CN112456638A - Modified steel slag filler and preparation method and application thereof - Google Patents
Modified steel slag filler and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a modified steel slag filler and a preparation method and application thereof. The modified steel slag filler can release iron ions, precipitate to remove phosphorus in wastewater, and S-LDHs can adsorb nitrate in gathered water and promote the generation of carbon source and sulfur source coupling denitrification, so that the modified steel slag filler also has higher synchronous nitrogen and phosphorus removal effects on slightly polluted water. The steel slag is used as a waste, is low in price and easy to obtain as a raw material, and is combined with the hydrotalcite and then roasted to obtain the filler, so that the specific surface area of the obtained filler is large, and microorganisms are easy to attach. The filler of the invention is applied to the biological treatment of wastewater, and can achieve the purpose of treating the waste with the waste.
Description
Technical Field
The invention belongs to the technical field of biological sewage treatment, relates to a modified steel slag filler and a preparation method and application thereof, and particularly relates to a modified steel slag filler with adsorption, nitrogen and phosphorus removal functions and a preparation method and application thereof.
Background
In recent years, countries have increasingly raised standards for total nitrogen emissions, and among them, biological methods are the most commonly used denitrification methods due to their low cost and non-toxic and harmless complete denitrification products.
The biofilter has the advantages of small occupied area, high denitrification efficiency, superior adsorption and filtration performance and the like, and has become a hotspot for research and application in the field of biological sewage treatment, and how to further improve the sewage treatment efficiency of the biofilter has become an important problem in the sewage treatment industry. In order to enhance the sewage treatment effect of the biological filter, the core factor is the selection of the filler. In recent years, modified biological fillers are increasingly researched, and the modified biological fillers not only provide a place for microbial biofilm formation, but also provide an electron donor for microbial denitrification. The Chinese patent application No. CN201911396207.4 discloses a carbon source-sulfur composite material for autotrophic denitrification nitrogen removal, a preparation method and application thereof, the patent adopts sulfur, coarse aggregate, a filling material, a sulfur modifier and a toughening agent to prepare a denitrification filling material, and the composite material has the advantages of high strength, resistance to long-term soaking in dirty water and the like, but the filling material is single autotrophic denitrification, the hydraulic retention time is long, and the treatment effect on slightly polluted water bodies is poor. Chinese patent CN201811113486.4 discloses a nitrogen and phosphorus removal active biological carrier, a preparation method and application thereof, sulfur and siderite are physically fused together to prepare an integrated composite biological carrier with a novel structure under the condition of not changing the composition of the carrier, the sulfur in the biological carrier can realize deep nitrogen removal, siderite can assist in realizing automatic pH adjustment, and generated ferrous ions can be used for the processes of phosphorus removal and denitrification, but the filler prepared by the patent has small specific surface area, lower strength and easy blockage.
The steel slag is used as waste in metallurgical industry, has great discharge amount, and brings environmental pollution when not being treated. The steel slag is loose and porous after being ground, has larger specific surface area, contains a large amount of alkaline oxides and a considerable amount of iron, and can provide reaction conditions for the dephosphorization of the wastewater. In addition, the steel slag has wide source, low price, high strength and adsorption effect, is suitable for being used as the filler of the biological filter, can achieve the effect of treating wastes with processes of wastes against one another, and can be recycled. At present, steel slag directly used as a filler has common adsorption capacity on nitrate and poor microorganism biofilm formation effect, so that the adsorption removal performance of the steel slag on the nitrate and microorganisms needs to be improved by a certain modification method, and the removal effect of the nitrate is strengthened. The nitrate adsorbed by the steel slag needs to be further converted into nontoxic and harmless nitrogen through denitrification, the coupling denitrification is the mainstream process of biological denitrification at present, and compared with the single denitrification process, the coupling denitrification has the advantages of high denitrification efficiency, low energy consumption and cost, low residual sludge yield and the like, and has wide application prospect in the biological denitrification process of wastewater. Therefore, how to attach the coupling denitrification function to the steel slag is also a problem to be overcome when the steel slag is used as the biological filter filler.
Disclosure of Invention
The purpose is as follows: the invention provides a modified steel slag filler and a preparation method and application thereof, aiming at overcoming the defects in the prior art and solving the problems of small specific surface area of the biological filler, long time for biofilm formation of microorganisms, poor treatment effect on slightly polluted water bodies and the like in the prior sewage treatment technology.
The technical scheme is as follows: in order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a modified steel slag filler comprises the following steps:
step (1): preparing clean steel slag with the particle size of 30-80 meshes;
step (2): adding ultrapure water into the steel slag prepared in the step (1), heating to 60-70 ℃ under normal pressure, stirring, respectively and simultaneously dropwise adding the mixed salt solution A and the coprecipitator B in the process, maintaining the pH at 9-10 by controlling the dropwise adding speed, and continuously stirring and reacting for 1-2 hours after dropwise adding is finished to obtain a suspension;
the mixed salt solution A contains Mg2+、Al3+、Fe3+The coprecipitate B is prepared from NaOH solution and Na2CO3Solution composition;
and (3): drying and aging the suspension obtained in the step (2) at 60-90 ℃, washing the suspension to be neutral, drying the suspension at 80-105 ℃, and roasting the dried suspension at 400-500 ℃ for 4-6 h to obtain the steel slag-like metal carbonate hydrotalcite S-LDHs;
and (4): crushing and screening S-LDHs, selecting S-LDHs with the particle size of less than 100 meshes, placing the S-LDHs into an anaerobic reaction tank, heating to 115-130 ℃, adding a carbon source and a sulfur source, stirring and reacting to form a molten mixture, and performing wet granulation or cooling granulation to obtain the modified steel slag filler.
In some embodiments, in the step (1), converter steel slag is used as a raw material, the steel slag is manually crushed into steel slag with a particle size of less than 50mm, the steel slag is finely crushed by a planetary high-energy ball mill and sieved to obtain the steel slag with a particle size of 30-80 meshes, and the steel slag is washed for three times by distilled water and then dried in an oven to obtain the clean steel slag with the particle size of 30-80 meshes.
In some embodiments, wherein the mixed salt solution a has the following molar ratio of metal ions: mg (magnesium)2+:(Al3++Fe3+)=1~3,Fe3+:Al3+=1~3;Mg2++Al3++Fe3+=0.8~1.2mol/L;
The relationship between the addition amount of the coprecipitate B and the molar concentration of the metal ions in the mixed salt solution A is as follows: NaOH: (Mg)2++Al3++Fe3+)=1.8~2.5,Na2CO3:(Al3++Fe3+)=1.8~2.5。
Further, in the mixed salt solution A, Mg2++Al3++Fe3+=0.8~1.2mol/L;
The relationship between the addition amount of the coprecipitate B and the molar concentration of the metal ions in the mixed salt solution A is as follows: NaOH: (Mg)2++Al3++Fe3+)=1.8~2.5,Na2CO3:(Al3++Fe3+)=1.8~2.5。
In some embodiments, in the step (2), the volume-to-mass ratio of the ultrapure water (ml) to the steel slag (g) is (10-30) ml: 1g of a compound; the volume ratio of the total volume of the mixed salt solution A and the coprecipitator B solution to the steel slag-containing ultrapure water is 1: (0.9-1.1).
In some embodiments, in the step (3), the suspension obtained in the step (2) is placed in a 60-90 ℃ forced air drying oven and aged for 10-12 hours; filtering and washing with water until the product is neutral, transferring the obtained product into a beaker, drying the product at the temperature of 80-105 ℃ for 6-12 h, and roasting the product in a box-type resistance furnace at the temperature of 400-500 ℃ (preferably 450 ℃) for 4-6 h to obtain the steel slag-like metal carbonate hydrotalcite S-LDHs.
In some embodiments, in the step (4), the carbon source is degradable polymer polybutylene succinate PBS, and the sulfur source is sulfur; further, in the step (4), the mass ratio of the added S-LDHs to the added PBS to the added sulfur is S-LDHs: PBS: 1, sulphur: (0.2-1.0): (0.2-1.0).
In the step (4), the wet granulation refers to uniformly dripping the molten mixture in the reaction tank into cold water, and rapidly cooling to form a solid filler; by cold granulation is meant that the molten mixture is cooled in the reaction tank to form a solid material which is then broken up to form a filler.
In a second aspect, the invention also provides a modified steel slag filler prepared by the preparation method of the modified steel slag filler.
In a third aspect, the invention also provides application of the modified steel slag filler in nitrogen and phosphorus removal treatment of wastewater.
The modified steel slag filler provided by the invention has the advantages that the specific surface area of the modified steel slag filler is large, the modified steel slag filler has adsorption and synchronous nitrogen and phosphorus removal functions, no additional liquid carbon source is needed, and the modified steel slag filler has good nitrogen and phosphorus removal effects on polluted water bodies with different degrees. The steel slag-like metal carbonate hydrotalcite can release iron ions to remove phosphorus, can adsorb and gather microorganisms and nitrates in water, and can perform harmless treatment on the nitrates through PBS and sulfur coupling denitrification to achieve the effect of desorption and nitrogen removal.
Has the advantages that: the modified steel slag filler and the preparation method and the application thereof provided by the invention have the following advantages:
(1) the modified steel slag filler with the functions of adsorption, nitrogen and phosphorus removal, and the preparation method and the application thereof provided by the invention have the advantages that the steel slag is used as a precursor, the raw materials are easy to obtain, the price is low, and the purpose of treating wastes with processes of wastes against one another can be achieved by using the steel slag as a raw material. And the steel slag can release iron ions into the water body, thereby achieving the purpose of dephosphorization.
(2) The composite metal oxide is loaded on the surface of the steel slag, and the steel slag is roasted at high temperature, so that the porosity and the surface performance of the steel slag can be improved to a great extent, functional groups on the surface of the steel slag are changed, and the anion exchange capacity of the surface of the steel slag is improved, so that the steel slag has the capacity of adsorbing nitrate.
(3) The solid carbon source PBS and the sulfur are loaded on the surface of the modified steel slag in a combined manner, so that the coupling denitrification can be realized, and compared with a single denitrification process, the coupling denitrification process has the advantages of high denitrification efficiency, low energy consumption and cost and low sludge yield. The adsorption of the modified steel slag on nitrate nitrogen can further promote the generation of coupling denitrification, and the modified steel slag has a good removal effect on low-pollution water bodies.
Drawings
FIG. 1 is a graph showing the effects of using a modified steel slag filler according to an embodiment of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
The micro-polluted water is polluted by organic matters, and part of water quality indexes exceed the first-class A discharge standard of pollutant discharge standard of urban sewage treatment plants. In the embodiment of the invention, M2+Is Mg2+,M3+Is Al3+With Fe3+And (4) summing. The mixed salt can adopt nitrate, hydrochloride or sulfate which is easy to dissolve in water; in this example, Mg (NO) is used3)2·6H2O、Al(NO3)3·9H2O、Fe(NO3)3·9H2O。
Example 1
A preparation method of a modified steel slag filler with adsorption, nitrogen and phosphorus removal functions comprises the following steps:
grinding open-hearth furnace steel slag to 30-80 mesh particle size, washing with distilled water for three times, drying, putting into a beaker, adding ultrapure water into the beaker, and simultaneously dripping a mixed solution A and a coprecipitator B with the same volume as the ultrapure water into the beaker, wherein the mixed salt solution A contains Mg (NO)3)2·6H2O、Al(NO3)3·9H2O、Fe(NO3)3·9H2O, coprecipitator B solution contains NaOH and Na2CO3(ii) a Wherein M in the solution A2+:M3+1 to 3 (molar ratio), M2++M3+1mol/L, Fe: 1-3 (molar ratio) of Al, NaOH in the B solution: (M)2++M3+) 2 (molar ratio), Na2CO3:M3+2 (molar concentration ratio). Keeping the dropping speed at 1 drop/s, stirring vigorously, keeping the pH value at 9-10, and continuing stirring for 1-2 hours after the dropping is finished. And (3) placing the obtained suspension in a 60 ℃ forced air drying box, and aging for 10-12 h. Filtering and washing with water until the solution is neutral, transferring the obtained product into a beaker, drying the product at 105 ℃ for 12h, and roasting the product in a box-type resistance furnace at 450 ℃ for 6h to obtain S-LDHs. Crushing and screening S-LDHs, selecting steel slag with the particle size of less than 100 meshes, putting the steel slag into an anaerobic reaction tank, heating to 120 ℃, adding a carbon source and a sulfur source into the reaction tank, and stirring for 30-60 min, wherein the S-LDHs: PBS: the mass ratio of sulfur is 3:1: 1. The modified filler in the embodiment is obtained through wet granulation, and the particle size is 5-10 mm.
The wastewater of a certain factory in Jiangsu enters a biological filter filled with the filler after aeration, the hydraulic retention time is 3h, and the pollutant removal rate in stable operation is as follows.
Contaminants | TN | TP | COD | SS |
Feed water concentration (mg/L) | 800~1000 | 35~50 | 100~120 | 30~40 |
Removal Rate (%) | 81~87 | 88~93 | 78~92 | 83~95 |
Example 2
A preparation method of a modified steel slag filler with adsorption, nitrogen and phosphorus removal functions comprises the following steps:
grinding open-hearth furnace steel slag to 30-80 mesh particle size, washing with distilled water for three times, drying, putting into a beaker, adding ultrapure water into the beaker, and simultaneously dripping a mixed solution A and a coprecipitator B with the same volume as the ultrapure water into the beaker, wherein the mixed salt solution A contains Mg (NO)3)2·6H2O、Al(NO3)3·9H2O、Fe(NO3)3·9H2O, coprecipitator B solution contains NaOH and Na2CO3(ii) a Wherein M in the solution A2+:M3+1 to 3 (molar ratio), M2++M3+1mol/L, Fe: 1-3 (molar ratio) of Al, NaOH in the B solution: (M)2++M3+) 2 (molar ratio), Na2CO3::M3+2 (molar concentration ratio). Keeping the dropping speed at 1 drop/s, stirring vigorously, keeping the pH value at 9-10, and continuing stirring for 1-2 hours after the dropping is finished. And (3) placing the obtained suspension in a 60 ℃ forced air drying box, and aging for 10-12 h. And filtering and washing with water until the solution is neutral, transferring the obtained product into a beaker, drying the product at 105 ℃ for 12 hours, and roasting the product in a box-type resistance furnace at 450 ℃ for 4-6 hours to obtain S-LDHs. Putting the steel slag with the particle size of less than 100 meshes obtained by crushing and screening S-LDHs into an anaerobic reaction tank, heating to 115-130 ℃, adding PBS and sulfur into the reaction tank, and stirring for 30-60 min, wherein the S-LDHs: PBS: the sulfur (mass ratio) is 1: 1:1, screening out the modified steel slag with the particle size of 8-10 mm as the filler of the embodiment through cooling granulation.
The laboratory prepares the simulated wastewater with the ammonia nitrogen concentration of 5mg/L, the nitrate nitrogen concentration of 25mg/L and the TP of 5 mg/L. The filler is filled into a denitrification biological filter, simulated wastewater is pumped into the reactor from the bottom end of the reactor by a peristaltic pump, the hydraulic retention time of the sewage in the reactor is 1h, the detected ammonia nitrogen concentration is lower than 0.5mg/L, the nitrate nitrogen concentration is lower than 2.5mg/L, the nitrite nitrogen concentration is lower than 1mg/L, the TN removal efficiency reaches 86.7%, the effluent TP concentration is lower than 0.15mg/L, and the TP removal efficiency reaches 97%.
Example 3
Grinding open-hearth furnace steel slag to 30-80 mesh particle size, washing with distilled water, drying, placing into a beaker, adding ultrapure water into the beaker, and simultaneously dripping a mixed solution A and a coprecipitator B with the same volume as the ultrapure water into the beaker, wherein the mixed salt solution A contains Mg (NO)3)2·6H2O、Al(NO3)3·9H2O、Fe(NO3)3·9H2O, coprecipitator B solution contains NaOH and Na2CO3(ii) a Wherein M in the solution A2+:M3+1 to 3 (molar ratio), M2++M3+1mol/L, Fe: 1-3 (molar ratio) of Al, NaOH in the B solution: (M)2++M3+) 2 (molar ratio), Na2CO3::M3+2 (molar concentration ratio). Keeping the dropping speed at 1 drop/s, stirring vigorously, keeping the pH value at 9-10, and continuing stirring for 1-2 hours after the dropping is finished. And (3) placing the obtained suspension in a 60 ℃ forced air drying box, and aging for 10-12 h. Filtering and washing with water until the solution is neutral, transferring the obtained product into a beaker, drying the product for 12 hours at the temperature of 100 ℃, and roasting the product for 4 to 6 hours in a box-type resistance furnace at the temperature of 450 ℃ to obtain S-LDHs. Putting the steel slag with the particle size of less than 100 meshes obtained by crushing and screening S-LDHs into an anaerobic reaction tank, heating to 115-130 ℃, adding PBS and sulfur into the reaction tank, and stirring for 30-60 min, wherein the S-LDHs: PBS: the sulfur (mass ratio) is 2: 1:1, the modified steel slag with the grain size controlled to be 5-8 mm is used as the filler of the embodiment by wet granulation.
Effect verification:
the filler is filled into a biological filter (h is 700mm, D is 80mm) with the filling height of 650mm, and simulated wastewater (NO) is introduced into the biological filter from top to bottom3 -The concentration of N is 100mg/L, the concentration of TP is 20mg/L), HRT is set to be 2h, the sampling time interval is 1d, the concentration of effluent pollutants is shown in figure 1, and it can be seen that the biofilter has stable removal efficiency on total phosphorus on day 2, the concentration of effluent total phosphorus is lower than 0.2mg/L, the removal efficiency on nitrate nitrogen on day 16 is stable, and the concentration of effluent nitrate nitrogen is lower than 3 mg/L.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (10)
1. A preparation method of a modified steel slag filler is characterized by comprising the following steps:
step (1): preparing clean steel slag with the particle size of 30-80 meshes;
step (2): adding ultrapure water into the steel slag prepared in the step (1), heating to 60-70 ℃ under normal pressure, stirring, respectively and simultaneously dropwise adding the mixed salt solution A and the coprecipitator B in the process, maintaining the pH at 9-10 by controlling the dropwise adding speed, and continuously stirring and reacting for 1-2 hours after dropwise adding is finished to obtain a suspension;
the mixed salt solution A contains Mg2+、Al3+、Fe3+The coprecipitate B is prepared from NaOH solution and Na2CO3Solution composition;
and (3): drying and aging the suspension obtained in the step (2) at 60-90 ℃, washing the suspension to be neutral, drying the suspension at 80-105 ℃, and roasting the dried suspension at 400-500 ℃ for 4-6 h to obtain steel slag-like metal carbonate hydrotalcite S-LDHs;
and (4): crushing and screening S-LDHs, selecting S-LDHs with the particle size of less than 100 meshes, placing the S-LDHs into an anaerobic reaction tank, heating to 115-130 ℃, adding a carbon source and a sulfur source, stirring and reacting to form a molten mixture, and performing wet granulation or cooling granulation to obtain the modified steel slag filler.
2. The preparation method of the modified steel slag filler according to claim 1, wherein in the step (1), converter steel slag is used as a raw material, the steel slag is manually crushed to hammer-crush the massive steel slag into steel slag with the particle size of less than 50mm, the steel slag is finely crushed by a planetary high-energy ball mill and sieved to obtain the steel slag with the particle size of 30-80 meshes, and the steel slag is washed for three times by distilled water and then placed in an oven to be dried to obtain the clean steel slag with the particle size of 30-80 meshes.
3. The method of claim 1, wherein the mixed salt solution A contains the following metal ions in the following molar ratio: mg (magnesium)2+:(Al3++Fe3+)=1~3,Fe3+:Al3+=1~3。
4. The method of claim 3, wherein the steel slag filler is a steel slag filler,
in mixed salt solution A, Mg2++Al3++Fe3+=0.8~1.2mol/L;
The relationship between the addition amount of the coprecipitate B and the molar concentration of the metal ions in the mixed salt solution A is as follows: NaOH: (Mg)2++Al3++Fe3+)=1.8~2.5,Na2CO3:(Al3++Fe3+)=1.8~2.5。
5. The preparation method of the modified steel slag filler according to claim 4, wherein in the step (2), the volume-to-mass ratio of the added ultrapure water to the steel slag is (10-30) ml: 1g of a compound;
the volume ratio of the total volume of the mixed salt solution A and the coprecipitator B solution to the steel slag-containing ultrapure water is 1: (0.9-1.1).
6. The preparation method of the modified steel slag filler according to claim 1, wherein in the step (3), the suspension obtained in the step (2) is placed in a blast drying oven at 60-90 ℃ and aged for 10-12 h; filtering and washing with water until the product is neutral, transferring the obtained product into a beaker, drying the product at the temperature of 80-105 ℃ for 6-12 h, and roasting the product in a box-type resistance furnace at the temperature of 400-500 ℃ for 4-6 h to obtain the steel slag-like metal carbonate hydrotalcite S-LDHs.
7. The method for preparing modified steel slag filler according to claim 1, wherein in the step (4), the carbon source is degradable polymer polybutylene succinate (PBS), and the sulfur source is sulfur;
the mass ratio of the added S-LDHs to the added PBS to the added sulfur is S-LDHs: PBS: sulfur = 1: (0.2-1.0): (0.2-1.0).
8. The method for preparing modified steel slag filler according to claim 1, wherein in the step (4), the wet granulation is to uniformly drop the molten mixture in the reaction tank into cold water and rapidly cool the mixture to form solid filler; by cold granulation is meant that the molten mixture is cooled in the reaction tank to form a solid material which is then broken up to form a filler.
9. A modified steel slag filler prepared by the method of preparing a modified steel slag filler according to any one of claims 1 to 9.
10. The use of the modified steel slag filler of claim 9 in the nitrogen and phosphorus removal treatment of wastewater.
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CN112978912A (en) * | 2021-05-06 | 2021-06-18 | 臻和慧联(浙江)环境科技有限公司 | Sewage treatment agent, autotrophic denitrification microorganism carrier and preparation method thereof |
CN114160116A (en) * | 2021-11-08 | 2022-03-11 | 万华化学集团股份有限公司 | Steel slag-based zirconium catalyst, preparation method and application of steel slag-based zirconium catalyst in preparation of 1, 4-butanediol and coproduction of methacrolein |
CN114956306A (en) * | 2022-04-28 | 2022-08-30 | 南京大学 | Modified coupling denitrification biological filler and preparation method and application thereof |
CN117125808A (en) * | 2023-09-28 | 2023-11-28 | 青岛鑫源环保集团有限公司 | Special nitrogen-removing composite modified filler for water purification treatment and preparation method thereof |
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