CN115650426B - Efficient denitrification process based on micro-electrolysis waste iron mud-based filling material - Google Patents
Efficient denitrification process based on micro-electrolysis waste iron mud-based filling material Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 213
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 99
- 239000002699 waste material Substances 0.000 title claims abstract description 75
- 239000000463 material Substances 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 58
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 58
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000010865 sewage Substances 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 238000011282 treatment Methods 0.000 claims abstract description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 8
- 230000008878 coupling Effects 0.000 claims abstract description 5
- 238000010168 coupling process Methods 0.000 claims abstract description 5
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- 239000000843 powder Substances 0.000 claims description 75
- 239000011230 binding agent Substances 0.000 claims description 45
- 239000002245 particle Substances 0.000 claims description 34
- 239000011028 pyrite Substances 0.000 claims description 33
- 229910052683 pyrite Inorganic materials 0.000 claims description 33
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 17
- 239000000945 filler Substances 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 15
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- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 claims description 14
- 239000005995 Aluminium silicate Substances 0.000 claims description 10
- 235000012211 aluminium silicate Nutrition 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000428 dust Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
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- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
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- 238000002791 soaking Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000011343 solid material Substances 0.000 claims description 4
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- 239000002023 wood Substances 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 2
- 239000010902 straw Substances 0.000 claims description 2
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 17
- 239000002910 solid waste Substances 0.000 abstract description 5
- 239000002352 surface water Substances 0.000 abstract description 4
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- 241000894006 Bacteria Species 0.000 description 8
- 230000002572 peristaltic effect Effects 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
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- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
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- 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 4
- 238000005273 aeration Methods 0.000 description 4
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- 241001453382 Nitrosomonadales Species 0.000 description 3
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
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- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229910052863 mullite Inorganic materials 0.000 description 1
- 230000001546 nitrifying effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a high-efficiency biological denitrification process based on micro-electrolysis waste iron mud-based filling materials, which comprises a Feamox reaction area and an NDFO reaction area, wherein the effluent of the Feamox reaction area is the water inlet of the NDFO reaction area, an iron source provided by TF materials is adopted to provide an electron pair for the Feamox reaction, an iron source provided by TN materials is adopted to provide reduced iron for the NDFO reaction, the high-efficiency denitrification treatment of sewage containing ammonia and nitrogen is realized through the coupling of the two reactions and the two reactions, and finally ammonia nitrogen, total nitrogen and COD of the effluent can reach IV water standard limit values in the surface water environment quality standard (GB 3838-2002); meanwhile, the invention also realizes the recycling of solid waste resources, and changes waste iron mud, agricultural and forestry wastes and other solid waste resources generated by the micro-electrolysis of iron and carbon into valuable, thereby avoiding secondary pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a high-efficiency denitrification process based on a micro-electrolysis waste iron mud-based filling material.
Background
In recent years, with the continuous improvement of comprehensive strength, continuous acceleration of urban and industrialized degrees in China, the water environment problem is increasingly prominent, and the sustainable development of national economy and society in China is directly related. More than 75% of closed water bodies in the whole world have eutrophication problems. In 2019, the ammonia nitrogen emission amount in national sewage is up to 46.3 ten thousand tons.
The most widely used and most traditional biological denitrification technology is the nitrification-denitrification technology. Nitration (Nitriltion) refers to NH under the action of nitrifying bacteria 4 + Oxidized by oxygen to NO 2 - And NO 3 - Is a biological reaction of (a). The nitration is a sequential multistage process, NH 4 + Is oxidized to NO under the action of ammonia oxidizing bacteria (ammonia oxidizing bacteria, AOB) 2 - (formula 1.1) and then NO 2 - Oxidized to NO by nitrite oxidizing bacteria (nitrite-oxidizing bacteria, NOB) 3 - (formula 1.2). Denitrification (Denitrification) refers to the Denitrification of NO by denitrifying bacteria (denitrifying bacteria, DB) using an organic carbon source under anoxic conditions 2 - Or NO 3 - The reduction to nitrogen (formulas 1.3 and 1.4).
NH 4 + +1.5O 2 →NO 2 - +2H + +H 2 O (1.1)
NO 2 - +0.5O 2 →NO 3 - (1.2)
24NO 3 - +5C 6 H 12 O 6 →30CO 2 +12N 2 +18H 2 O+24OH - (1.3)
8NO 2 - +C 6 H 12 O 6 →6CO 2 +4N 2 +2H 2 O+8OH - (1.4)
The nitrification-denitrification process has the advantages of high efficiency and low cost. However, the chemical oxygen demand (ChemicalOxygenDemand, COD) in wastewater is a limiting factor for denitrification, and the C/N ratio plays a critical role in the biological denitrification process, and particularly has an important influence on the treatment of wastewater with lower C/N ratio. This is because the biological denitrification process is performed by heterotrophic bacteria using an organic carbon source as an electron donor, that is, the biological denitrification process needs to consume the organic carbon source, and the insufficient carbon source can cause the problems of incomplete denitrification, low actual sewage denitrification efficiency, and the like. Therefore, development of an economical and practical denitrification process is needed, so that wastewater lacking in carbon sources in a wastewater treatment plant can meet increasingly strict effluent standards, and the development of the economical and practical denitrification process is still a current research hotspot.
As a novel biological denitrification process rapidly developed in recent years, the Anammox process (anaerobic ammonia oxidation) has advantages of short process flow, no need of organic carbon source, low energy consumption, high treatment load, and the like, compared with the conventional nitrification-denitrification process. The Anamox process is to oxidize the NO by anaerobic ammonia oxidizing bacteria 2 - Reduction and NH 4 + Oxidation to give N 2 And NO 3 - Is a biological reaction of (a). The currently accepted anaerobic ammoxidation reaction formula (formula 1.5) is as follows: NH (NH) 4 + +1.32NO 2 - +0.066HCO 3 - +0.13H + →1.02N 2 +0.26NO 3 - +0.066CH 2 O 0.5 N 0.15 +2.03H 2 O (1.5)
However, the Anamox process has long reactor start-up time, low cell yield, inhibition of high concentration substrates, NH feed 4 + /NO 2 - The application of the composite material in practical engineering is limited by the influence of unbalance, high sensitivity to external environment and other factors.
In the existing sewage denitrification technology, the denitrification process has the defects that the actual sewage denitrification efficiency is low due to incomplete denitrification caused by insufficient carbon source, the sewage treatment cost is increased and secondary pollution is caused because the additional carbon source is needed for improving the denitrification efficiency, and meanwhile, the process flow is complex, the structures are more, the construction cost is high and the like. The Anamox process has the disadvantage of introducing NH 4 + /NO 2 - Unbalance and high sensitivity to external environment.
Feamox (iron ammoxidation) is a biological reaction process that can utilize Fe 3+ NH is added to 4 + Oxidation to N 2 、NO 3 - Or NO 2 - By Fe (OH) 3 The reaction equation of Feamox as an electron acceptor is as follows (formula 2.1-formula 2.3). Most studies indicate that Feamox functional bacteria are an autotrophic bacteria that do not consume carbon sources. Therefore, the Feamox process can be used for treating NH in sewage 4 + Is a potential approach to (a) is provided. However, the Feamox reaction is only performed on Fe 3+ Can be realized only when the participation amount is large, and Fe 3+ The method is extremely easy to form a precipitate under the non-acidic condition, and is easy to cause sludge surface crust during the long-term running process of the Feamox, which is unfavorable for the utilization of the substrate by microorganisms, and is the source of the large-scale practical application of the Feamox processTherefore, if the Feammox process is to be applied to practical engineering, it is necessary to select an appropriate iron source for the process.
3Fe(OH) 3 +5H + +NH 4 + →3Fe 2+ +9H 2 O+0.5N 2 (2.1)
3Fe(OH) 3 +10H + +NH 4 + →6Fe 2+ +16H 2 O+NO 2 - (2.2)
3Fe(OH) 3 +14H + +NH 4 + →8Fe 2+ +21H 2 O+NO 3 - (2.3)
NDFO (nitrate dependent ferrous oxidation) is also a biological reaction process that can utilize NO 3 - Fe is added to 2+ Oxidizing and applying the released electrons to NO 3 - Reduction to N 2 The process (formula 2.4) does not consume carbon source, so the NDFO process can be used for treating NO in sewage 3 - Is a potential approach to (a) is provided. However, NDFO requires a large amount of Fe 2+ Is involved in Fe 2+ Precipitate is also very easily formed and is very unstable under non-acidic conditions, so that it is also necessary to select a suitable iron source for NDFO process to be used in practical engineering.
10Fe 2+ +2NO 3 - +12H + →10Fe 3+ +N 2 +6H 2 O (2.4)
The iron-carbon micro-electrolysis process is a common process for treating high-concentration organic sewage at present, and is widely applied to the industries of textile, pharmacy, papermaking, chemical industry and the like. However, iron-carbon micro-electrolysis can produce a large amount of iron-containing chemical sludge, the iron content of the iron-carbon micro-electrolysis waste iron sludge is extremely high, if the iron-carbon micro-electrolysis waste iron sludge is treated like ordinary biochemical sludge, the waste of resources can be caused, and if the iron-carbon micro-electrolysis waste iron sludge cannot be well treated, secondary pollution can be caused to the environment. Therefore, the micro-electrolysis waste iron mud is a solid waste resource object with great potential, and in view of the characteristic of high iron content in the micro-electrolysis waste iron mud, the micro-electrolysis waste iron mud is considered to be used as an iron source to provide reaction substrates for Feamox and NDFO.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a high-efficiency biological denitrification process based on a micro-electrolysis waste iron mud-based filling material. The process has the advantages of no need of additional carbon source, no need of aeration, high denitrification efficiency, stable operation and the like.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a high-efficiency biological denitrification process based on micro-electrolysis waste iron mud-based filling materials comprises a Feamox reaction zone and an NDFO reaction zone, wherein the effluent of the Feamox reaction zone is the water inlet of the NDFO reaction zone, the Feamox reaction zone adopts an iron source provided by a filler I to provide an electron pair for the Feamox reaction, the NDFO reaction zone adopts an iron source provided by a filler II to provide reduced iron for the NDFO reaction, and denitrification treatment of ammonia nitrogen-containing sewage is realized through coupling the Feamox reaction with the NDFO reaction and performing biological denitrification twice;
wherein the filler I is TF material, and the raw materials comprise the following components in percentage by mass: 25-35% of waste iron mud generated by iron-carbon micro-electrolysis, 60-70% of binder and 2-5% of agriculture and forestry waste;
the filler II is TN material, and comprises the following raw materials in percentage by mass: 15-20% of waste iron mud produced by iron-carbon micro-electrolysis, 55-60% of binder and 25-30% of pyrite.
Preferably, the binder comprises kaolin, fly ash, caO and MgO, and the sum of the masses of the kaolin and the fly ash accounts for 70-90% wt of the total mass of the binder; the agricultural and forestry waste is one or a combination of more of sawdust, wood dust and straw.
Preferably, the TF material is prepared by the following steps: (a) Crushing and grinding waste iron mud and binder generated by micro-electrolysis of iron and carbon respectively, and sieving with a 100-200 mesh sieve to obtain waste iron mud powder and binder powder; (b) Crushing and grinding the agricultural and forestry waste, and sieving with a 40-100 mesh sieve to obtain agricultural and forestry waste powder; (c) Adding the waste iron mud powder, the agriculture and forestry waste powder and the binder powder into deionized water, uniformly mixing, granulating and drying to obtain mixed particles; (d) And calcining the obtained mixed particles, and cooling to room temperature to obtain the TF material.
Preferably, the mass of the deionized water is 10-15% wt of the total mass of the solid materials, the particle size of the mixed particles is 6-9 mm, the drying temperature is 105-130 ℃, and the drying time is 8-15 h.
Preferably, the process conditions of the calcination treatment are as follows: heating to 400-450 ℃ at a heating rate of 10-15 ℃/min, preheating for 5-50 min, heating to 1050-1200 ℃ and preserving heat for 35-45 min.
Preferably, the TN material is prepared by the following steps: (a) Crushing and grinding waste iron mud, a binder and pyrite generated by micro-electrolysis of iron and carbon respectively, and sieving with a 100-200 mesh sieve to obtain waste iron mud powder, a binder powder and pyrite powder; (b) Soaking the obtained pyrite powder with dilute hydrochloric acid to remove carbonate and surface oxide layers possibly existing in a sample, washing the soaked pyrite powder with distilled water to be neutral, and freeze-drying the soaked pyrite powder for later use; (c) Adding the waste iron mud powder, the pyrite powder and the binder powder into deionized water, uniformly mixing, granulating and vacuum drying to obtain mixed particles; (d) And (3) placing the obtained mixed particles in a protective gas atmosphere for calcination treatment, and cooling to room temperature to obtain the TN material.
Preferably, the mass of the deionized water is 10-15% wt of the total mass of the solid materials, the particle size of the mixed particles is 6-9 mm, and the conditions of vacuum drying are as follows: the cold trap temperature is-40 ℃ to-20 ℃, the vacuum degree is 5Pa to 20Pa, and the holding time is 12 to 24 hours.
Preferably, the process conditions of the calcination treatment are as follows: heating to 1000-1100 deg.c at the heating rate of 5-10 deg.c/min and maintaining for 0.5-3 hr.
Preferably, in step S1, the residence time is 10 to 12 hours in the first stage reactor.
Preferably, in step S2, the residence time is 6 to 8 hours in the second stage reactor.
The invention has the following beneficial effects:
(1) According to the invention, the self-made TF material and TN material which are prepared by taking micro-electrolysis waste iron mud as raw materials are utilized to provide respective required iron sources for a Feamox reaction zone and an NDFO reaction zone respectively, and the denitrification treatment of sewage containing ammonia nitrogen is realized through coupling the Feamox reaction with the NDFO reaction and two times of biological denitrification, so that the problem of substrate crusting of the existing Feamox and NDFO processes is solved; wherein, through the iron source (providing electron pair) provided by TF material, the Feamox reaction process of the first stage is realized, and the sewage containing ammonia nitrogen is successfully converted into the sewage containing nitrate nitrogen; the NDFO reaction process of the second stage is realized through an iron source (reduced iron) provided by the TN material, so that the nitrate nitrogen sewage is successfully converted into standard drainage, the removal of ammonia nitrogen and total nitrogen is well realized, and the denitrification efficiency is high and the operation is stable. The ammonia nitrogen, total nitrogen and COD of the finally detected effluent can reach the IV water standard limit value in the quality standard (GB 3838-2002) of the surface water environment.
(2) Because the reaction process of Feamox and NDFO is an autotrophic process, the denitrification process does not need an additional carbon source in the operation process; because the two-stage reactors are all anaerobic processes, aeration is not needed; the anaerobic biological treatment has slower microorganism growth and lower sludge yield, so the residual sludge amount is less.
(3) The denitrification process not only can realize the high-efficiency denitrification of the sewage containing ammonia and nitrogen, but also can realize the recycling of solid waste resources, so that solid waste resources such as waste iron mud, agriculture and forestry waste and the like generated by the micro-electrolysis of iron and carbon are turned into wealth, and secondary pollution to the environment is avoided.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a biological denitrification device according to the present invention;
FIG. 2 is an XRD pattern of the micro-electrolytic scrap iron sludge and binder;
FIG. 3 is an XRD pattern of the TF material prepared in example 1;
FIG. 4 is an XRD pattern of TN material prepared in example 1;
FIG. 5 is a graph showing the change in ammonia nitrogen concentration of the water fed into and discharged from the first stage reactor;
FIG. 6 is a graph showing the total nitrogen concentration variation of the water fed into and discharged from the first stage reactor;
FIG. 7 is a graph of the change in nitrate nitrogen concentration of the first stage reactor inlet and outlet water;
FIG. 8 is a graph showing the change in ammonia nitrogen concentration of water entering and exiting the second stage reactor;
FIG. 9 is a graph showing the total nitrogen concentration variation of the second stage reactor inlet and outlet water;
FIG. 10 is a bar graph of COD (chemical oxygen demand) change of the second stage reactor inlet and outlet water.
Reference numerals:
1. a water inlet tank; 2. a first peristaltic pump; 3. a first water inlet; 4. a first reactor; 5. cobblestones; 6. TF material; 7. a first gas collecting port; 8. a first water outlet; 9. a first-stage water outlet tank; 10. a second peristaltic pump; 11. a second water inlet; 12. a second reactor; 13. TN material; 14. a second gas collecting port (for discharging gas generated in the reaction process, and not aeration); 15. a second water outlet; 16. a secondary water outlet tank.
Detailed Description
In the following description, for purposes of explanation and not limitation, specific details are set forth such as the particular system architecture, techniques, etc., in order to provide a thorough understanding of the embodiments of the present invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details.
The invention provides a high-efficiency biological denitrification system based on micro-electrolysis waste iron mud-based filling materials, which comprises a water inlet tank, a Feamox reaction zone, an NDFO reaction zone and a water outlet tank which are connected in sequence; wherein, an iron source provided by a filler I is adopted in the Feamox reaction zone to provide electron pairs for Feamox reaction; the NDFO reaction zone adopts an iron source provided by a filler II to provide reduced iron for the NDFO reaction, and the nitrogen-containing sewage is subjected to denitrification treatment by coupling the Feamox reaction and the NDFO reaction and performing biological denitrification twice.
Specifically, referring to fig. 1, the above-mentioned high-efficiency biological denitrification system based on the micro-electrolysis scrap iron mud-based packing material comprises: a water inlet tank 1, a first-stage reactor 4, a first-stage water outlet tank 9, a second-stage reactor 12 and a second-stage water outlet tank 16; one side of the water inlet tank 1 is provided with a first peristaltic pump 2, the first-stage reactor 4 is provided with a first water inlet 3, a cobble supporting layer, a filler I, a first air collecting port 7 and a first water outlet 8, the second-stage reactor 12 is provided with a second water inlet 11, a cobble supporting layer, a filler II, a second air collecting port 14 and a second water outlet 15, one side of the first-stage water outlet tank 9 is provided with a second peristaltic pump 10, and the first-stage reactor 4 and the second-stage reactor 12 are both in an upflow anaerobic biological filter (UAF) configuration, and water enters from the bottom and water exits from the top. The high-efficiency biological denitrification process based on the micro-electrolysis waste iron mud-based filling material by utilizing the high-efficiency biological denitrification system based on the micro-electrolysis waste iron mud-based filling material comprises the following steps:
s1, pumping the sewage containing ammonia and nitrogen in the water inlet tank 1 into a first-stage reactor 4 from a first water inlet 3 through a first peristaltic pump 2, mixing with a filler I, staying for 10-12 h, and enabling the obtained effluent to flow into a first-stage water outlet tank 9 from a first water outlet 8 for temporary storage;
s2, pumping the sewage subjected to the primary treatment temporarily stored in the primary water outlet tank 9 into a secondary reactor 12 through a second water inlet 11 by a second peristaltic pump 10, mixing with a filler II, and staying for 6-8 hours, wherein the obtained effluent flows into a secondary water outlet tank 16 from a second water outlet 15, and the obtained effluent is the effluent of biological denitrification;
wherein the filler I is a self-made TF material, and comprises the following raw materials in percentage by mass: 25-35% of waste iron mud generated by iron-carbon micro-electrolysis, 60-70% of binder and 2-5% of agriculture and forestry waste;
the filler II is a self-made TN material and comprises the following raw materials in percentage by mass: 15-20% of waste iron mud generated by iron-carbon micro-electrolysis, 55-60% of binder and 25-30% of pyrite; the binder comprises kaolin, fly ash, caO and MgO, and the sum of the masses of the kaolin and the fly ash accounts for 70-90% by weight of the total mass of the binder.
Example 1
Preparing TF material: (a) Crushing and grinding 35 parts of waste iron mud generated by iron-carbon micro-electrolysis and 60 parts of binder (which are obtained by mixing kaolin, fly ash, caO and MgO according to the mass ratio of 6:6:1:1) respectively, and sieving with a 150-mesh sieve to obtain waste iron mud powder and binder powder; (b) Crushing and grinding 5 parts of saw dust, and sieving with a 60-mesh sieve to obtain saw dust powder; (c) Adding waste iron mud powder, saw dust powder and binder powder into 12 parts of deionized water, uniformly mixing, granulating, and drying in a forced air drying oven at 110 ℃ for 12 hours to obtain mixed particles with the particle size of 6-9 mm; (d) And (3) placing the obtained mixed particles in a muffle furnace, heating to 450 ℃ at a heating rate of 15 ℃/min, preheating for 20min, continuously heating to 1100 ℃ for calcining, preserving heat for 40min, and finally naturally cooling to room temperature to obtain the TF material.
Preparing TN material: (a) Respectively crushing and grinding 15 parts of waste iron mud generated by micro-electrolysis of iron and carbon, 60 parts of binder (prepared by mixing kaolin, fly ash, caO and MgO according to a mass ratio of 6:6:1:1) and 25 parts of pyrite, and sieving with a 150-mesh sieve to obtain iron mud powder, binder powder and pyrite powder; (b) Soaking the obtained pyrite powder with dilute hydrochloric acid to remove carbonate and surface oxide layers possibly existing in a sample, washing the soaked pyrite powder with distilled water to be neutral, and freeze-drying the soaked pyrite powder for later use; (c) Adding waste iron mud powder, pyrite powder and binder powder into 15 parts of deionized water, uniformly mixing, granulating, then placing into a vacuum freeze dryer, vacuumizing to 15Pa, setting the cold trap temperature to-40 ℃ and keeping for 12 hours to obtain mixed particles with the particle size of 6-9 mm; (d) And (3) placing the obtained mixed particles in a protective gas atmosphere, heating to 1100 ℃ at a heating rate of 8 ℃/min for calcination, preserving heat for 0.5h, and naturally cooling to room temperature to obtain the TN material. The characterization results are shown in Table 1 and FIGS. 2-4.
The results in table 1 and fig. 2 show that the waste iron mud produced by the iron-carbon micro-electrolysis has no obvious diffraction peak in the XRD result because the crystallinity is not high; whereas XRD results of the binder show the main components as silica and alumina.
TABLE 1 XRF results for waste iron sludge and binders produced by microelectrolysis
| Fe 2 O 3 | SiO 2 | CaO | Al 2 O 3 | CO 2 | Na 2 O | TiO 2 | MgO | K 2 O | |
| Waste iron mud | 82.12％ | 4.34％ | 4.32％ | 0.71％ | 4.34％ | 0.13％ | 0.05％ | 0.41％ | 0.06％ |
| Adhesive agent | 2.99％ | 42.73％ | 11.93％ | 30.95％ | 3.76％ | -- | 1.18％ | 4.28％ | 1.21％ |
As can be seen from the results of fig. 3, the main form of iron in the obtained TF material is ferric oxide, and after high-temperature calcination, mineral phases such as mullite are formed in the TF material, so that the TF material forms a main framework and is used as a stress framework to provide strength for the TF material.
As can be seen from the results of fig. 4, the main form of iron in the obtained TN material was FeS.
Example 2
Preparing TF material: (a) Crushing and grinding waste iron mud produced by micro-electrolysis of 25 parts of iron and carbon and 70 parts of binder (which are obtained by mixing kaolin, fly ash, caO and MgO according to a mass ratio of 6:6:1:1) respectively, and sieving with a 100-mesh sieve to obtain waste iron mud powder and binder powder; (b) Crushing and grinding 5 parts of saw dust, and sieving with a 100-mesh sieve to obtain saw dust powder; (c) Adding waste iron mud powder, saw dust powder and binder powder into 15 parts of deionized water, uniformly mixing, granulating, and drying in a forced air drying oven at 120 ℃ for 12 hours to obtain mixed particles with the particle size of 6-9 mm; (d) And (3) placing the obtained mixed particles in a muffle furnace, heating to 420 ℃ at a heating rate of 10 ℃/min, preheating for 35min, continuously heating to 1100 ℃ for calcination, preserving heat for 40min, and finally naturally cooling to room temperature to obtain the TF material.
Preparing TN material: (a) Crushing and grinding 20 parts of waste iron mud produced by micro-electrolysis of iron and carbon, 55 parts of binder and 25 parts of pyrite respectively according to parts by mass, and sieving with a 100-mesh sieve to obtain waste iron mud powder, binder powder and pyrite powder; (b) Soaking the obtained pyrite powder with dilute hydrochloric acid to remove carbonate and surface oxide layers possibly existing in a sample, washing the soaked pyrite powder with distilled water to be neutral, and freeze-drying the soaked pyrite powder for later use; (c) Adding waste iron mud powder, pyrite powder and binder powder into 15 parts of deionized water, uniformly mixing, granulating, then placing into a vacuum freeze dryer, vacuumizing to 15Pa, setting the cold trap temperature to-40 ℃ and keeping for 18 hours to obtain mixed particles with the particle size of 6-9 mm; (d) And (3) placing the obtained mixed particles in a protective gas atmosphere, heating to 1050 ℃ at a heating rate of 10 ℃/min for calcining, preserving heat for 3 hours, and naturally cooling to room temperature to obtain the TN material.
Example 3
Preparing TF material: (a) Crushing and grinding 32 parts of waste iron mud generated by iron-carbon micro-electrolysis and 65 parts of binder (which are obtained by mixing kaolin, fly ash, caO and MgO according to the mass ratio of 6:6:1:1) respectively, and sieving with a 150-mesh sieve to obtain waste iron mud powder and binder powder; (b) Crushing and grinding 3 parts of agricultural and forestry waste (sawdust and wood chips in a mass ratio of 1:1), and sieving with a 60-mesh sieve to obtain agricultural and forestry waste powder; (c) Adding waste iron mud powder, agriculture and forestry waste powder and binder powder into 12 parts of deionized water, uniformly mixing, granulating, and drying in a blast drying oven at 105 ℃ for 12 hours to obtain mixed particles with the particle size of 6-9 mm; (d) And (3) placing the obtained mixed particles in a muffle furnace, heating to 450 ℃ at a heating rate of 15 ℃/min, preheating for 10min, continuously heating to 1200 ℃ for calcining, preserving heat for 40min, and finally naturally cooling to room temperature to obtain the TF material.
Preparing TN material: (a) Crushing and grinding 18 parts of waste iron mud produced by micro-electrolysis of iron and carbon, 62 parts of binder and 20 parts of pyrite respectively according to parts by mass, and sieving with a 200-mesh sieve to obtain waste iron mud powder, binder powder and pyrite powder; (b) Soaking the obtained pyrite powder with dilute hydrochloric acid to remove carbonate and surface oxide layers possibly existing in a sample, washing the soaked pyrite powder with distilled water to be neutral, and freeze-drying the soaked pyrite powder for later use; (c) Adding waste iron mud powder, pyrite powder and binder powder into 15 parts of deionized water, uniformly mixing, granulating, then placing into a vacuum freeze dryer, vacuumizing to 10Pa, setting the cold trap temperature to minus 30 ℃ and keeping for 24 hours to obtain mixed particles with the particle size of 6-9 mm; (d) And (3) placing the obtained mixed particles in a protective gas atmosphere, heating to 1000 ℃ at a heating rate of 5 ℃/min for calcination, preserving heat for 1h, and naturally cooling to room temperature to obtain the TN material.
The TF material and the TN material prepared in the above example 1 were filled in the first stage reactor 4 and the second stage reactor 12, and then the sewage containing ammonia nitrogen to be treated was flowed into the water inlet tank 1, and the water quality index thereof is shown in table 2.
TABLE 2 Water quality index of wastewater containing ammonia and nitrogen to be treated
Firstly, pumping the sewage containing ammonia and nitrogen to be treated in a water inlet tank 1 into a first stage reactor 4 from a first water inlet 3 through a first peristaltic pump 2, mixing with TF materials and staying for 12 hours, and naturally flowing the obtained effluent into a first stage water outlet tank 9 from a first water outlet 8 for temporary storage;
then, the sewage after the primary treatment temporarily stored in the primary water outlet tank 9 is pumped into the secondary reactor 12 through the second water inlet 11 by the second peristaltic pump 10, is mixed with TN materials and stays for 6 hours, and the obtained effluent naturally flows into the secondary water outlet tank 16 from the second water outlet 15, so that the obtained effluent is the effluent of biological denitrification.
The first stage reactor 4 produces water:
during the process operation (0-86 days), the concentration changes of ammonia nitrogen, total nitrogen, nitrate nitrogen and nitrite nitrogen in the water inlet and outlet of the first-stage reactor 4 are shown in fig. 5-7.
As can be seen from the results of FIGS. 5 to 7, the NH in the effluent of the first stage reactor 4 at the initial stage of operation 4 + The N concentration and the total nitrogen concentration are significantly higher than those of the feed water, mainly because of the lack of carbon source at this stage, the death of heterotrophic microorganisms in the inoculated sludge and of some autotrophic microorganisms that are not able to obtain nutrients, leading to NH in the system 4 + -increase in N (ammonia nitrogen) and total nitrogen concentration. After the first stage reactor 4 was operated for 23d, water NH was discharged 4 + -N starts to steadily decrease until 57d, yielding waterNH 4 + -the N concentration has been substantially 0; because high-purity nitrogen is used for aeration for 20min every water distribution, the concentration of dissolved oxygen in the water fed into the first reactor 4 is very low, so that the possibility of ammonia nitrogen oxidation caused by aerobic nitration reaction is eliminated, and a possible electron acceptor in the first-stage reactor 4 is Fe 3+ Therefore, it is considered to be Fe 3+ And NH 4 + The reaction, namely the Feamox reaction, occurs; after 60d, the effluent NH of the first stage reactor 4 4 + The N concentration was almost 0, the average total nitrogen concentration at the outlet of the first stage reactor 4 was 29.19mg/L, and the average total nitrogen removal was 14.19%. As can be seen from the results of FIG. 7, after passing through the first stage reactor 4, the N element in the feed water is substantially converted into NO 3 - -N.
The second stage reactor 12 effluent:
the effluent of the second-stage reactor 12 is the effluent of the whole denitrification process, and the changes of ammonia nitrogen, total nitrogen concentration and COD (chemical oxygen demand) of the effluent of the second-stage reactor 12 are shown in figures 8-10 in the operation period (0-89 d).
As can be seen from the results of FIGS. 8-10, since the first stage reactor 4 has been able to completely convert ammonia nitrogen, but the ammonia nitrogen is substantially converted to NO 3 - N, the second stage reactor 12 is provided for the purpose of NO removal 3 - N, the main form of iron in the TN material in the second stage reactor 12 is FeS (as known from XRD results of the TN material), i.e. iron in reduced form, which provides a precondition for NDFO reactions. After 89d operation, the total nitrogen in the effluent of the second-stage reactor 12 can meet the standard limit value of IV-class water in the following table 3 of the surface water environment quality standard (GB 3838-2002), so that NO in the effluent of the first-stage reactor 4 can be identified 3 - N NDFO reaction takes place in the second stage reactor 12, which is in turn converted to N 2 And the denitrification treatment is realized.
TABLE 3 class IV Water Standard Limit
Meanwhile, ammonia nitrogen and COD (chemical oxygen demand) of the discharged water also meet the IV water standard limit value in the table 3 of the surface water environment quality standard (GB 3838-2002). Therefore, the high-efficiency biological denitrification process based on the micro-electrolysis waste iron mud-based filling material provided by the invention can realize high-efficiency denitrification of sewage containing ammonia and nitrogen.
The present invention is not limited to the above-described specific embodiments, and various modifications may be made by those skilled in the art without inventive effort from the above-described concepts, and are within the scope of the present invention.
Claims (7)
1. The efficient biological denitrification process based on the micro-electrolysis waste iron mud-based filling material is characterized by comprising a Feamox reaction zone and an NDFO reaction zone, wherein the effluent of the Feamox reaction zone is the influent water of the NDFO reaction zone, the Feamox reaction zone adopts an iron source provided by a filler I to provide an electron pair for the Feamox reaction, the NDFO reaction zone adopts an iron source provided by a filler II to provide reduced iron for the NDFO reaction, and denitrification treatment of sewage containing ammonia and nitrogen is realized by coupling the Feamox reaction with the NDFO reaction and performing biological denitrification twice;
wherein the filler I is TF material, and the raw materials comprise the following components in percentage by mass: 25-35% of waste iron mud generated by iron-carbon micro-electrolysis, 60-70% of binder and 2-5% of agriculture and forestry waste;
the filler II is TN material, and comprises the following raw materials in percentage by mass: 15-20% of waste iron mud generated by iron-carbon micro-electrolysis, 55-60% of binder and 25-30% of pyrite;
the binder comprises kaolin, fly ash, caO and MgO, and the sum of the masses of the kaolin and the fly ash accounts for 70-90% by weight of the total mass of the binder; the agricultural and forestry waste is one or a combination of more of sawdust, wood dust and straw;
the TF material is prepared through the following steps: (a) Crushing and grinding waste iron mud and a binder generated by micro-electrolysis of iron and carbon respectively, and sieving with a 100-200 mesh sieve to obtain waste iron mud powder and binder powder; (b) Crushing and grinding the agricultural and forestry waste, and sieving with a 40-100 mesh sieve to obtain agricultural and forestry waste powder; (c) Adding the waste iron mud powder, the agriculture and forestry waste powder and the binder powder into deionized water, uniformly mixing, granulating and drying to obtain mixed particles; (d) Calcining the obtained mixed particles, and cooling to room temperature to obtain TF material;
the TN material is prepared by the following steps: (a) Crushing and grinding waste iron mud, a binder and pyrite generated by micro-electrolysis of iron and carbon respectively, and sieving with a 100-200 mesh sieve to obtain waste iron mud powder, a binder powder and pyrite powder; (b) Soaking the obtained pyrite powder with dilute hydrochloric acid to remove carbonate and surface oxide layers possibly existing in a sample, washing the soaked pyrite powder with distilled water to be neutral, and freeze-drying the soaked pyrite powder for later use; (c) Adding the waste iron mud powder, the pyrite powder and the binder powder into deionized water, uniformly mixing, granulating and vacuum drying to obtain mixed particles; (d) And (3) placing the obtained mixed particles in a protective gas atmosphere for calcination treatment, and cooling to room temperature to obtain the TN material.
2. The efficient biological denitrification process based on the micro-electrolysis scrap iron mud-based filling material according to claim 1, wherein in the process of preparing the TF material, the mass of deionized water is 10-15% wt of the total mass of the solid material, the particle size of the mixed particles is 6-9 mm, the drying temperature is 105-130 ℃, and the drying time is 8-15 h.
3. The efficient biological denitrification process based on micro-electrolysis scrap iron mud-based packing material according to claim 1, wherein in the process of preparing TF material, the process conditions of the calcination treatment are: heating to 400-450 ℃ at a heating rate of 10-15 ℃/min, preheating for 5-50 min, heating to 1050-1200 ℃, and preserving heat for 35-45 min.
4. The efficient biological denitrification process based on the micro-electrolysis scrap iron mud-based filling material according to claim 1, wherein in the process of preparing TN materials, the mass of deionized water is 10-15% wt of the total mass of solid materials, the particle size of mixed particles is 6-9 mm, and the conditions of vacuum drying are as follows: the temperature of the cold trap is-40 ℃ to-20 ℃, the vacuum degree is 5Pa to 20Pa, and the holding time is 12 to 24 hours.
5. The efficient biological denitrification process based on the micro-electrolysis scrap iron mud-based filling material according to claim 1, wherein in the process of preparing TN material, the process conditions of the calcination treatment are as follows: and heating to 1000-1100 ℃ at a heating rate of 5-10 ℃/min, and preserving heat for 0.5-3 h.
6. The efficient biological denitrification process based on the micro-electrolysis scrap iron mud-based filling material according to claim 1, wherein the residence time of water in the Feamox reaction zone is 10-12 h.
7. The efficient biological denitrification process based on the micro-electrolysis scrap iron mud-based filling material according to claim 1, wherein the residence time of water in the NDFO reaction zone is 6-8 hours.
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