbon source filler and microbial liquid loaded on the surface of the slow-release carbon source filler, wherein the slow-release carbon source filler is a tetramethyl ammonium hydroxide modified shell/polyethylene glycol succinate compound; the microbial liquid is a mixed microbial agent of paracoccus and rhodococcus.
Compared with the prior art, the invention provides a bacteria-carrying slow-release carbon source, which comprises two parts, slow-release carbon source filler and microbial bacteria liquid loaded on the surface of the slow-release carbon source filler. The microbial liquid takes slow-release carbon source filler as an external electron donor and a carbon source supplementing material, takes N-methyl pyrrolidone in wastewater as a part of electron donor, and takes nitrate nitrogen in wastewater as an electron acceptor for metabolism and growth. Meanwhile, the paracoccus and rhodococcus have high-efficiency N-methylpyrrolidone degradation capability and denitrification capability, and can convert toxic nitrate nitrogen in wastewater into nontoxic nitrogen while degrading N-methylpyrrolidone, so that the aim of efficiently degrading the wastewater containing N-methylpyrrolidone is fulfilled.
The invention takes tetramethyl ammonium hydroxide modified fruit shell/polyethylene glycol succinate compound as a slow-release carbon source filler, and the polyethylene glycol succinate can gradually release some dissolved organic matters with higher biodegradability under the action of microorganisms, so as to achieve the effect of slow-release carbon. But the single high molecular polymer has higher cost and is unfavorable for large-scale treatment of wastewater. Therefore, the inventor utilizes the tetramethyl ammonium hydroxide modified fruit shell as a natural carbon source to be compounded with the natural carbon source, and the tetramethyl ammonium hydroxide modified fruit shell can release part of organic matters to provide electrons and energy for denitrification reaction, so that the denitrification degradation process is accelerated. And the compact structure formed by closely connecting cellulose-hemicellulose-lignin in the modified shell is degraded, so that the specific surface area is increased, and the larger specific surface area is favorable for attaching more microorganisms in the denitrification process, thereby improving the denitrification efficiency. The combination of the two greatly reduces the treatment cost and further improves the efficiency of degrading the production wastewater containing the N-methyl pyrrolidone by microorganisms.
Preferably, the preparation method of the slow-release carbon source filler comprises the following steps:
s1, crushing and sieving shells, adding the crushed shells into deionized water, soaking, and filtering to obtain pretreated shell powder;
S2, uniformly mixing the pretreated shell powder with a tetramethyl ammonium hydroxide solution, reacting for 6-8 hours at 80-95 ℃, centrifuging, washing and drying to obtain tetramethyl ammonium hydroxide modified shells;
S3, dissolving the embedding material in water to obtain embedding material solution; adding the tetramethyl ammonium hydroxide modified fruit shell and polyethylene glycol succinate into the embedding material solution, reacting for 2-4 hours at 95-110 ℃, transferring into a mould, and freezing to obtain a frozen mixed material;
s4, uniformly mixing the frozen mixed material with a cross-linking agent, performing cross-linking reaction at 0-5 ℃, washing and drying to obtain the slow-release carbon source filler.
The invention utilizes tetramethyl ammonium hydroxide to modify the fruit shell, improves the specific surface area of the fruit shell, enables the fruit shell to load more microorganisms in the denitrification process, and promotes the denitrification treatment efficiency of wastewater. And the tetramethyl ammonium hydroxide modified shell is combined with polyethylene glycol succinate, so that the biodegradability of the slow-release carbon source filler is improved, the slow-release carbon source filler is easy to degrade, and the problem of secondary pollution is avoided.
Further preferably, in S1, the shell is any one or more of peanut shell, walnut shell or hawaii shell.
Further preferably, in S1, the mesh number of the sieve is 40 mesh to 60 mesh.
Further preferably, in S2, the concentration of the tetramethylammonium hydroxide solution is 0.1mol/L to 0.3mol/L.
Further preferably, in S2, the mass-volume ratio of the pretreated shell to the tetramethylammonium hydroxide solution is 1g (4-6) mL.
Further preferably, in S2, the rotational speed of the centrifugation is 1000rpm to 2000rpm, and the centrifugation time is 3min to 8min.
Further preferably, in S2, the drying temperature is 90 to 100 ℃ and the drying time is 6 to 8 hours.
Further preferably, in S3, the embedding material is sodium alginate, and the mass concentration of the embedding material solution is 8g/mL to 10g/mL.
Further preferably, in S3, the specific operation of dissolving the embedding material in water is to stir the embedding material at 85-90 ℃ for 4-5 h.
Further preferably, in S3, the mass ratio of the tetramethylammonium hydroxide modified fruit shell to the polyethylene succinate is 1.5:1-2:1.
Further preferably, in S3, the mass-volume ratio of the tetramethylammonium hydroxide modified shell to the embedding material solution is 1g (6-8) mL.
Further preferably, in S3, the freezing temperature is-40 ℃ to-30 ℃ and the freezing time is 24h to 30h.
Further preferably, in S4, the mass volume ratio of the frozen mixed material to the cross-linking agent is 1g (2-3) mL, and the time of the cross-linking reaction is 2-5 h.
Further preferably, in S4, the cross-linking agent is a mixed solution of a calcium chloride solution and a sodium sulfate solution in a mass ratio of 1:1-1:0.9; wherein the mass concentration of the calcium chloride solution is 0.3g/mL-0.5g/mL; the concentration of the sodium sulfate solution is 0.1mol/L-0.5mol/L.
Further preferably, in S4, the drying temperature is 80 ℃ to 100 ℃ and the drying time is 4h to 6h.
Preferably, the number ratio of the live bacteria of the paracoccus to the rhodococcus is 0.5-1:1-1.2, and the concentration of the live bacteria in the microbial liquid is (1X 10 7)-(1×109) CFU/mL.
Preferably, the paracoccus is paracoccus ubiquitosus with a deposit number BNCC 336995.
Preferably, the rhodococcus is rhodococcus equi with deposit number BNCC 186169.
The second aspect of the invention provides a preparation method of the bacteria-carrying slow-release carbon source, which comprises the following steps:
And uniformly mixing the slow-release carbon source filler with the microbial liquid, filtering and drying to obtain the bacteria-carrying slow-release carbon source.
Preferably, the mass volume ratio of the slow-release carbon source filler to the microbial liquid is 1g (2-3) mL.
Preferably, the culture medium used for the microbial broth is one or more of a nutrient broth culture medium, a secondary seed culture medium or a mixed fermentation culture medium.
The third aspect of the invention provides an application of the bacteria-carrying slow-release carbon source in degrading battery production wastewater.
In summary, the invention provides a bacteria-carrying slow-release carbon source, which utilizes the slow-release carbon source carrying the microbial liquid of degradable N-methyl pyrrolidone to carry out denitrification treatment on the wastewater produced by the lithium battery, so that not only is the N-methyl pyrrolidone difficult to treat in the wastewater degraded, but also the degradation of nitrate nitrogen is promoted. Tests show that the carrier slow-release carbon source provided by the invention can realize complete degradation of N-methylpyrrolidone and nitrate nitrogen in wastewater, and the degradation rate is up to 100%. The bacteria-carrying slow-release carbon source provided by the invention not only solves the technical problem that a large amount of carbon source is consumed when the production wastewater containing N-methyl pyrrolidone is treated by a biochemical method in the prior art, but also has low cost and simple operation, and provides a new idea for treating the production wastewater of lithium batteries.
Drawings
FIG. 1 is a graph showing the concentration change of N-methylpyrrolidone in wastewater produced by degrading N-methylpyrrolidone by using a carrier slow-release carbon source provided in examples 6 to 8 and comparative examples 1 to 2;
FIG. 2 is a graph showing the change in nitrate nitrogen concentration of wastewater from the degradation of N-methylpyrrolidone-containing production of the carrier slow-release carbon source provided in examples 6 to 8 and comparative examples 1 to 2.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a slow-release carbon source filler, which specifically comprises the following steps:
s1, crushing 50g of peanut shells, sieving with a 50-mesh sieve, adding into deionized water, soaking for 4 hours, and filtering to obtain pretreated shell powder;
S2, uniformly mixing the pretreated shell powder with 280mL of tetramethyl ammonium hydroxide solution with the concentration of 0.1mol/L, reacting at 90 ℃ for 6.5h, centrifuging at 1500rpm for 5min, washing with 30mL of deionized water for 3 times, and drying at 100 ℃ for 7h to obtain tetramethyl ammonium hydroxide modified shells;
S3, dissolving 50g of sodium alginate in 400mL of water, and stirring for 5 hours at 85 ℃ to obtain an embedding material solution; adding 50g of tetramethyl ammonium hydroxide modified fruit shell and 30g of polyethylene glycol succinate into the embedding material solution, reacting for 3 hours at 100 ℃, transferring the reaction system into a particle mould, freezing for 28 hours at-40 ℃, thawing to normal temperature, and then freezing for 26 hours at-35 ℃ to obtain a frozen mixed material;
S4, soaking the frozen mixed material in a cross-linking agent solution, performing cross-linking reaction at 3 ℃, washing for 2 times by adopting 50mL of deionized water after 4 hours of reaction, and drying for 5 hours at 90 ℃ to obtain the slow-release carbon source filler.
Wherein, the cross-linking agent adopts a calcium chloride solution and a sodium sulfate solution with the mass ratio of 1:1, and the mass concentration of the calcium chloride solution is 0.4g/mL; the concentration of the sodium sulfate solution is 0.3mol/L.
Example 2
The embodiment provides a microbial liquid, which specifically comprises the following steps:
S1, inoculating paracoccus pantoea and rhodococcus equi strain on a nutrient broth culture medium respectively, performing primary slant culture at 28 ℃, then performing secondary seed culture and mixed fermentation culture until the viable bacteria concentration in the product reaches 1X 10 8 CFU/mL, and obtaining paracoccus pantoea enlarged culture bacterial liquid and rhodococcus equi enlarged culture bacterial liquid;
S2, uniformly mixing 0.5mL of the paracoccus ubiquitously cultured bacterial liquid and 1mL of the rhodococcus equi cultured bacterial liquid to obtain the microbial bacterial liquid.
Wherein, the formula of the nutrient broth culture medium is as follows: beef extract 3g, protein wine 5g and water 1000mL; the pH of the nutrient broth was 7.3.
The formula of the secondary seed culture medium is as follows: 3% of hydrolyzed sugar, 3% of corn steep liquor, 0.4% of urea and K 2HPO4: 0.2% and MgSO 4: 0.05%; the pH of the secondary seed medium was 7.0.
The mixed fermentation medium adopts MRS medium.
Example 3
The embodiment provides a slow-release carbon source filler, which specifically comprises the following steps:
S1, crushing 50g of walnut shells, sieving with a 60-mesh sieve, soaking in deionized water for 4 hours, and filtering to obtain pretreated shell powder;
s2, uniformly mixing the pretreated shell powder with 300mL of tetramethyl ammonium hydroxide solution with the concentration of 0.1mol/L, reacting for 8 hours at 82 ℃, centrifuging for 8 minutes at the rotating speed of 1100rpm, washing for 3 times by adopting 30mL of deionized water, and drying for 8 hours at 90 ℃ to obtain tetramethyl ammonium hydroxide modified shells;
S3, dissolving 50g of sodium alginate in 450mL of water, and stirring for 5 hours at 90 ℃ to obtain an embedding material solution; adding 50g of tetramethyl ammonium hydroxide modified fruit shell and 33g of polyethylene glycol succinate into the embedding material solution, reacting for 3 hours at 100 ℃, transferring the reaction system into a particle mould, freezing for 30 hours at minus 35 ℃, thawing to normal temperature, and then freezing for 24 hours at minus 40 ℃ to obtain a frozen mixed material;
S4, soaking the frozen mixed material in a cross-linking agent solution, performing cross-linking reaction at 5 ℃, washing 2 times by adopting 50mL of deionized water after 2 hours of reaction, and drying at 90 ℃ for 5 hours to obtain the slow-release carbon source filler.
Wherein, the cross-linking agent adopts a calcium chloride solution and a sodium sulfate solution with the mass ratio of 1:1, and the mass concentration of the calcium chloride solution is 0.3g/mL; the concentration of the sodium sulfate solution is 0.1mol/L.
Example 4
The embodiment provides a slow-release carbon source filler, which specifically comprises the following steps:
S1, crushing 50g of Hawaii shells, sieving with a 40-mesh sieve, adding into deionized water, soaking for 4 hours, and filtering to obtain pretreated shell powder;
S2, uniformly mixing the pretreated shell powder with 250mL of tetramethyl ammonium hydroxide solution with the concentration of 0.3mol/L, reacting at 95 ℃ for 6h, centrifuging at 2000rpm for 3min, washing with 30mL of deionized water for 3 times, and drying at 100 ℃ for 7h to obtain tetramethyl ammonium hydroxide modified shells;
S3, dissolving 50g of sodium alginate in 500mL of water, and stirring for 4 hours at 85 ℃ to obtain an embedding material solution; adding 50g of tetramethyl ammonium hydroxide modified fruit shell and 25g of polyethylene glycol succinate into the embedding material solution, reacting for 3 hours at 100 ℃, transferring the reaction system into a particle mould, freezing for 28 hours at-40 ℃, thawing to normal temperature, and then freezing for 24 hours at-30 ℃ to obtain a frozen mixed material;
s4, soaking the frozen mixed material in a cross-linking agent solution, performing cross-linking reaction at 0 ℃, washing with 50mL of deionized water for 2 times after the cross-linking reaction is performed for 5 hours, and drying at 90 ℃ for 5 hours to obtain the slow-release carbon source filler.
Wherein, the cross-linking agent adopts a calcium chloride solution and a sodium sulfate solution with the mass ratio of 1:0.9, and the mass concentration of the calcium chloride solution is 0.5g/mL; the concentration of the sodium sulfate solution is 0.5mol/L.
Example 5
The embodiment provides a microbial liquid, which specifically comprises the following steps:
S1, inoculating paracoccus pantoea and rhodococcus equi strain on a nutrient broth culture medium respectively, performing primary slant culture at 28 ℃, then performing secondary seed culture and mixed fermentation culture until the viable count in the product reaches 1X 10 8 CFU/mL, and obtaining paracoccus pantoea enlarged culture bacterial liquid and rhodococcus equi enlarged culture bacterial liquid;
S2, uniformly mixing 1mL of the paracoccus ubiquitously cultured expansion bacterial liquid and 1mL of the rhodococcus equi cultured expansion bacterial liquid to obtain the microbial bacterial liquid.
Wherein, the formula of the nutrient broth culture medium is as follows: beef extract 3g, protein wine 5g and water 1000mL; the pH of the nutrient broth was 7.3.
The formula of the secondary seed culture medium is as follows: 3% of hydrolyzed sugar, 3% of corn steep liquor, 0.4% of urea and K 2HPO4: 0.2% and MgSO 4: 0.05%; the pH of the secondary seed medium was 7.0.
The mixed fermentation medium adopts MRS medium.
Example 6
The embodiment provides a bacteria-carrying slow-release carbon source, wherein the slow-release carbon source filler adopts the slow-release carbon source filler provided in the embodiment 1; the microbial liquid provided in the embodiment 2 is adopted, and specifically comprises the following steps:
and uniformly mixing the slow-release carbon source filler and the microbial liquid for the expanded culture according to the mass volume ratio of 1g to 2.5mL, filtering, and drying at 40 ℃ to obtain the bacteria-carrying slow-release carbon source.
Example 7
The embodiment provides a bacteria-carrying slow-release carbon source, wherein the slow-release carbon source filler adopts the slow-release carbon source filler provided in the embodiment 3; the microbial liquid provided in the example 5 is adopted, and specifically comprises the following steps:
And uniformly mixing the slow-release carbon source filler and the microbial liquid for the expanded culture according to the mass volume ratio of 1g to 2mL, filtering, and drying at 40 ℃ to obtain the bacteria-carrying slow-release carbon source.
Example 8
The embodiment provides a bacteria-carrying slow-release carbon source, wherein the slow-release carbon source filler adopts the slow-release carbon source filler provided in the embodiment 4; the microbial liquid provided in the embodiment 2 is adopted, and specifically comprises the following steps:
And uniformly mixing the slow-release carbon source filler and the microbial liquid for the expanded culture according to the mass-volume ratio of 1g to 3mL, filtering, and drying at 40 ℃ to obtain the bacteria-carrying slow-release carbon source.
Comparative example 1
This comparative example provides a carrier slow release carbon source, which differs from example 6 in that: the slow-release carbon source filler is starch-polyvinyl alcohol composite filler, other components and the preparation method remain unchanged, and the method specifically comprises the following steps:
and uniformly mixing the starch-polyvinyl alcohol composite filler and the microbial liquid for the expanded culture according to the mass volume ratio of 1g to 2.5mL, filtering, and drying at 40 ℃ to obtain the bacteria-carrying slow-release carbon source.
The preparation method of the starch-polyvinyl alcohol composite filler comprises the following steps:
S1, weighing 50g of starch and 50g of polyvinyl alcohol, dissolving in 200mL of deionized water, heating in a water bath to gradually raise the temperature of water from room temperature to 95 ℃, and stirring in the water bath at 95 ℃ for 1h to prepare a blend;
s2, pouring the blend into a particle grinding tool, putting into a refrigerator at the temperature of minus 20 ℃ for freezing for 20 hours, thawing for 4 hours at room temperature, freezing and thawing for 3 times, and drying for 24 hours at the temperature of 60 ℃ after demolding to obtain the starch-polyvinyl alcohol composite filler.
Comparative example 2
This comparative example provides a carrier slow release carbon source, which differs from example 6 in that: the microbial liquid is a pseudomonas aeruginosa liquid for enlarged culture, other components and the preparation method remain unchanged, and the method specifically comprises the following steps:
and uniformly mixing the slow-release carbon source filler and the microbial liquid for the expanded culture according to the mass volume ratio of 1g to 2.5mL, filtering, and drying at 40 ℃ to obtain the bacteria-carrying slow-release carbon source.
The preparation method of the amplified culture pseudomonas aeruginosa bacterial liquid comprises the following steps:
The pseudomonas aeruginosa is firstly subjected to primary slant culture on a culture medium at 30 ℃, then secondary seed culture and mixed fermentation culture until the viable count in the product reaches 1.0X10 9 CFU/mL.
Wherein, the formula of the culture medium is ：NH4Cl：1.0g,CH3COONa：3.5g,MgCl2：0.1g,CaCl2：0.1g,KH2PO4：0.6g,K2HPO4：0.4g, yeast extract: 0.1g and water: 1000mI; the pH of the medium was 7.2.
The formula of the secondary seed culture medium is as follows: 3% of hydrolyzed sugar, 3% of corn steep liquor, 0.4% of urea and K 2HPO4: 0.2% and MgSO 4: 0.05%; the pH of the secondary seed medium was 7.0.
The mixed fermentation medium adopts MRS medium.
In order to further prove the capability of the carrier slow-release carbon source provided by the invention to degrade the N-methyl pyrrolidone-containing production wastewater, the carrier slow-release carbon source obtained in examples 6-8 and comparative examples 1-2 is subjected to degradation test, the specific operation steps are shown in test example 1, and the test results are shown in table 1.
Test example 1
10G of the obtained bacteria-carrying slow-release carbon source is added into 500mL of lithium battery production wastewater which contains nitrate nitrogen and N-methyl pyrrolidone after deoxidization, degradation is carried out at 25 ℃ and 250rpm, and the concentration change of the nitrate nitrogen and the N-methyl pyrrolidone before and after wastewater treatment is monitored.
TABLE 1 degradation test results
According to table 1 and fig. 1-2, it can be seen that the bacteria-carrying slow-release carbon source provided by embodiments 6-8 of the invention can be successfully applied to degradation of battery production wastewater containing nitrate nitrogen and N-methylpyrrolidone, so as to realize efficient removal of nitrate nitrogen and N-methylpyrrolidone in the wastewater.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (8)
1. The application of a bacteria-carrying slow-release carbon source in degrading the battery production wastewater containing N-methyl pyrrolidone is characterized in that: the bacteria-carrying slow-release carbon source comprises slow-release carbon source filler and microbial bacteria liquid loaded on the surface of the slow-release carbon source filler; wherein the slow-release carbon source filler is a tetramethyl ammonium hydroxide modified shell/polyethylene glycol succinate compound; the microbial liquid is mixed liquid of paracoccus and rhodococcus;
the preparation method of the slow-release carbon source filler comprises the following steps:
s1, crushing and sieving shells, adding the crushed shells into deionized water, soaking, and filtering to obtain pretreated shell powder;
S2, uniformly mixing the pretreated shell powder and a tetramethyl ammonium hydroxide solution, reacting for 6-8 hours at 80-95 ℃, centrifuging, washing and drying to obtain tetramethyl ammonium hydroxide modified shells;
S3, dissolving the embedding material in water to obtain embedding material solution; adding the tetramethyl ammonium hydroxide modified fruit shell and polyethylene glycol succinate into the embedding material solution, reacting for 2-4 hours at 95-110 ℃, transferring into a mould, and freezing to obtain a frozen mixed material;
S4, uniformly mixing the frozen mixed material with a cross-linking agent, performing cross-linking reaction at 0-5 ℃, washing, and drying to obtain the slow-release carbon source filler;
s3, the embedding material is sodium alginate;
in S4, the time of the crosslinking reaction is 2-5 h.
2. The use of the bacteria-carrying slow-release carbon source of claim 1 for degrading N-methyl pyrrolidone-containing battery production wastewater, characterized in that: in the S1, the shell is any one or more of peanut shell, walnut shell or Hawaii shell; and/or
In S2, the concentration of the tetramethyl ammonium hydroxide solution is 0.1 mol/L-0.3 mol/L; and/or
S2, the mass volume ratio of the pretreated fruit shell to the tetramethylammonium hydroxide solution is 1g (4-6) mL; and/or
In S3, the mass concentration of the embedding material solution is 8 g/mL-10 g/mL.
3. The use of the bacteria-carrying slow-release carbon source of claim 1 for degrading N-methyl pyrrolidone-containing battery production wastewater, characterized in that: in S3, the mass ratio of the tetramethyl ammonium hydroxide modified fruit shell to the polyethylene glycol succinate is 1.5:1-2:1; and/or
S3, the mass volume ratio of the tetramethyl ammonium hydroxide modified shell to the embedding material solution is 1g (6-8) mL; and/or
S3, freezing at the temperature of-40 ℃ to-30 ℃ for 24-30 hours; and/or
And S4, the mass volume ratio of the frozen mixed material to the cross-linking agent is 1g (2-3) mL.
4. The use of the bacteria-carrying slow-release carbon source of claim 1 for degrading N-methyl pyrrolidone-containing battery production wastewater, characterized in that: s4, the cross-linking agent is a mixed solution of a calcium chloride solution and a sodium sulfate solution in a mass ratio of 1:1-1:0.9; wherein the mass concentration of the calcium chloride solution is 0.3 g/mL-0.5 g/mL, and the concentration of the sodium sulfate solution is 0.1 mol/L-0.5 mol/L.
5. The use of the bacteria-carrying slow-release carbon source of claim 1 for degrading N-methyl pyrrolidone-containing battery production wastewater, characterized in that: the number ratio of live bacteria of the paracoccus to the rhodococcus is 0.5-1:1-1.2, and the concentration of the live bacteria in the microbial bacteria liquid is (1X 10 7)~(1×109) CFU/mL.
6. The use of the bacteria-carrying slow-release carbon source of claim 1 for degrading N-methyl pyrrolidone-containing battery production wastewater, characterized in that: the paracoccus is paracoccus ubiquitosus, and the preservation number is BNCC 336995; and/or
The rhodococcus is rhodococcus equi and has a preservation number BNCC 186169.
7. The use of the bacteria-carrying slow-release carbon source of claim 1 for degrading N-methyl pyrrolidone-containing battery production wastewater, characterized in that: the preparation method of the bacteria-carrying slow-release carbon source comprises the following steps:
And uniformly mixing the slow-release carbon source filler with the microbial liquid, filtering and drying to obtain the bacteria-carrying slow-release carbon source.
8. The use of the bacteria-loaded slow-release carbon source of claim 7 for degrading N-methyl pyrrolidone-containing battery production wastewater, wherein the bacteria-loaded slow-release carbon source is characterized by: the mass volume ratio of the slow-release carbon source filler to the microbial liquid is 1g (2-3) mL.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793428A (en) * | 2018-06-27 | 2018-11-13 | 郑州大学 | A kind of preparation method of composite slow release carbon source |
| CN109913387A (en) * | 2019-03-19 | 2019-06-21 | 南京理工大学 | Degrade N-Methyl pyrrolidone enterobacteria and application in the treatment of waste water |
| CN112547012A (en) * | 2020-11-27 | 2021-03-26 | 郑州大学 | For VOCsPreparation method of adsorbed biomass-based activated carbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793428A (en) * | 2018-06-27 | 2018-11-13 | 郑州大学 | A kind of preparation method of composite slow release carbon source |
| CN109913387A (en) * | 2019-03-19 | 2019-06-21 | 南京理工大学 | Degrade N-Methyl pyrrolidone enterobacteria and application in the treatment of waste water |
| CN112547012A (en) * | 2020-11-27 | 2021-03-26 | 郑州大学 | For VOCsPreparation method of adsorbed biomass-based activated carbon |
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