CN114671577A - Denitrification purification method for mariculture wastewater - Google Patents
Denitrification purification method for mariculture wastewater Download PDFInfo
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Abstract
The invention relates to the field of mariculture, and discloses a method for denitrifying and purifying mariculture wastewater, which comprises the following steps: step 1, after the mariculture wastewater is subjected to standing treatment, discarding sludge and collecting supernatant liquor to obtain first wastewater treatment liquor; step 2, filtering the first wastewater treatment liquid through a first filter screen, and collecting the filtered liquid to obtain a second wastewater treatment liquid; step 3, treating the second wastewater treatment liquid by a bioreactor provided with a denitrification biological layer, and collecting the treated liquid to obtain purified seawater; wherein, the denitrification biological layer comprises two layers of second filter screens and a biological film filler filled between the two layers of second filter screens. Compared with common physical purification or biological purification, the purification method combines the advantages of the two, is improved on the basis of the existing biological purification, greatly shortens the time of the biological purification process and improves the purification effect of the biological purification.
Description
Technical Field
The invention relates to the field of mariculture, in particular to a method for denitrifying and purifying mariculture wastewater.
Background
With the rapid development of the marine aquaculture industry in China, the wastewater discharge amount of coastal nursery and cultivation farms is increased day by day, and the environment of offshore waters is seriously deteriorated, so that the ecological system of the offshore area is unbalanced, red tide is frequent, and diseases are bred. The mariculture wastewater may include granular solid waste derived from excrement and feed, dissolved metabolic waste, dissolved nutritive salt, antimicrobial agents, drug residues, etc., and thus, when discharged in large quantities, may cause eutrophication or deterioration in water quality of the aquaculture water and adjacent waters.
Compared with industrial wastewater and domestic sewage, the mariculture wastewater has two obvious characteristics, namely low content of potential pollutants and large water quantity, and increases the treatment difficulty of the mariculture wastewater due to the salinity effect of seawater and the particularity of a polluted structure of the mariculture wastewater. The organic matters in the mariculture wastewater mainly comprise carbohydrates, proteins, fats and the like, have good biodegradability, are particularly suitable for adopting a biomembrane method treatment technology, and have good treatment effect on ammonia nitrogen substances in the mariculture wastewater. The carriers of the biological membrane are different, the growth amount of microorganisms attached to the carriers is different, and the treatment effect on the aquaculture wastewater is also different. The biofilm filler in the biofilm method is the core determining the purification effect, most of the commercially available biofilm fillers adopt a single high-molecular polymer material, such as polyethylene or polypropylene, and although a certain amount of microorganisms can be loaded on the high-molecular polymer material, the high-molecular polymer material belongs to a hydrophobic material, has the defects of poor biocompatibility, incapability of being recycled for many times, long operation time and the like, and cannot be widely applied to treatment of aquaculture sewage.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a denitrification purification method for mariculture wastewater, which has good biocompatibility, can be recycled for multiple times and has short running time.
The purpose of the invention is realized by adopting the following technical scheme:
a denitrification purification method for mariculture wastewater comprises the following steps:
step 1, after the mariculture wastewater is subjected to standing treatment, discarding sludge and collecting supernatant liquor to obtain first wastewater treatment liquor;
step 2, filtering the first wastewater treatment liquid through a first filter screen, and collecting the filtered liquid to obtain a second wastewater treatment liquid;
step 3, treating the second wastewater treatment liquid by a bioreactor provided with a denitrification biological layer, and collecting the treated liquid to obtain purified seawater;
the denitrification biological layer comprises two layers of second filter screens and a biological film filler filled between the two layers of second filter screens.
Preferably, the first filter screen is made of a ceramic material, and the pore size is 500-800 μm.
Preferably, the second filter screen is made of a ceramic material, and the pore size is 300-500 μm.
Preferably, the biofilm filler is a denitrification carrier loaded with aerobic denitrification microorganisms.
Preferably, the aerobic denitrifying microorganisms consist of marine pseudomonas and hydrocarbon-removing marinobacter in a mass ratio of 1-2: 1.
Preferably, the preparation method of the biofilm filler comprises the following steps:
x1. an aerobic denitrification microorganism liquid culture medium is prepared according to the following mixture ratio: 10g of glucose, 35g of sodium chloride, 0.6g of sodium acetate, 0.2g of potassium nitrate, 0.01g of monopotassium phosphate, 0.02g of magnesium chloride, 0.1g of calcium chloride and 1L of water; then, adjusting the pH value of the culture medium to 7-7.5, sterilizing at 121 ℃ for 10-20 min, and cooling to room temperature to obtain a liquid culture medium of the denitrifying bacteria;
x2. adding aerobic denitrifying microorganisms into the liquid culture medium of denitrifying bacteria, and placing in an automatic shaking table at 25-35 deg.C and 100-200 rpm for aerobic culture for 15-25 h until the number of viable bacteria is not less than 2 × 109After CFU/mL, obtaining an aerobic denitrification microbial agent;
x3. adding the denitrification carrier into the aerobic denitrification microbial agent, soaking for 120-150 h under the condition of normal temperature aeration, then removing the aeration and cooling to 4 ℃, taking out the denitrification carrier, and freeze-drying until the water content is lower than 20% to obtain the biomembrane filler; wherein the mass ratio of the denitrification carrier to the aerobic denitrification microbial agent is 1: 8-12.
Preferably, in the operation process of the bioreactor, the mass ratio of the second wastewater treatment liquid to the biofilm filler is 20-30: 1.
Preferably, the particle size of the denitrification carrier is 5-10 mm.
Preferably, in step 3, during the operation of the bioreactor, the set conditions of the denitrification biological layer are as follows: the dissolved oxygen amount is 5-6 mg/L, the pH is 7-7.5, and the temperature is 25-35 ℃.
Preferably, in the step 3, the second wastewater treatment liquid stays in the bioreactor for 1-3 hours.
Preferably, the preparation method of the denitrification carrier comprises the following steps:
s1, weighing imogolite powder, mixing the imogolite powder with deionized water, adding vinyl triethoxysilane, carrying out ultrasonic dispersion treatment, standing and soaking for 6-8 h, filtering and collecting solid, washing the solid with pure water for at least three times, and drying in an oven to obtain an imogolite powder activator; wherein the mass ratio of the imogolite powder, the vinyl triethoxysilane to the deionized water is 1: 0.1-0.3: 5-8;
s2, weighing caffeic acid, mixing the caffeic acid with a 90% polyethylene glycol-400 aqueous solution, fully stirring, adding sodium carbonate as a catalyst, fully stirring again, heating to 55-65 ℃, dropwise adding beta-phenethyl alcohol, reacting for 24-48 h under a heat preservation condition after the dropwise adding is finished, removing the solvent, and sequentially purifying and drying to obtain a caffeic acid esterified substance; wherein the mass ratio of the caffeic acid to the beta-phenethyl alcohol to the polyethylene glycol-400 aqueous solution is 1.8: 1.3-1.8: 10-15, and the mass ratio of the sodium carbonate to the caffeic acid is 0.04-0.08: 1;
s3, mixing the caffeic acid esterified substance into an ethanol solution with the mass fraction of 50-70%, adding an imogolite powder activator, uniformly mixing by ultrasonic waves, adding a hydrogen peroxide solution with the mass fraction of 20-30%, dropwise adding a peroxidase aqueous solution with the concentration of 1-3U/mL, stirring and reacting for 6-8 h at room temperature, dropwise adding a sodium hydroxide solution with the mass fraction of 10-20% until the pH = 10.0-11.0 of a reaction liquid, rapidly filtering and collecting a solid, washing the solid to be neutral by using pure water, washing the solid by using acetone for three times, and drying under reduced pressure to obtain the imogolite modified by the poly-caffeic acid, namely a denitrification carrier; wherein the mass ratio of the caffeic acid ester compound, the imogolite powder activator and the ethanol solution is 1: 3-6: 10-20, and the mass ratio of the hydrogen peroxide solution, the peroxidase aqueous solution and the caffeic acid ester compound is 1: 5-8: 80-100.
The invention has the beneficial effects that:
1. the invention provides a denitrification purification method for mariculture wastewater, which is simple and convenient to operate and high in purification efficiency, and can be used for removing impurities in the mariculture wastewater in batches and finally purifying to obtain seawater with less solid impurities and low ammonia nitrogen content. Compared with common physical purification or biological purification, the purification method combines the advantages of the two, is improved on the basis of the existing biological purification, greatly shortens the time of the biological purification process and improves the purification effect of the biological purification.
2. The treatment method of the invention has no toxicity or harm to the cultured aquatic organisms, simple process, obvious effect, no drug residue and no secondary pollution. The purification process used by the invention is simple, and the whole process comprises three steps: the method comprises the following steps of firstly removing heavier precipitated particulate matters and impurities in the mariculture wastewater by using a self-precipitation method, secondly removing lighter or suspended impurities in the mariculture wastewater by using a filter screen, and thirdly removing ammonia nitrogen compounds in the mariculture wastewater to finish purification.
3. The method uses a denitrification carrier loaded by aerobic denitrification microorganisms in the process of biological purification, wherein the denitrification carrier uses the self-made poly-caffeic acid modified imogolite material. The denitrification carrier of the invention abandons the conventional polymer material, uses the crystalline hydrated aluminosilicate mineral imogolite with fibrous shape as a matrix, and carries out chemical combination coating modification on the basis of the imogolite, wherein the coated material is obtained by polymerizing an ester compound formed by the reaction of caffeic acid and beta-phenylethyl alcohol. The denitrification carrier prepared by the invention has better adsorbability, not only can adsorb and fix a large amount of aerobic denitrification microorganisms, but also has certain adsorbability on ammonia nitrogen compounds in the wastewater, thereby achieving better purification effect.
4. Because the salinity of the seawater is higher, in order to obtain the microorganisms with stronger activity under the condition of high salinity, the culture medium with higher salinity content is selected in the process of culturing the denitrifying microorganisms, so that the denitrifying microorganisms which are more suitable for living under the condition of high salinity are screened out, and the purifying efficiency of the biofilm packing on the seawater wastewater is further enhanced.
Detailed Description
For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but are not to be construed as limiting the implementable scope of the present invention.
At present, an activated sludge method is adopted in the market for treating aquaculture water, the effect of removing nitrogen and phosphorus is good, but the method occupies a large area, secondary pollution can be caused if the produced sludge is not treated well, and the operation cost is high. Among the existing biological methods, the activated sludge method has ideal effect only under the condition of low salinity, and is not suitable for treating the mariculture wastewater.
The ammonia nitrogen is the excrement of aquatic organisms and is the end product of the decomposition of nitrogenous organic matters such as residual feed, excrement, animal and plant corpses and the like. Aerobic denitrification refers to a process that aerobic denitrifying bacteria convert nitrate nitrogen with higher concentration in an aerobic pool into nitrogen through periplasmic nitrate reductases (periplasmic nitrate reductases) under aerobic conditions, so that the removal of ammonia nitrogen depends on the activity of the denitrifying bacteria, and the activity of the denitrifying bacteria is related to a carrier biofilm material loaded by the denitrifying bacteria.
Conventional biological membrane materials, such as polyethylene or polypropylene, which are high molecular polymer materials capable of supporting a certain amount of microorganisms, are poor in biocompatibility and not enough in supported microorganism amount, so that the microorganisms are easy to fall off, and thus the problems of poor purification effect and poor multi-use effect are caused.
The invention abandons the conventional biological membrane material, the carrier used in the prepared denitrification biological layer is poly caffeic acid modified imogolite, the imogolite is a crystalline hydrated aluminosilicate mineral with fibrous shape, is one of few natural nano minerals in nature, has a single-wall tubular nano structure, and has a pipe outer framework formed by curled gibbsite, the inner side of the pipe is an orthosilicic acid group, and the unique structure and the surface functional group determine that the nano-porous structure has larger specific surface area and stronger hydrophilicity. However, imogolite has a low degree of structural order and does not perform as well as other silicate materials in adsorption and specific applications, and therefore, few studies have been made on the imogolite. However, the invention is based on the application of small single-wall tubular nano-structures, which are cross-linked and coated by using polymers to form larger particles.
The denitrification carrier prepared by the invention achieves better effect, and the preparation principle is as follows: the activated imogolite is cross-linked and coated by using a product obtained by reacting beta-phenylethyl alcohol with caffeic acid as a raw material. The invention uses sodium carbonate as a catalyst and polyethylene glycol-400 aqueous solution as a solvent to produce proper reaction conditions, facilitates the condensation of the caffeic acid and the beta-phenylethyl alcohol to form a caffeic acid ester product, then mixes the generated caffeic acid ester product with activated imogolite, utilizes the special structure of the caffeic acid to generate the poly-caffeic acid ester for crosslinking and coating on the surface of the imogolite under the action of hydrogen peroxide and peroxidase (preferably horseradish peroxidase), and then utilizes the principle that the imogolite is easy to agglomerate under the alkaline condition to agglomerate and precipitate the crosslinked and coated imogolite. In order to avoid depolymerization and reduction, filtering and washing are carried out quickly after coagulation and precipitation, and then the poly caffeic acid modified imogolite, namely the denitrification carrier, is obtained after drying treatment under reduced pressure. During the reduced pressure drying process, the solvent absorbed on the surface and inside the imogolite modified by the poly-caffeic acid can be rapidly evaporated to form a pore size which is beneficial to inhabitation and fixation of subsequent microorganisms.
Since caffeic acid, beta-phenethyl alcohol and imogolite are hydrophilic materials, the finally prepared poly-caffeic acid modified imogolite has stronger hydrophilicity, and detection of subsequent experiments shows that the denitrification carrier prepared by the method has better ammonia nitrogen purification performance, and probably the poly-caffeic acid ester modified imogolite has stronger adsorbability on ammonia nitrogen compounds in water, so that the decomposition of microorganisms on ammonia nitrogen is accelerated, and the efficiency of purifying the ammonia nitrogen is improved. In addition, the generated caffeic acid ester product contains abundant carbon elements and can be used as a carbon source required by microorganism consumption, so that the activity of the microorganism is further improved, and the purification efficiency of the microorganism on ammonia nitrogen is accelerated.
The invention is further described below with reference to the following examples.
Example 1
A denitrification purification method for mariculture wastewater comprises the following steps:
step 1, after the mariculture wastewater is subjected to standing treatment, discarding sludge and collecting supernatant liquor to obtain first wastewater treatment liquor;
step 2, filtering the first wastewater treatment liquid through a first filter screen, and collecting the filtered liquid to obtain a second wastewater treatment liquid;
step 3, treating the second wastewater treatment liquid by a bioreactor provided with a denitrification biological layer, and collecting the treated liquid to obtain purified seawater; in the operation process of the bioreactor, the set conditions of the denitrification biological layer are as follows: the dissolved oxygen amount is 5-6 mg/L, the pH is 7.0-7.5, and the temperature is 30 ℃; the mass ratio of the second wastewater treatment liquid to the biofilm filler is 25: 1; the second wastewater treatment liquid stays in the bioreactor for 2 hours;
the denitrification biological layer comprises two layers of second filter screens and a biological film filler filled between the two layers of second filter screens; the first filter screen is made of ceramic materials, and the pore size is 600 mu m; the second filter screen is made of ceramic materials, and the pore size is 400 mu m.
The biofilm filler is a denitrification carrier loaded with aerobic denitrification microorganisms, wherein the aerobic denitrification microorganisms consist of marine pseudomonas and hydrocarbon-removing marinobacter in a mass ratio of 1.5: 1.
The grain size of the denitrification carrier is 8 mm; the preparation method of the denitrification carrier comprises the following steps:
s1, weighing imogolite powder, mixing the imogolite powder with deionized water, adding vinyl triethoxysilane, carrying out ultrasonic dispersion treatment, standing and soaking for 7 hours, filtering and collecting solids, washing the solids for at least three times by using pure water, and carrying out drying treatment in an oven to obtain an imogolite powder activator; wherein the mass ratio of the imogolite powder, the vinyl triethoxysilane to the deionized water is 1:0.2: 6;
s2, weighing caffeic acid, mixing the caffeic acid with a 90% polyethylene glycol-400 aqueous solution, fully stirring, adding sodium carbonate as a catalyst, fully stirring again, heating to 60 ℃, dropwise adding beta-phenethyl alcohol, keeping the temperature for reaction for 36 hours after dropwise adding is finished, removing the solvent, and then sequentially purifying and drying to obtain a caffeic acid esterified substance; wherein the mass ratio of the caffeic acid, the beta-phenethyl alcohol and the polyethylene glycol-400 aqueous solution is 1.8:1.5:12, and the mass ratio of the sodium carbonate and the caffeic acid is 0.05: 1;
s3, mixing the caffeic acid ester compound into an ethanol solution with the mass fraction of 60%, adding an imogolite powder activator, uniformly mixing by ultrasonic waves, adding a 25% hydrogen peroxide aqueous solution, dropwise adding a peroxidase aqueous solution with the concentration of 2U/mL, stirring and reacting for 7 hours at room temperature, dropwise adding a 15% sodium hydroxide solution until the pH = 10.0-11.0 of a reaction liquid, quickly filtering and collecting a solid, washing the solid to be neutral by using pure water, washing the solid by using acetone for three times, and drying under reduced pressure to obtain the imogolite modified by the poly-caffeic acid, namely a denitrification carrier; wherein the mass ratio of the caffeic acid esterified substance, the imogolite powder activating substance and the ethanol solution is 1:5:12, and the mass ratio of the aqueous hydrogen peroxide solution, the aqueous peroxidase solution and the caffeic acid esterified substance is 1:6: 85.
The preparation method of the biomembrane filler comprises the following steps:
x1. an aerobic denitrification microorganism liquid culture medium is prepared according to the following mixture ratio: 10g of glucose, 35g of sodium chloride, 0.6g of sodium acetate, 0.2g of potassium nitrate, 0.01g of monopotassium phosphate, 0.02g of magnesium chloride, 0.1g of calcium chloride and 1L of water; then, adjusting the pH value of the culture medium to 7.0-7.5, sterilizing at 121 ℃ for 15min, and cooling to room temperature to obtain a liquid culture medium of the denitrifying bacteria;
x2. adding aerobic denitrifying microorganism into liquid culture medium of denitrifying bacteria, and culturing in an automatic shaking table at 30 deg.C and 150rpm for 20h until the number of viable bacteria is not less than 2 × 109After CFU/mL, obtaining the aerobic denitrifying microorganismA microbial inoculum;
x3, adding a denitrification carrier into an aerobic denitrification microbial agent, soaking for 135 hours under the condition of normal-temperature oxygen exposure, then removing the explosive oxygen, cooling to 4 ℃, taking out the denitrification carrier, and freeze-drying until the water content is lower than 20% to obtain a biofilm filler; wherein the mass ratio of the denitrification carrier to the aerobic denitrification microbial agent is 1: 10.
Example 2
A denitrification purification method for mariculture wastewater comprises the following steps:
step 1, after the mariculture wastewater is subjected to standing treatment, discarding sludge and collecting supernatant liquor to obtain first wastewater treatment liquor;
step 2, filtering the first wastewater treatment liquid through a first filter screen, and collecting the filtered liquid to obtain a second wastewater treatment liquid;
step 3, treating the second wastewater treatment liquid by a bioreactor provided with a denitrification biological layer, and collecting the treated liquid to obtain purified seawater; in the operation process of the bioreactor, the set conditions of the denitrification biological layer are as follows: the dissolved oxygen amount is 5-6 mg/L, the pH is 7.0-7.5, and the temperature is 25 ℃; the mass ratio of the second wastewater treatment liquid to the biofilm filler is 20: 1; the second wastewater treatment liquid stays in the bioreactor for 1 h;
the denitrification biological layer comprises two layers of second filter screens and a biological film filler filled between the two layers of second filter screens; the first filter screen is made of a ceramic material, and the pore size is 500 mu m; the second filter screen is made of ceramic materials, and the pore size is 300 mu m.
The biomembrane filler is a denitrification carrier loaded with aerobic denitrification microorganisms, wherein the aerobic denitrification microorganisms consist of marine pseudomonas and hydrocarbon removing marinobacter in a mass ratio of 1: 1.
The grain size of the denitrification carrier is 5 mm; the preparation method of the denitrification carrier comprises the following steps:
s1, weighing imogolite powder, mixing the imogolite powder with deionized water, adding vinyl triethoxysilane, carrying out ultrasonic dispersion treatment, standing and soaking for 6 hours, filtering and collecting solids, washing the solids for at least three times by using pure water, and carrying out drying treatment in an oven to obtain an imogolite powder activator; wherein the mass ratio of the imogolite powder, the vinyl triethoxysilane to the deionized water is 1:0.1: 5;
s2, weighing caffeic acid, mixing the caffeic acid with a 90% polyethylene glycol-400 aqueous solution, fully stirring, adding sodium carbonate as a catalyst, fully stirring again, heating to 55 ℃, dropwise adding beta-phenethyl alcohol, carrying out heat preservation reaction for 24 hours after dropwise adding is finished, removing the solvent, and sequentially carrying out purification and drying treatment to obtain a caffeic acid esterified substance; wherein the mass ratio of the caffeic acid, the beta-phenethyl alcohol and the polyethylene glycol-400 aqueous solution is 1.8:1.3:10, and the mass ratio of the sodium carbonate and the caffeic acid is 0.04: 1;
s3, mixing the caffeic acid esterified substance into an ethanol solution with the mass fraction of 50%, adding an imogolite powder activator, uniformly mixing by ultrasonic waves, adding a 20% hydrogen peroxide aqueous solution, dropwise adding a 1U/mL peroxidase aqueous solution, stirring and reacting for 6 hours at room temperature, dropwise adding a 10-20% sodium hydroxide solution until the pH = 10.0-11.0 of the reaction liquid, quickly filtering and collecting a solid, washing the solid to be neutral by using pure water, washing the solid by using acetone for three times, and drying under reduced pressure to obtain the imogolite modified by the poly-caffeic acid, namely a denitrification carrier; wherein the mass ratio of the caffeic acid esterified substance, the imogolite powder activating substance and the ethanol solution is 1:3:10, and the mass ratio of the aqueous hydrogen peroxide solution, the aqueous peroxidase solution and the caffeic acid esterified substance is 1:5: 80.
The preparation method of the biomembrane filler comprises the following steps:
x1. an aerobic denitrification microorganism liquid culture medium is prepared according to the following mixture ratio: 10g of glucose, 35g of sodium chloride, 0.6g of sodium acetate, 0.2g of potassium nitrate, 0.01g of monopotassium phosphate, 0.02g of magnesium chloride, 0.1g of calcium chloride and 1L of water; then, adjusting the pH value of the culture medium to 7-7.5, sterilizing at 121 ℃ for 10min, and cooling to room temperature to obtain a liquid culture medium of the denitrifying bacteria;
x2. adding aerobic denitrifying microorganism into liquid culture medium of denitrifying bacteria, and culturing in an automatic shaking table at 25 deg.C and 100rpm for 15h until the number of viable bacteria is not less than 2 × 109After CFU/mL, get aerobicA denitrifying microbial agent;
x3, adding the denitrification carrier into the aerobic denitrification microbial agent, soaking for 120h under the condition of normal-temperature oxygen exposure, then removing the explosive oxygen, cooling to 4 ℃, taking out the denitrification carrier, and freeze-drying until the water content is lower than 20% to obtain the biomembrane filler; wherein the mass ratio of the denitrification carrier to the aerobic denitrification microbial agent is 1: 12.
Example 3
A denitrification purification method for mariculture wastewater comprises the following steps:
step 1, after the mariculture wastewater is subjected to standing treatment, discarding sludge and collecting supernatant liquor to obtain first wastewater treatment liquor;
step 2, filtering the first wastewater treatment liquid through a first filter screen, and collecting the filtered liquid to obtain a second wastewater treatment liquid;
step 3, treating the second wastewater treatment liquid by a bioreactor provided with a denitrification biological layer, and collecting the treated liquid to obtain purified seawater; in the operation process of the bioreactor, the set conditions of the denitrification biological layer are as follows: the dissolved oxygen amount is 5-6 mg/L, the pH is 7.0-7.5, the temperature is 35 ℃, and the mass ratio of the second wastewater treatment liquid to the biofilm filler is 30: 1; the second wastewater treatment liquid stays in the bioreactor for 3 hours;
the denitrification biological layer comprises two layers of second filter screens and a biological film filler filled between the two layers of second filter screens; the first filter screen is made of ceramic materials, and the aperture size is 800 mu m; the second filter screen is made of ceramic materials, and the pore size is 500 mu m.
The biofilm filler is a denitrification carrier loaded with aerobic denitrification microorganisms, wherein the aerobic denitrification microorganisms consist of marine pseudomonas and hydrocarbon-removing bacillus marinus with the mass ratio of 2: 1.
The grain size of the denitrification carrier is 10 mm; the preparation method of the denitrification carrier comprises the following steps:
s1, weighing imogolite powder, mixing the imogolite powder with deionized water, adding vinyl triethoxysilane, carrying out ultrasonic dispersion treatment, standing and soaking for 8 hours, filtering and collecting solids, washing the solids for at least three times by using pure water, and carrying out drying treatment in an oven to obtain an imogolite powder activator; wherein the mass ratio of the imogolite powder, the vinyl triethoxysilane to the deionized water is 1:0.3: 8;
s2, weighing caffeic acid, mixing the caffeic acid with 90% of polyethylene glycol-400 aqueous solution, fully stirring, adding sodium carbonate serving as a catalyst, fully stirring again, heating to 65 ℃, dropwise adding beta-phenethyl alcohol, keeping the temperature for reaction for 48 hours after dropwise adding is finished, removing the solvent, and then sequentially purifying and drying to obtain a caffeic acid esterified substance; wherein the mass ratio of the caffeic acid, the beta-phenethyl alcohol and the polyethylene glycol-400 aqueous solution is 1.8:1.8:15, and the mass ratio of the sodium carbonate to the caffeic acid is 0.08: 1;
s3, mixing the caffeic acid esterified substance into an ethanol solution with the mass fraction of 70%, adding an imogolite powder activator, uniformly mixing by ultrasonic waves, adding a hydrogen peroxide water solution with the mass fraction of 30%, dropwise adding a peroxidase water solution with the concentration of 3U/mL, stirring and reacting for 8 hours at room temperature, dropwise adding a sodium hydroxide solution with the mass fraction of 20% till the pH = 10.0-11.0 of a reaction liquid, quickly filtering and collecting a solid, washing the solid to be neutral by using pure water, washing the solid by using acetone for three times, and drying under reduced pressure to obtain the imogolite modified by the poly-caffeic acid, namely a denitrification carrier; wherein the mass ratio of the caffeic acid esterified substance, the imogolite powder activating substance and the ethanol solution is 1:6:20, and the mass ratio of the aqueous hydrogen peroxide solution, the aqueous peroxidase solution and the caffeic acid esterified substance is 1:8: 100.
The preparation method of the biomembrane filler comprises the following steps:
x1. an aerobic denitrification microorganism liquid culture medium is prepared according to the following mixture ratio: 10g of glucose, 35g of sodium chloride, 0.6g of sodium acetate, 0.2g of potassium nitrate, 0.01g of monopotassium phosphate, 0.02g of magnesium chloride, 0.1g of calcium chloride and 1L of water; then, adjusting the pH value of the culture medium to 7-7.5, sterilizing at 121 ℃ for 20min, and cooling to room temperature to obtain a liquid culture medium of the denitrifying bacteria;
x2. adding aerobic denitrifying microorganism into liquid culture medium of denitrifying bacteria, and culturing in an automatic shaker at 35 deg.C and 200rpm for 25 hr until the number of viable bacteria is not less than 2 × 109After CFU/mLObtaining an aerobic denitrification microbial agent;
x3, adding a denitrification carrier into an aerobic denitrification microbial agent, soaking for 150 hours under the condition of normal-temperature oxygen exposure, then removing the explosive oxygen, cooling to 4 ℃, taking out the denitrification carrier, and freeze-drying until the water content is lower than 20% to obtain a biofilm filler; wherein the mass ratio of the denitrification carrier to the aerobic denitrification microbial agent is 1: 8.
Comparative example 1
A denitrification purification method for mariculture wastewater comprises the following steps:
step 1, after the mariculture wastewater is subjected to standing treatment, discarding sludge and collecting supernatant liquor to obtain first wastewater treatment liquor;
step 2, filtering the first wastewater treatment liquid through a first filter screen, and collecting the filtered liquid to obtain a second wastewater treatment liquid;
step 3, treating the second wastewater treatment liquid by a bioreactor provided with a denitrification biological layer, and collecting the treated liquid to obtain purified seawater; in the operation process of the bioreactor, the set conditions of the denitrification biological layer are as follows: the dissolved oxygen amount is 5-6 mg/L, the pH is 7.0-7.5, and the temperature is 30 ℃; the mass ratio of the second wastewater treatment liquid to the biofilm filler is 25: 1; the second wastewater treatment liquid stays in the bioreactor for 2 hours;
the denitrification biological layer comprises two layers of second filter screens and a biological film filler filled between the two layers of second filter screens; the first filter screen is made of ceramic materials, and the pore size is 600 mu m; the second filter screen is made of ceramic materials, and the pore size is 400 mu m.
The biomembrane filler is a denitrification carrier loaded with aerobic denitrification microorganisms, wherein the aerobic denitrification microorganisms consist of marine pseudomonas and hydrocarbon removing marine bacillus in a mass ratio of 1.5: 1; the denitrification carrier is a polypropylene biological membrane.
The preparation method of the biomembrane filler comprises the following steps:
x1. an aerobic denitrification microorganism liquid culture medium is prepared according to the following mixture ratio: 10g of glucose, 35g of sodium chloride, 0.6g of sodium acetate, 0.2g of potassium nitrate, 0.01g of monopotassium phosphate, 0.02g of magnesium chloride, 0.1g of calcium chloride and 1L of water; then, adjusting the pH value of the culture medium to 7.0-7.5, sterilizing at 121 ℃ for 15min, and cooling to room temperature to obtain a liquid culture medium of the denitrifying bacteria;
x2. adding aerobic denitrifying microorganism into liquid culture medium of denitrifying bacteria, and culturing in an automatic shaking table at 30 deg.C and 150rpm for 20h until the number of viable bacteria is not less than 2 × 109After CFU/mL, obtaining an aerobic denitrification microbial agent;
x3, adding a denitrification carrier into an aerobic denitrification microbial agent, soaking for 135 hours under the condition of normal-temperature oxygen exposure, then removing the explosive oxygen, cooling to 4 ℃, taking out the denitrification carrier, and freeze-drying until the water content is lower than 20% to obtain a biofilm filler; wherein the mass ratio of the denitrification carrier to the aerobic denitrification microbial agent is 1: 10.
Comparative example 2
A denitrification purification method for mariculture wastewater comprises the following steps:
step 1, after the mariculture wastewater is subjected to standing treatment, discarding sludge and collecting supernatant liquor to obtain first wastewater treatment liquor;
step 2, filtering the first wastewater treatment liquid through a first filter screen, and collecting the filtered liquid to obtain a second wastewater treatment liquid;
step 3, treating the second wastewater treatment liquid by a bioreactor provided with a denitrification biological layer, and collecting the treated liquid to obtain purified seawater; in the operation process of the bioreactor, the set conditions of the denitrification biological layer are as follows: the dissolved oxygen amount is 5-6 mg/L, the pH is 7.0-7.5, and the temperature is 30 ℃; the mass ratio of the second wastewater treatment liquid to the biofilm filler is 25: 1; the second wastewater treatment liquid stays in the bioreactor for 2 hours;
the denitrification biological layer comprises two layers of second filter screens and a biological film filler filled between the two layers of second filter screens; the first filter screen is made of ceramic materials, and the pore size is 600 mu m; the second filter screen is made of ceramic materials, and the pore size is 400 mu m.
The biomembrane filler is a denitrification carrier loaded with aerobic denitrification microorganisms, wherein the aerobic denitrification microorganisms consist of marine pseudomonas and hydrocarbon removing marinobacter in a mass ratio of 1.5: 1.
The grain size of the denitrification carrier is 8 mm; the preparation method of the denitrification carrier comprises the following steps:
s1, weighing imogolite powder, mixing the imogolite powder with deionized water, adding vinyl triethoxysilane, carrying out ultrasonic dispersion treatment, standing and soaking for 7 hours, filtering and collecting solids, washing the solids for at least three times by using pure water, and carrying out drying treatment in an oven to obtain an imogolite powder activator; wherein the mass ratio of the imogolite powder, the vinyl triethoxysilane to the deionized water is 1:0.2: 6;
s2, adding caffeic acid into an ethanol solution with the mass fraction of 60%, adding an imogolite powder activator, uniformly mixing by ultrasonic waves, adding a 25% hydrogen peroxide aqueous solution, dropwise adding a 2U/mL peroxidase aqueous solution, stirring and reacting for 7 hours at room temperature, dropwise adding a 15% sodium hydroxide solution until the pH = 10.0-11.0 of a reaction solution, quickly filtering and collecting a solid, washing the solid to be neutral by using pure water, washing the solid by using acetone for three times, and drying under reduced pressure to obtain the imogolite modified by the caffeic acid, namely a denitrification carrier; wherein the mass ratio of the caffeic acid, the imogolite powder activator and the ethanol solution is 1:5:12, and the mass ratio of the aqueous hydrogen peroxide solution, the aqueous peroxidase solution and the caffeic acid is 1:6: 85.
The preparation method of the biomembrane filler comprises the following steps:
x1. an aerobic denitrification microorganism liquid culture medium is prepared according to the following mixture ratio: 10g of glucose, 35g of sodium chloride, 0.6g of sodium acetate, 0.2g of potassium nitrate, 0.01g of monopotassium phosphate, 0.02g of magnesium chloride, 0.1g of calcium chloride and 1L of water; then, adjusting the pH value of the culture medium to 7-7.5, sterilizing at 121 ℃ for 15min, and cooling to room temperature to obtain a liquid culture medium of the denitrifying bacteria;
x2. adding aerobic denitrifying microorganism into liquid culture medium of denitrifying bacteria, and culturing in an automatic shaking table at 30 deg.C and 150rpm for 20h until the number of viable bacteria is not less than 2 × 109After CFU/mL, obtaining an aerobic denitrification microbial agent;
x3, adding a denitrification carrier into an aerobic denitrification microbial agent, soaking for 135 hours under the condition of normal-temperature oxygen exposure, then removing the explosive oxygen, cooling to 4 ℃, taking out the denitrification carrier, and freeze-drying until the water content is lower than 20% to obtain a biofilm filler; wherein the mass ratio of the denitrification carrier to the aerobic denitrification microbial agent is 1: 10.
In order to more clearly illustrate the present invention, the following experiments were also performed:
taking the wastewater after mariculture at a certain position, detecting the ammonia nitrogen content and the total nitrogen content in the wastewater before purification treatment, and obtaining the following results after detection: the ammonia nitrogen content of the original wastewater is 132.5mg/L, the total nitrogen content is 187.4mg/L, then denitrification purification is respectively carried out by using the purification methods in the embodiments 1-3 and the comparative example, detection is divided into one-time purification treatment and continuous purification treatment, the one-time purification treatment is to detect and purify the ammonia nitrogen content and the total nitrogen content of water after the wastewater is subjected to one-time purification treatment, and the continuous purification treatment is to detect and purify the ammonia nitrogen content and the total nitrogen content of water after the same batch of wastewater is continuously purified for 720 hours by using the purification method.
The results are shown in table 1:
TABLE 1 comparison of the different denitrification purification methods for treating wastewater
As can be seen from Table 1, examples 1 to 3 of the present invention all had a good purification effect, and could maintain a good purification rate after 720 hours of continuous purification, and the reason for the decrease in the purification rate of continuous purification may be that after a long period of continuous purification, the carbon source in the denitrification carrier is gradually consumed, resulting in a decrease in the activity of the denitrification microorganisms. Although the purification methods of examples 1 to 3 are different, the most difference is the residence time, and although the purification effect of example 3 is not much different from that of example 1, the residence time is longer than that of example 1, and the purification effect of example 2 is not as good as that of examples 1 and 3, possibly because the residence time is too short. With respect to comparative examples 1 and 2, comparative example 1 employs a conventional polypropylene material as a biofilm, and the primary purification effect and continuous purification effect thereof are much lower than those of examples 1 to 3, while comparative example 2 is different from example 1 only in that a denitrification carrier material is prepared, and is inferior to example 1 in both primary purification effect and continuous purification effect.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A denitrification purification method for mariculture wastewater is characterized by comprising the following steps:
step 1, after the mariculture wastewater is subjected to standing treatment, discarding sludge and collecting supernatant liquor to obtain first wastewater treatment liquor;
step 2, filtering the first wastewater treatment liquid through a first filter screen, and collecting the filtered liquid to obtain a second wastewater treatment liquid;
step 3, treating the second wastewater treatment liquid by a bioreactor provided with a denitrification biological layer, and collecting the treated liquid to obtain purified seawater;
wherein, the denitrification biological layer comprises two layers of second filter screens and a biological film filler filled between the two layers of second filter screens.
2. The denitrification purification method for the mariculture wastewater as claimed in claim 1, wherein the first filter screen is made of a ceramic material, and the pore size is 500-800 μm; the second filter screen is made of a ceramic material, and the aperture size is 300-500 mu m.
3. The method for denitrifying and purifying mariculture wastewater according to claim 1, wherein the biofilm carrier is a denitrification carrier loaded with aerobic denitrification microorganisms.
4. The method for denitrifying and purifying mariculture wastewater according to claim 1, wherein the aerobic denitrifying microorganisms consist of marine pseudomonas and hydrocarbon-removing marinobacter in a mass ratio of 1-2: 1.
5. The method for denitrifying and purifying mariculture wastewater according to claim 1, wherein the preparation method of the biofilm carrier is as follows:
x1. an aerobic denitrification microorganism liquid culture medium is prepared according to the following mixture ratio: 10g of glucose, 35g of sodium chloride, 0.6g of sodium acetate, 0.2g of potassium nitrate, 0.01g of monopotassium phosphate, 0.02g of magnesium chloride, 0.1g of calcium chloride and 1L of water; then, adjusting the pH value of the culture medium to 7-7.5, sterilizing at 121 ℃ for 10-20 min, and cooling to room temperature to obtain a liquid culture medium of the denitrifying bacteria;
x2. adding aerobic denitrifying microorganisms into the liquid culture medium of denitrifying bacteria, and placing in an automatic shaking table at 25-35 deg.C and 100-200 rpm for aerobic culture for 15-25 h until the number of viable bacteria is not less than 2 × 109After CFU/mL, obtaining an aerobic denitrification microbial agent;
x3, adding a denitrification carrier into an aerobic denitrification microbial agent, soaking for 120-150 h under the condition of normal-temperature oxygen exposure, then removing the explosive oxygen, cooling to 4 ℃, taking out the denitrification carrier, and freeze-drying until the water content is lower than 20% to obtain a biofilm filler; wherein the mass ratio of the denitrification carrier to the aerobic denitrification microbial agent is 1: 8-12.
6. The method for denitrifying and purifying the mariculture wastewater according to claim 1, wherein the mass ratio of the second wastewater treatment solution to the biofilm filler is 20-30: 1 during the operation of the bioreactor.
7. The method for denitrifying and purifying mariculture wastewater according to claim 3, wherein the particle size of the denitrification carrier is 5-10 mm.
8. The method for denitrifying and purifying seawater wastewater of claim 1, wherein in the step 3, the conditions of the denitrification biological layer during the operation of the bioreactor are as follows: the dissolved oxygen amount is 5-6 mg/L, the pH is 7-7.5, and the temperature is 25-35 ℃.
9. The method for denitrifying and purifying mariculture wastewater according to claim 1, wherein in the step 3, the second wastewater treatment solution stays in the bioreactor for 1-3 hours.
10. The method for denitrifying and purifying mariculture wastewater according to claim 3, wherein the method for preparing the denitrification carrier comprises the following steps:
s1, weighing imogolite powder, mixing the imogolite powder with deionized water, adding vinyl triethoxysilane, carrying out ultrasonic dispersion treatment, standing and soaking for 6-8 h, filtering and collecting solid, washing the solid with pure water for at least three times, and drying in an oven to obtain an imogolite powder activator; wherein the mass ratio of the imogolite powder, the vinyl triethoxysilane to the deionized water is 1: 0.1-0.3: 5-8;
s2, weighing caffeic acid, mixing the caffeic acid with a 90% polyethylene glycol-400 aqueous solution, fully stirring, adding sodium carbonate as a catalyst, fully stirring again, heating to 55-65 ℃, dropwise adding beta-phenethyl alcohol, reacting for 24-48 h under a heat preservation condition after the dropwise adding is finished, removing the solvent, and sequentially purifying and drying to obtain a caffeic acid esterified substance; wherein the mass ratio of the caffeic acid to the beta-phenethyl alcohol to the polyethylene glycol-400 aqueous solution is 1.8: 1.3-1.8: 10-15, and the mass ratio of the sodium carbonate to the caffeic acid is 0.04-0.08: 1;
s3, mixing the caffeic acid esterified substance into an ethanol solution with the mass fraction of 50-70%, adding an imogolite powder activator, uniformly mixing by ultrasonic waves, adding a hydrogen peroxide solution with the mass fraction of 20-30%, dropwise adding a peroxidase aqueous solution with the concentration of 1-3U/mL, stirring and reacting for 6-8 h at room temperature, dropwise adding a sodium hydroxide solution with the mass fraction of 10-20% until the pH = 10.0-11.0 of a reaction liquid, rapidly filtering and collecting a solid, washing the solid to be neutral by using pure water, washing the solid by using acetone for three times, and drying under reduced pressure to obtain the imogolite modified by the poly-caffeic acid, namely a denitrification carrier; wherein the mass ratio of the caffeic acid ester compound, the imogolite powder activator and the ethanol solution is 1: 3-6: 10-20, and the mass ratio of the hydrogen peroxide solution, the peroxidase aqueous solution and the caffeic acid ester compound is 1: 5-8: 80-100.
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