CN113912179A - Rapid culture method for anaerobic ferric salt oxidized ammonia nitrogen and synchronous denitrification sludge - Google Patents
Rapid culture method for anaerobic ferric salt oxidized ammonia nitrogen and synchronous denitrification sludge Download PDFInfo
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Abstract
A rapid culture method for anaerobic ferric salt oxidized ammonia nitrogen and synchronous denitrification sludge belongs to the field of water environment recovery and regeneration and utilizes Fe3+The ammonia nitrogen is oxidized and the synchronous denitrification is realized, and the problems of high aeration energy consumption and insufficient carbon source in the traditional biological denitrification technology are solved. The upper part of an up-flow type mud-film mixing reactor is filled with a three-dimensional latticed fiber filler made of polyvinylidene chloride, the bottom of the reactor is inoculated with anaerobic ammonia oxidation granular sludge, inflow water is artificially distributed and contains NH4Cl and FeCl3·6H2O; controlling the temperature in the reactor to be 25-30 ℃, controlling the pH to be 7.0-9.0, and maintaining an anaerobic environment in the reactor; the reactor adopts a periodic operation mode, and each period is divided into water inlet, reaction, precipitation and drainage stages. The invention greatly shortens the culture time of the sludge, improves the operation stability, and has the ammonia nitrogen removal rate of over 95 percent and the total nitrogen removal rate of over 90 percent.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and relates to a rapid culture method for ammonia nitrogen oxidation and synchronous denitrification of sludge by using anaerobic ferric salt.
Background
The traditional biological denitrification of the urban domestic sewage adopts nitrification and denitrification processes. Under aerobic conditions, nitrifying bacteria oxidize ammonia nitrogen into nitrate nitrogen by using oxygen; under anoxic conditions, denitrifying bacteria utilize a carbon source to reduce nitrate to nitrogen. The traditional biological denitrification technology has the problems of large sludge yield, high aeration energy consumption, insufficient carbon source and the like.
In recent years, researchers have reported a novel microbial nitrogen cycle pathway-anammox reaction. Under anaerobic condition, the anaerobic molysite ammonia oxidizing bacteria can utilize Fe3+Reacting NH4 +Oxidation of-N to NO2 --N、NO3 --N or N2，Fe3+Is reduced to Fe2+. The iron salt denitrifying bacteria can utilize Fe2+Adding NO3 --N and NO2 -Conversion of-N to N2，Fe2+Is oxidized into Fe3+. The anaerobic iron ammoxidation reaction plays an important role in biological denitrification of paddy field soil, riparian zone sediments and forest wetland soil. At present, few researches on enrichment and culture of anaerobic iron ammonia oxidizing bacteria are carried out at home and abroad. The anaerobic molysite ammonia oxidizing bacteria are autotrophic bacteria, have slow growth rate and are difficult to enrich and culture. Some studies have shown that anammox sludge can utilize ferric iron to convert ammonia nitrogen to nitrate nitrogen and nitrogen. The granular sludge formed by the microorganisms has the characteristics of good sedimentation performance, high biological concentration, impact load resistance, toxicity resistance and the like, and can better solve the problems of long sludge-water separation time, easy sludge loss, high volume load rate and the like in the traditional process. The biofilm reactor has good microorganism adhesion capability and is beneficial to realizing the rapid enrichment of anaerobic iron salt ammonia oxidizing bacteria.
Disclosure of Invention
The invention can enrich anaerobic ferric salt to oxidize ammonia nitrogen and synchronously remove nitrogen and sewageMud, under anaerobic conditions, using Fe3+Oxidizing ammonia nitrogen in the wastewater and realizing the removal of total nitrogen. The invention relates to a method for culturing anaerobic ferric salt oxidized ammonia nitrogen and synchronous denitrified sludge, which comprises the following steps:
(1) experimental apparatus: an up-flow type sludge-film mixing reactor is adopted, the effective volume is 7L, and the reactor is in a sealed state to maintain an anaerobic environment. The upper part of the reactor is filled with a three-dimensional grid-shaped fiber filler made of polyvinylidene chloride, the stacking volume of the filler is 3L, meshes formed by the three-dimensional grid-shaped fiber filler are smaller than 0.1mm, and granular sludge with the particle size larger than 0.1mm can be effectively intercepted (in the process of backflow of mixed liquid, the granular sludge can be prevented from being extruded and crushed by a mixed liquid backflow pump, meanwhile, the filler has good microorganism adhesion capacity, the formation of anaerobic iron salt for oxidizing ammonia nitrogen and a synchronous denitrification biomembrane is facilitated, and the starting time of the reactor is shortened). The reactor adopts a periodic operation mode, and each periodic operation program comprises water inlet, reaction, precipitation and water drainage. In the water inlet stage, water is fed into the middle of the reactor through a peristaltic pump, the water inlet volume is 3.5L each time, and the water inlet time is 20 min; in the reaction stage, a sludge reflux pump is started to reflux the muddy water mixed liquor on the upper part of the reactor to the bottom of the reactor, so that the contact between the substrate and the microorganism is promoted, and the mass transfer effect is enhanced. Through daily sample measurement and analysis, when the ammonia nitrogen concentration in the reactor is reduced to 0-5mg/L, the reaction stage is ended; in the precipitation stage, a return sludge pump is closed, and the precipitation time is 30 min; and in the drainage stage, in order to avoid the loss of granular sludge along with effluent, drainage is carried out in the middle of the reactor through a peristaltic pump, the volume of drainage is 3.5L each time, and the drainage time is 20 min. Through the periodic operation mode, the anaerobic iron salt can be ensured to oxidize ammonia nitrogen and the synchronous denitrification sludge can be ensured to fully react with the substrate, the change trend of the ammonia nitrogen concentration can be conveniently analyzed, and the loss of the sludge can be avoided.
(2) Sludge inoculation: 2L of anaerobic ammonia oxidation granular sludge is inoculated at the bottom of the reactor, the sludge concentration is 8000mg/L, the sludge particle size is 1.0-2.0mm, and the volume of the inoculated sludge accounts for 28.5% of the effective volume of the reactor. The anaerobic ammonia oxidation sludge can quickly show the ammonia nitrogen oxidation performance of anaerobic iron salt, and the starting time of the reactor is shortened; the anaerobic ammonia oxidation granular sludge with the grain size has better sedimentation performance and better resistance to adverse environment.
(3) Water inlet of the reactor:
the water inlet of the reactor is manually distributed.
In the 1 st operation period, the water inlet component concentration of the reactor is as follows: NH (NH)4 +-N(NH4Cl)，50-60mg/L；FeCl3·6H2O，1450mg/L；KH2PO4，30mg/L；CaCl2，90mg/L；MgSO4·7H2O, 140 mg/L; trace elements 1 mL/L. The concentration of the trace element component is Na2-EDTA，50g/L；FeSO4·7H2O，5g/L；CoSO4·5H2O，1.9g/L；MnCl2·4H2O，5.1g/L；CuSO4·5H2O，1.6g/L；ZnSO4·7H2O，5g/L；NaMoO4·2H2O, 1.1 g/L. The pH was first adjusted to 7.0 with NaOH solution (5mol/L) and NaHCO was added3NaHCO in the feed water3The concentration was 1200 mg/L. By NaOH and NaHCO3The pH value can be maintained to be proper, the pH value buffering capacity is good, and the inorganic carbon source required by the growth of the microorganism can be provided.
Since the water discharge ratio of the reactor is 50%, in order to ensure that the concentrations of the components in the reactor are consistent at the initial moment of each period, the concentrations of the components of the feed water to the reactor are set to be 2 times of the concentrations of the components of the feed water in the 1 st period from the 2 nd period.
(4) The temperature in the reactor is controlled to be 25-30 ℃, the pH is controlled to be 7.0-9.0, the anaerobic environment is maintained in the reactor, and the reflux quantity of the mixed liquid reflux sludge of the reflux sludge pump is 120 mL/min. In the temperature range, the microorganism has better activity; in the pH range, the sludge has better capability of oxidizing ammonia nitrogen by anaerobic ferric salt; the mixed liquor reflux pump is arranged to reflux the mixed liquor at the upper part of the reactor to the bottom of the reactor, so that the contact between the substrate and the microorganism can be promoted, and the mass transfer effect is enhanced.
(5) FeCl was added to the reactor daily during a single run cycle3·6H2O and NaHCO350mL of the concentrated solution of (1), FeCl in the concentrated solution3·6H2O and NaHCO3The concentrations are respectively 203g/L and 168g/L, and the purpose is to provide a substrate Fe for anaerobic ferric salt to oxidize ammonia nitrogen and synchronous denitrification sludge3+And maintain a higher pH.
The invention can culture anaerobic iron salt oxidized ammonia nitrogen and synchronous denitrification sludge, greatly shorten the culture time of the sludge, realize the high-efficiency removal of ammonia nitrogen and total nitrogen, and improve the operation stability of the anaerobic iron salt oxidized ammonia nitrogen and synchronous denitrification reactor.
Drawings
FIG. 1 is a diagram of a reactor apparatus.
In FIG. 1, 1-bioreactor; 2-a water inlet tank; 3-a water inlet pump; 4, discharging a water pump; 5-water outlet tank; 6-mixed liquid reflux pump; 7-water bath; 8-heating rod
FIG. 2 is a diagram of a batch experimental apparatus.
FIG. 3 shows the results of a batch experiment.
FIG. 4 is a graph showing the change in nitrogen concentration in the reactor.
Figure 5 is the ammonia nitrogen and total nitrogen removal from the reactor.
Detailed Description
1. The reactor set-up is shown in FIG. 1.
2. Example the influent water used was manually distributed. In the 1 st operation period, the water inlet component concentration of the reactor is as follows: NH (NH)4 +-N(NH4Cl)，50-60mg/L；FeCl3·6H2O，1450mg/L；KH2PO4，30mg/L；CaCl2，90mg/L；MgSO4·7H2O, 140 mg/L; trace elements 1 mL/L. The concentration of the trace element component is Na2-EDTA，50g/L；FeSO4·7H2O，5g/L；CoSO4·5H2O，1.9g/L；MnCl2·4H2O，5.1g/L；CuSO4·5H2O，1.6g/L；ZnSO4·7H2O，5g/L；NaMoO4·2H2O, 1.1 g/L. The pH was first adjusted to 7.0 with NaOH solution (5mol/L) and NaHCO was added3NaHCO in the feed water3The concentration was 1200 mg/L.
Since the water discharge ratio of the reactor is 50%, in order to ensure that the concentrations of the components in the reactor are consistent at the initial moment of each period, the concentrations of the components of the feed water to the reactor are set to be 2 times of the concentrations of the components of the feed water in the 1 st period from the 2 nd period.
3. The method comprises the following operation steps:
(1) sludge inoculation: 2L of anaerobic ammonia oxidation granular sludge is inoculated at the bottom of the reactor, the sludge concentration is 8000mg/L, the sludge particle size is 1.0-2.0mm, and the volume of the inoculated sludge accounts for 28.5% of the effective volume of the reactor.
(2) Batch experiments:
the influence of pH on the ammonia nitrogen oxidation and synchronous denitrification performance of the anaerobic ferric salt of the inoculated sludge and the domesticated sludge is researched, and the proper pH value is determined. The initial pH was set at 9.0, 8.0, 7.0, 5.0 and 3.0, respectively.
1) Batch type experimental device:
batch experiments were performed using 500mL serum vials, as shown in figure 2. In FIG. 2, 1-magnetic stirrer; 2-serum bottle; 3-temperature probe; 4-a rotor; 5-water sealing; 6-sampling port or nitrogen interface.
2) Batch type experimental sludge
And (3) respectively taking inoculated sludge and anaerobic ferric salt to oxidize ammonia nitrogen and domesticated sludge cultured by a synchronous denitrification reactor, and carrying out batch experiments.
3) Water for experiment: the water for batch experiment is used for manual water distribution, and the component concentration is as follows: NH (NH)4 +-N(NH4Cl)，70-80mg/L；FeCl3·6H2O，1450mg/L；KH2PO4，30mg/L；CaCl2，90mg/L；MgSO4·7H2O, 140 mg/L; trace elements 1 mL/L. The concentrations of the trace element components were the same as described above for the reactor feed water. The initial pH was adjusted with NaOH solution (5 mol/L).
3) The method for measuring the ammoxidation activity of the anaerobic iron comprises the following steps: a. preparing mud-water mixed liquid; b. starting a constant-temperature magnetic stirrer, covering the bottle stopper tightly at the rotating speed of 200r/min, and introducing nitrogen for 30min (the nitrogen purity is 99.999%); c. stopping introducing nitrogen, placing the serum bottle together with a magnetic stirrer into a 30 ℃ constant temperature incubator, and sampling after 8 days to determine the change of the concentration of the main nitrogen component.
Determination of sludge concentration: weighing 25g of granular wet sludge by using an analytical balance, and putting the sludge and simulated water into a serum bottle with an effective volume of 500 mL; meanwhile, 5g of wet sludge is wrapped by filter paper, and processed by an oven and a muffle furnace, and MLSS and MLVSS in a serum bottle are calculated.
4) The experimental results are as follows:
the batch test results are shown in FIG. 3. When the initial pH value is 9.0, 8.0 and 7.0, the removal efficiency of the anaerobic iron salt oxidized ammonia nitrogen of the inoculated sludge is 53.62%, 26.43% and 28.40% respectively; when the initial pH value is 5.0 and 3.0, the ammonia nitrogen oxidation capability of anaerobic iron salt of inoculated sludge is completely inhibited. When the initial pH value is 9.0, 8.0 and 7.0, the removal efficiency of the anaerobic iron salt oxidized ammonia nitrogen of the domesticated sludge is 88.41%, 67.07% and 33.06% respectively; when the initial pH value is 5.0 and 3.0, the ammonia nitrogen oxidation capability of the anaerobic iron salt of the domesticated sludge is completely inhibited. The results show that the optimal pH value of the inoculated sludge and the domesticated sludge is 9.0, and the proper pH value for the reaction of oxidizing ammonia nitrogen by anaerobic iron salt is 7.0-9.0.
(2) And (3) a sludge culture stage of the reactor:
the nitrogen concentration in the reactor varied as shown in figure 4. The ammonia nitrogen and total nitrogen removal from the reactor is shown in figure 5.
An up-flow type sludge-film mixing reactor is adopted, the effective volume is 7L, and the anaerobic environment is maintained in the reactor. The upper part of the reactor is filled with a three-dimensional grid-shaped fiber filler made of polyvinylidene chloride, the packing accumulation volume is 3L, meshes formed by the three-dimensional grid-shaped fiber filler are smaller than 0.1mm, and granular sludge with the particle size larger than 0.1mm can be effectively intercepted. And the sludge-water mixed liquor at the upper part of the reactor is refluxed to the bottom of the reactor through the sludge reflux pump, so that the contact between the substrate and the microorganism is promoted, and the mass transfer effect is enhanced. The temperature in the reactor is controlled to be 25-30 ℃, the pH is controlled to be 7.0-9.0, the anaerobic environment is maintained in the reactor, and the reflux quantity of the mixed liquid reflux sludge of the reflux sludge pump is 120 mL/min. FeCl was added to the reactor daily3·6H2O and NaHCO350mL of the concentrated solution of (1), FeCl in the concentrated solution3·6H2O and NaHCO3The concentrations were 203g/L and 168g/L, respectively. In the 1 st period, the ammonia nitrogen concentration in the reactor is gradually reduced; by the 9 th day, the concentration of the ammonia nitrogen and the total nitrogen in the effluent of the reactor are respectively reduced to 4.0mg/L and 5.9mg/L, and the removal rate of the ammonia nitrogen and the total nitrogen in the reactor respectively reaches 92.3 percent and 89.1 percent. In the 3 rd period, the oxidizing property of anaerobic ferric ammonia nitrogen in the sludge in the reactor is obviously enhanced; after 5 days, the concentration of the ammonia nitrogen and the total nitrogen in the effluent of the reactor are respectively reduced to 0.5mg/L and 3.6mg/L, and the removal rate of the ammonia nitrogen and the total nitrogen in the reactor respectively reaches 99.1 percent and 93.9 percent; compared with the 1 st period, the time required for reducing the ammonia nitrogen concentration to 0-5mg/L is shortened by 1 time.
3) And (3) continuous operation: in the 4 th to 6 th periods, the anaerobic ferric ammonia nitrogen oxidation performance of the sludge in the reactor is kept stable; when the period is over, the average values of the concentrations of the ammonia nitrogen and the total nitrogen in the effluent of the reactor are 1.3mg/L and 4.8mg/L, and the removal rates of the ammonia nitrogen and the total nitrogen in the reactor respectively reach 97.4 percent and 91.3 percent; the time required for reducing the ammonia nitrogen concentration to 0-5mg/L is shortened to 4 days.
4) Other variations and modifications may be made on the above principles. Such variations and modifications are intended to be within the scope of the present invention.
Claims (3)
1. A rapid culture method for anaerobic ferric salt oxidized ammonia nitrogen and synchronous denitrification sludge is characterized by comprising the following steps:
1) an upflow sludge-membrane mixing reactor is adopted, which is hereinafter referred to as a reactor; the effective volume is 7L; the upper part of the reactor is filled with a three-dimensional latticed fiber filler made of polyvinylidene chloride, and the packing accumulation volume is 3L;
2) sludge inoculation: 2L of anaerobic ammonia oxidation granular sludge is inoculated at the bottom of the reactor, the sludge concentration is 8000mg/L, the sludge particle size is 1.0-2.0mm, and the volume of the inoculated sludge accounts for 28.5% of the effective volume of the reactor;
3) the water inlet is manually distributed; NH in artificial water preparation4 +-N(NH4Cl) concentration of 50-60mg/L, FeCl3·6H2The concentration of O is 1450mg/L, the pH is firstly adjusted to 7.0 by NaOH solution, and NaHCO is added3Into the waterNaHCO3The concentration is 1200 mg/L;
4) controlling the temperature in the reactor to be 25-30 ℃, controlling the pH to be 7.0-9.0, maintaining an anaerobic environment, refluxing the mixed liquor at the upper part of the reactor to the bottom of the reactor by a reflux sludge pump, wherein the reflux quantity of the reflux sludge pump is 120 mL/min;
5) the reactor adopts a periodic operation mode, and each periodic operation program comprises water inlet, reaction, precipitation and water drainage; the water inlet volume and the water discharge volume in each period are both 3.5L, and the water discharge ratio is 50 percent; in the reaction stage, a sludge reflux pump is started to reflux the muddy water mixed liquor on the upper part of the reactor to the bottom of the reactor;
6) FeCl was added to the reactor daily during a single run cycle3·6H2O and NaHCO350mL of the concentrated solution of (1), FeCl in the concentrated solution3·6H2O and NaHCO3The concentrations were 203g/L and 168g/L, respectively.
2. The method for rapidly culturing anaerobic ferric salt oxidized ammonia nitrogen and synchronous denitrification sludge according to claim 1, which is characterized in that: the mesh formed by the three-dimensional latticed fiber filler is less than 0.1 mm.
3. The method for rapidly culturing anaerobic ferric salt oxidized ammonia nitrogen and synchronous denitrification sludge according to claim 1, which is characterized in that: the water inlet is manually distributed; the component concentration is as follows: NH (NH)4 +-N(NH4Cl)，50-60mg/L；FeCl3·6H2O，1450mg/L；KH2PO4，30mg/L；CaCl2，90mg/L；MgSO4·7H2O, 140 mg/L; 1mL/L of trace elements; the concentration of the trace element component is Na2-EDTA,50g/L；FeSO4·7H2O,5g/L；CoSO4·5H2O,1.9g/L；MnCl2·4H2O,5.1g/L；CuSO4·5H2O,1.6g/L；ZnSO4·7H2O,5g/L；NaMoO4·2H2O,1.1g/L。
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