CN114591098A - Modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen and preparation method thereof - Google Patents
Modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen and preparation method thereof Download PDFInfo
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Abstract
The invention provides a modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen and a preparation method thereof, wherein the modified cancrinite ceramsite comprises the following raw material components in percentage by mass: 40-90% of fly ash, 0-20% of rare earth tailings, 0-20% of blast furnace slag, 5-30% of pore-forming agent and 0-20% of additive. The raw materials are solid wastes such as fly ash and rare earth tailings, so that high-value utilization of the solid wastes and efficient and rapid adsorption of ammonia nitrogen can be realized; the modified cancrinite ceramsite prepared by the method is used for efficiently adsorbing ammonia nitrogen in wastewater, treats waste with waste, and has great significance for high-valued utilization of solid waste and water pollution treatment.
Description
Technical Field
The invention belongs to the technical field of solid waste treatment and environmental engineering water treatment, and particularly relates to a modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen and a preparation method thereof.
Background
The nitrogen element is usually present in the water body in four forms of organic nitrogen, ammonium nitrogen, nitrate and nitrite, wherein the ammonium Nitrogen (NH)4-N) is the predominant form of presence. The ammonia nitrogen wastewater mainly comes from two major types, namely nature and man-made, and along with the development of the economic society, the amount of the ammonia nitrogen wastewater from man-made sources is increased year by year, such as urban domestic sewage, agricultural sewage, industrial sewage and the like. A large amount of untreated wastewater reaching the standard is discharged into rivers, lakes and the like, so that serious water eutrophication is caused, and a large amount of algae and microorganisms are propagated in the water. At the same time, NH4the-N can carry out nitration reaction with nitrifying bacteria, consume dissolved oxygen in the water body, and cause mass death of fishes in the water body due to oxygen deficiency. Therefore, strict discharge standards of ammonia nitrogen wastewater have been promulgated both in China and in other places.
At present, the treatment methods for ammonia nitrogen wastewater mainly include magnesium ammonium phosphate chemical precipitation method, physical methods represented by adsorption method and ammonia stripping method, ion exchange method, chlorine breaking point method and the like. Wherein, the adsorption method has the advantages of wide application range, good treatment effect, simple operation, small secondary pollution, reusable adsorbent and the like. The common adsorbent comprises diatomite, alumina, natural zeolite, artificial zeolite, bentonite, active carbon, artificial ceramsite and the like.
However, the existing adsorbents mainly have the following problems: firstly, the dependence on natural minerals, such as bentonite and natural zeolite, does not accord with the sustainable development strategy; secondly, the artificially synthesized zeolite usually mainly takes zeolite powder, so that the difficulty of solid-liquid separation in the later period is high, and the operation cost is increased; thirdly, the artificial ceramsite adsorbing material has small adsorption capacity and poor treatment effect.
The preparation of artificial ceramsite by utilizing solid waste is utilized in the prior art, however, the ceramsite prepared by the prior art and used for adsorption has generally poor adsorption performance and cannot be widely applied to the treatment of ammonia nitrogen wastewater. Therefore, how to synthesize the modified cancrinite ceramsite adsorbent with good adsorption performance and low cost by using the solid waste has important significance for high-valued treatment of the solid waste and high-efficiency treatment of water resources.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide the modified cancrinite ceramsite for efficiently removing ammonia nitrogen and the preparation method thereof.
The technical scheme adopted for solving the problems in the prior art is as follows:
the modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen is characterized by comprising the following raw materials in percentage by mass: 40-90% of fly ash, 0-20% of rare earth tailings, 0-20% of blast furnace slag, 5-30% of pore-forming agent and 0-20% of additive.
The pore-forming agent is one or a mixture of more of activated carbon, graphite powder, coal powder, straws and leaves.
The additive is quartz sand or waste glass.
The preparation method of the modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen is characterized by comprising the following steps of:
and 3, mixing the ceramsite obtained in the step 2 with a sodium hydroxide solution, placing the mixture into a reaction kettle, and placing the reaction kettle into an oven to react for a certain time to obtain the modified cancrinite ceramsite.
The preheating temperature in the step 2 is 400-600 ℃, and the preheating time is 10-30 min.
The sintering temperature in the step 2 is 900-.
The concentration of the sodium hydroxide in the step 3 is 1-6mol/L, and the solid-to-liquid ratio of the ceramsite to the solution is 1: 5-1: 20 g/mL.
The reaction temperature in the step 3 is 100-200 ℃, and the reaction time is 2-48 h.
The invention has the following advantages:
1. the raw materials adopted by the invention are solid wastes such as solid wastes fly ash, rare earth tailings, waste glass and the like, and the invention has the beneficial effects of environmental protection and high-value utilization of the solid wastes. The basic principle of the invention is as follows: the main chemical component of the solid waste is SiO2、Al2O3And CaO, etc., which is consistent with the basic composition of cancrinite, with the potential to synthesize cancrinite. The ceramsite can be fired at high temperature, meanwhile, the activating effect on components in solid waste can be generated, cancrinite crystals can be synthesized more easily, and then NaOH solution is adopted as a modifier to convert the ceramsite from albite crystals to cancrinite crystals under hydrothermal conditions, as shown in figures 1(a) to 1 (f). The prepared modified cancrinite ceramsite is used for efficiently adsorbing ammonia nitrogen in wastewater, treats waste with waste, and has great significance for high-valued utilization of solid waste and water pollution treatment.
2. The modified cancrinite ceramsite of the invention is ceramsite with zeolite cancrinite phase, and the occurrence of cancrinite crystals can greatly increase the specific surface area and the adsorption performance of the ceramsite, as shown in figure 2, the specific surface area can be 1.259m before modification2Lifting the weight per gram to 17.92m2(ii) in terms of/g. The modified cancrinite ceramsite has the characteristics of high strength and high water absorption of the ceramsite, and also has the high adsorption property of zeolite, so that the application value of the modified cancrinite ceramsite can be greatly expanded.
3. When the adding amount of the modified cancrinite ceramsite is 2g/L for a solution with the original ammonia nitrogen concentration of 100mg/L, the unit ammonia nitrogen adsorption amount can reach 17mg/g, and the modified cancrinite ceramsite is about 5-10 times of the adsorption performance of common ceramsite; when the adding amount is 5g/L, the ammonia nitrogen removal rate of 2h can reach about 90 percent.
Drawings
FIG. 1(a) shows the molecular structure of albite contained in ceramsite before modification;
FIG. 1(b) shows the molecular structure of cancrinite contained in the modified ceramsite;
FIG. 1(c) is a pore structure of cancrinite contained in the modified ceramsite;
FIG. 1(d) shows albite [ SiO ] contained in the ceramsite before modification4]4-And [ AiO ]4]5-A connection mode;
FIG. 1(e) shows modified ceramsite containing nepheline [ SiO ]4]4-And [ AiO ]4]5-A connection mode;
FIG. 1(f) is the SiO pore canal containing calcium nepheline in the modified ceramsite4]4-And [ AiO ]4]5-A connection mode;
FIG. 2(a) shows the N content of the ceramsite2Adsorption-desorption curves;
FIG. 2(b) is the N of cancrinite ceramsite2Adsorption-desorption curves;
FIG. 3 is an XRD spectrum of the ceramsite before and after modification;
FIG. 4(a) SEM photograph of ceramsite before modification;
FIG. 4(b) is an SEM photograph of the modified ceramsite of example 1;
FIG. 4(c) is an SEM photograph of the modified ceramsite of example 2;
FIG. 4(d) is an SEM photograph of the modified ceramsite of example 3;
FIG. 4(e) is an SEM photograph of the modified ceramsite of example 4;
FIG. 5 shows NH of ceramsite before and after modification4N unit adsorption amount (the adding amount of the ceramsite is 2 g/L);
FIG. 6 shows NH of ceramsite before and after modification4The N removal rate (the addition of the ceramsite is 5 g/L).
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments and the accompanying drawings.
Example 1
1. Raw materials: weighing 70g of fly ash, 10g of rare earth tailings, 20g of quartz sand, 30g of activated carbon and 130g of total mass.
2. The preparation method comprises the following steps: putting the weighed raw materials into a planetary ball mill (QM-3SP2) for wet milling for 4h, wherein the ball-material ratio is 4:1, the ball milling medium is absolute ethyl alcohol, the rotating speed is 300rpm, and the obtained slurry is put into a 90 ℃ constant temperature drying oven (DHG-9040A) for drying for 24 h. The dried powder is made into raw material balls with the diameter of 8-10mm by a ball forming mill. Placing the raw material balls into a muffle furnace (KSL-1700X) for firing, wherein the sintering system is as follows: preheating at 600 deg.C for 10 min; the sintering temperature is 1050 ℃, the heat preservation time is 30min, the heating rate is 5 ℃/min, and after the firing is finished, the sample is taken out after the furnace is cooled to the room temperature. And (3) placing 1.5g of fired ceramsite into a reaction kettle, adding 15mL of 3mol/L NaOH solution, placing the mixture into an oven for reacting for 12h at 160 ℃, and taking out the mixture to obtain the modified cancrinite ceramsite.
Example 2
1. Raw materials: weighing 70g of fly ash, 10g of rare earth tailings, 20g of waste glass, 40g of leaves and 140g of total mass.
2. The preparation method comprises the following steps: putting the weighed raw materials into a planetary ball mill (QM-3SP2) for wet milling for 4h, wherein the ball-material ratio is 4:1, the ball milling medium is absolute ethyl alcohol, the rotating speed is 300rpm, and the obtained slurry is put into a 90 ℃ constant temperature drying oven (DHG-9040A) for drying for 24 h. And drying to obtain powder, and making into raw material balls with diameter of 8-10mm by using a ball forming mill. Placing the raw material balls into a muffle furnace (KSL-1700X) for firing, wherein the sintering system is as follows: preheating at 500 deg.C for 5 min; the sintering temperature is 1040 ℃, the holding time is 40min, the heating rate is 5 ℃/min, and after the firing is finished, the sample is taken out after the furnace is cooled to the room temperature. And (3) placing 1.5g of fired ceramsite into a reaction kettle, adding 20mL of 4mol/L NaOH solution, placing the mixture into an oven for reaction at 180 ℃ for 10 hours, and taking out the mixture to obtain the modified cancrinite ceramsite.
Example 3
1. Raw materials: weighing 70g of fly ash, 25g of rare earth tailings, 10g of quartz sand, 30g of coal powder and 130g of total mass.
2. The preparation method comprises the following steps: putting the weighed raw materials into a planetary ball mill (QM-3SP2) for wet milling for 4h, wherein the ball-material ratio is 4:1, the ball milling medium is absolute ethyl alcohol, the rotating speed is 300rpm, and the obtained slurry is put into a 90 ℃ constant-temperature drying oven (DHG-9040A) for drying for 24 h. And preparing the dried powder into raw material balls with the diameter of 8-10mm by adopting an artificial granulation mode. Placing the raw material balls into a muffle furnace (KSL-1700X) for firing, wherein the sintering system is as follows: preheating at 500 deg.C for 20 min; and (3) carrying out heat preservation for 30min at the sintering temperature of 1050 ℃, wherein the heating rate is 5 ℃/min, and taking out the sample after cooling to room temperature along with the furnace after firing. And (3) placing 1.5g of fired ceramsite into a reaction kettle, adding 15mL of 3.5mol/L NaOH solution, placing the mixture into an oven for reacting for 24 hours at 160 ℃, and taking out the mixture to obtain the modified cancrinite ceramsite.
Example 4
1. Raw materials: weighing 70g of fly ash, 20g of rare earth tailings, 10g of waste glass, 30g of graphite powder and 130g of total mass.
2. The preparation method comprises the following steps: putting the weighed raw materials into a planetary ball mill (QM-3SP2) for wet milling for 4h, wherein the ball-material ratio is 4:1, the ball milling medium is absolute ethyl alcohol, the rotating speed is 300rpm, and the obtained slurry is put into a 90 ℃ constant temperature drying oven (DHG-9040A) for drying for 24 h. And (3) preparing the dried powder into raw material balls with the diameter of 6-8mm by using a pelletizer. Placing the raw material balls into a muffle furnace (KSL-1700X) for firing, wherein the sintering system is as follows: preheating at 500 deg.C for 10 min; the sintering temperature is 1050 ℃, the temperature is kept for 60min, the heating rate is 5 ℃/min, and after the firing is finished, the sample is taken out after the furnace is cooled to the room temperature. And (3) putting 1.5g of fired ceramsite into a reaction kettle, adding 15mL of 2.5mol/L NaOH solution, putting the mixture into an oven for reacting for 48 hours at 160 ℃, and taking out the mixture to obtain the modified cancrinite ceramsite.
The above description is only exemplary of the present invention and is not intended to limit the present invention, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
TABLE 1 physical Properties and Ammonia Nitrogen adsorption Properties of modified cancrinite ceramsite prepared by each example
From the above table, it can be seen that the modified cancrinite ceramsite prepared by the novel process provided by the invention. By making use ofAfter the performance is improved, the high water absorption of the original ceramsite is kept, and the specific surface area and the pore volume are greatly improved, wherein the specific surface area and the pore volume are represented by N in a figure 22The absorption and desorption curves show that the modified ceramsite has N2The adsorption capacity of the adsorbent is obviously improved, and the specific surface area is improved by about 14 times through calculation. Fig. 3 is an XRD spectrum of the ceramsite before and after modification, and the ceramsite is transformed from the original albite crystal into cancrinite crystal by the modification method provided by the present invention, which is the main reason why the modified ceramsite has a large specific surface area and is also the benefit of the present invention. FIG. 4 is SEM photographs of samples before and after modification, and comparison shows that a large amount of fine cancrinite crystals grow in the ceramsite modified by the method provided by the invention, and the pore structure of the ceramsite is also converted from a simple three-dimensional through hole into a composite-pore ceramsite with macropores, mesopores and cancrinite micropores. The data in table 1 can be seen in conjunction with fig. 5 and 6. The unit adsorption capacity of the ceramsite to ammonia nitrogen in water is improved by about 8 times, and simultaneously, the ceramsite is far higher than the current ceramsite sold in the market.
The protective scope of the present invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the present invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (8)
1. The modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen is characterized by comprising the following raw materials in percentage by mass: 40-90% of fly ash, 0-20% of rare earth tailings, 0-20% of blast furnace slag, 5-30% of pore-forming agent and 0-20% of additive.
2. The modified cancrinite ceramsite for efficiently removing ammonia nitrogen of claim 1, which is characterized in that: the pore-forming agent is one or a mixture of more of activated carbon, graphite powder, coal powder, straws and leaves.
3. The modified cancrinite ceramsite for efficiently removing ammonia nitrogen of claim 1, which is characterized in that: the additive is quartz sand or waste glass.
4. The preparation method of the modified cancrinite ceramsite for efficiently removing ammonia nitrogen according to any one of claims 1-3, which is characterized by comprising the following steps:
step 1, preparing raw materials into raw material balls with the diameter of 2-10mm by using a ball forming mill through material mixing and ball milling;
step 2, naturally drying the raw material balls obtained in the step 1 at room temperature for 24 hours, then placing the raw material balls in a drying oven, drying the raw material balls at 105 ℃ for 2 to 4 hours, placing the raw material balls in a muffle furnace, preheating the raw material balls for a certain time, and then sintering the raw material balls to obtain ceramsite;
and 3, mixing the ceramsite obtained in the step 2 with a sodium hydroxide solution, placing the mixture into a reaction kettle, and placing the reaction kettle into an oven to react for a certain time to obtain the modified cancrinite ceramsite.
5. The method for preparing the modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen according to claim 4, is characterized by comprising the following steps: the preheating temperature in the step 2 is 400-600 ℃, and the preheating time is 10-30 min.
6. The method for preparing the modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen according to claim 4, is characterized by comprising the following steps of: the sintering temperature in the step 2 is 900-.
7. The method for preparing the modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen according to claim 4, is characterized by comprising the following steps: the concentration of the sodium hydroxide in the step 3 is 1-6mol/L, and the solid-to-liquid ratio of the ceramsite to the solution is 1: 5-1: 20 g/mL.
8. The method for preparing the modified cancrinite ceramsite capable of efficiently removing ammonia nitrogen according to claim 4, is characterized by comprising the following steps: the reaction temperature in the step 3 is 100-200 ℃, and the reaction time is 2-48 h.
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| CN117229039A (en) * | 2023-11-13 | 2023-12-15 | 天津包钢稀土研究院有限责任公司 | Preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength |
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| CN116835997A (en) * | 2023-08-31 | 2023-10-03 | 内蒙古科技大学 | Method for preparing ceramsite filter material |
| CN116835997B (en) * | 2023-08-31 | 2023-11-21 | 内蒙古科技大学 | Method for preparing ceramsite filter material |
| CN117229039A (en) * | 2023-11-13 | 2023-12-15 | 天津包钢稀土研究院有限责任公司 | Preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength |
| CN117229039B (en) * | 2023-11-13 | 2024-01-23 | 天津包钢稀土研究院有限责任公司 | Preparation method of rare earth carbonate fly ash ceramsite with high barrel pressure strength |
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