CN110975811A - Method for preparing adsorbent by using high-alumina fly ash and application - Google Patents
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- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 7
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- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a method for preparing an adsorbent by using high-alumina fly ash, which comprises the steps of taking industrial solid waste high-alumina fly ash as a raw material, carrying out activation and acid leaching to obtain an aluminum solution, mixing and reacting the aluminum solution with a surfactant, adjusting the pH = 6.5-7.5 of the solution, carrying out flocculation and standing, drying a filtered solid, and calcining to obtain the adsorbent; the adsorbent is applied to adsorbing heavy metal ions of cadmium Cd (II), and has the characteristics of high adsorption speed, high adsorption rate, deep removal of cadmium in a water body with low cadmium concentration and the like; the invention provides a method for utilizing the high added value of the fly ash and provides a new way for treating the water body containing the heavy metal ion cadmium ion.
Description
Technical Field
The invention relates to a method for preparing a cadmium adsorbent by using high-alumina fly ash and application thereof, belonging to the fields of secondary utilization of solid waste resources and treatment of heavy metal-containing water bodies.
Background
The fly ash is one of byproducts of coal-fired power generation, and the storage amount of the fly ash in China exceeds 30 hundred million tons, and is one of main industrial waste residues. The fly ash is also a main pollution source of PM2.5 haze pollution in China, and the fly ash accumulated in large amount not only occupies land but also occupies large areaAnd the fly ash particles are fine and easy to fly dust, thus causing air pollution. The chemical component of the fly ash is mainly SiO2（40～60%）、 Al2O3(17-35%), FeO (2-15%), CaO (1-10%), and the balance of small amounts of K, P, S, Mg and other compounds and trace amounts of As, Cu, Zn and other compounds; the content of alumina in fly ash in inner Mongolia and Shanxi areas of China is often more than 30%, and the fly ash can be used as a raw material for synthesizing an aluminum adsorbent after activation and silicon-aluminum separation.
Cadmium is not an essential element for human bodies and is an environmental pollutant, and in general, cadmium poisoning can occur to people due to excessive intake of cadmium. Cadmium is a food pollutant for key research by the world health organization; the international agency for research on cancer (IARC) classifies cadmium as a human carcinogen, causing serious health damage to humans; the average dose of cadmium causing poisoning in humans is 100 mg. The acute poisoning symptoms are mainly manifested by nausea, salivation, vomiting, abdominal pain and diarrhea, and then central nervous poisoning symptoms are caused. The serious patient may die due to collapse.
Cadmium in the environment mainly comes from crusta and industrial pollution, and due to rapid development of urbanization and industrialization, industries such as metallurgy, smelting, ceramics, electroplating industry and chemical industry (such as batteries, plastic additives, food preservatives, pesticides and pigments) can generate a great amount of cadmium-containing wastewater, cadmium is high in hazard and difficult to remove, and when the environment is polluted by cadmium, cadmium can be enriched in organisms and enters human bodies through food chains to cause chronic poisoning. The existing treatment methods include neutralization precipitation, sulfide precipitation, bleaching powder oxidation, iron oxidation and adsorption. The adsorption method has the advantages of high efficiency, simple operation, reusable adsorbent and the like, but the adsorption effect is influenced by the adsorption performance of the adsorbent, the manufacturing cost is higher, and the preparation of the adsorbent with low cost and high performance becomes the key point for treating the cadmium-containing wastewater by utilizing the adsorption method.
Disclosure of Invention
The invention provides a method for preparing an adsorbent by using high-alumina fly ash, which is used for efficiently and quickly removing cadmium in industrial wastewater.
The method for preparing the adsorbent by using the high-alumina fly ash comprises the steps of mixing the high-alumina fly ash with anhydrous sodium carbonate, sintering and activating at 900-1200 ℃ for 60-120 min, cooling and grinding; acid leaching the ground material at 60-90 ℃ for 1-2 h, performing suction filtration, washing the ground material until filter residue is white, and collecting and combining filtrate and washing liquid to obtain an aluminum-containing solution; adding distilled water and a surfactant solution into an aluminum-containing solution, stirring for 8-12 h at 30-60 ℃, adjusting the pH value of the solution to 6.5-7.5 to enable the solution to flocculate and settle, standing for 48-72 h, then performing suction filtration, drying filter residues, and calcining at 400-800 ℃ to obtain the adsorbent.
The high alumina fly ash is a fly ash with an alumina content of greater than 37%, such as inner Mongolia fly ash.
The mass ratio of the high-alumina fly ash to the sodium carbonate is 1: 0.6-1.2.
The acid leaching uses hydrochloric acid with the mass concentration of 11.1-25.9%, and sodium hydroxide solution is used for adjusting the pH value.
The volume ratio of the distilled water to the aluminum-containing solution is 3-4: 1, and the volume ratio of the surfactant solution to the aluminum-containing solution is 1: 1.6-2.
The surfactant is polyether P123, and the concentration of the surfactant solution is 0.02-0.04 g/mL.
The temperature is increased to 400-800 ℃ at the heating rate of 1-2 ℃/min, collapse of adsorbent pore channels is easily caused by too fast heating, and the production speed is influenced by too slow heating and too long calcining time.
The drying temperature is 60-80 ℃.
The invention also aims to apply the adsorbent prepared by the method to the treatment of cadmium-containing wastewater.
The invention has the beneficial effects that:
1. the invention takes the high-alumina fly ash, the anhydrous sodium carbonate, the strong acid and the surfactant as raw materials to prepare the adsorption material with the mesoporous structure, the process has simple operation method, easy control of the preparation process, low cost and environmental friendliness, and the raw materials come from industrial solid wastes, thus being suitable for industrial production;
2. the adsorbent prepared by the invention has uniform pore size distribution and certain regularity;
3. the adsorbent is applied to the adsorption of heavy metal Cd, and has the characteristics of high adsorption speed, high adsorption rate, capability of adsorbing low-concentration cadmium and removing cadmium.
Drawings
FIG. 1 is a plot of the nitrogen-sorption desorption isotherm of the adsorbent of example 1;
FIG. 2 is a graph of the pore size distribution of the adsorbent of example 1;
FIG. 3 shows the effect of the adsorbent amount of the adsorbent used in example 2 on the adsorption of heavy metal ions Cd (II);
FIG. 4 is the effect of the adsorption time on the adsorption of heavy metal ions Cd (II) by the adsorbent material in example 3;
FIG. 5 is a graph showing the effect of the initial cadmium concentration on the adsorption of heavy metal ions Cd (II) by the adsorbent material in example 4;
FIG. 6 is a graph showing the effect of pH of the adsorption environment on adsorption of heavy metal ions Cd (II) by the adsorbent material in example 5.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the present invention is not limited to the above-described examples.
Example 1: the method for preparing the adsorbent by using the high-alumina fly ash comprises the following specific steps:
putting 50g of fly ash (Mongolian high-alumina fly ash) and 50g of anhydrous sodium carbonate into a crucible, uniformly mixing, putting the crucible into a box-type resistance furnace, uniformly heating to 900 ℃, reacting at constant temperature for 120min to obtain a sinter, cooling the sinter to room temperature, and grinding into powder; putting 10g of powdery sintering material into a conical flask, adding hydrochloric acid solution with the mass concentration of 18.5%, stirring for 1h under the condition of 90 ℃ water bath, performing suction filtration, washing the filter residue with distilled water until the filter residue is white, collecting and combining filtrate and washing liquid to prepare aluminum-containing solution, adding distilled water and surfactant solution (polyether P123, the concentration of the surfactant solution is 0.03 g/mL) into the aluminum-containing solution, wherein the volume ratio of the distilled water to the aluminum-containing solution is 3:1, the volume ratio of the surfactant solution to the aluminum-containing solution is 1:1, stirring for 10h at 40 ℃, adjusting the pH =7 with sodium hydroxide to generate flocculation and sedimentation, standing for 48h, performing suction filtration, drying the filter residue in an oven at 80 ℃, putting the obtained material into a crucible and a box-type resistance furnace, increasing the temperature to 600 ℃ at the rate of 1 ℃/min, keeping the temperature for 5h, taking out and grinding the material when the furnace temperature is reduced to be below 100 ℃, thus obtaining the adsorbent.
The adsorbent prepared in this example is analyzed by nitrogen-adsorption-desorption isotherm, and the result is shown in fig. 1, and it can be seen from fig. 1 that the adsorbent has typical mesoporous characteristics.
The result of desorption by BJH model of nitrogen-adsorption desorption isotherm is shown in FIG. 2, and from FIG. 2, it can be seen that the average pore diameter of the adsorbent is 7.483 (nm) and the specific surface area is 100.622 (m)2/g）。
The adsorbent of the embodiment is used for treating a heavy metal ion Cd (II) solution at normal temperature, 0.1g, 0.2g, 0.3g and 0.4g of adsorbents are weighed and respectively added into a 50mL cadmium nitrate solution with an initial cadmium ion concentration of 20mg/L, pH =5.5, the filtering is carried out after the adsorption time is 30min, the Cd ion content in the filtrate is detected, and the result is shown in FIG. 3, the Cd ion content is 0.2413mg/L, 0.1478mg/L, 0.0558mg/L and 0.029mg/L, and the adsorption efficiency is respectively 98.8%, 99.26%, 99.72% and 99.86%.
Example 2: the method for preparing the adsorbent by using the high-alumina fly ash comprises the following specific steps:
putting 50g of fly ash (Mongolia high-alumina fly ash) and 30g of anhydrous sodium carbonate into a crucible, uniformly mixing, putting the crucible into a box-type resistance furnace, uniformly heating to 1000 ℃, reacting at constant temperature for 80min to obtain a sinter, cooling the sinter to room temperature, and grinding into powder; putting 10g of powdery sintering material into a conical flask, adding a hydrochloric acid solution with the mass concentration of 15%, sealing by using a preservative film, stirring for 1.5h under the condition of 70 ℃ water bath, performing suction filtration, washing by using distilled water until filter residue is white, collecting and combining filtrate and washing liquid to prepare an aluminum-containing solution, adding distilled water and a surfactant solution (polyether P123, the concentration of the surfactant solution is 0.02 g/mL) into the aluminum-containing solution, wherein the volume ratio of the distilled water to the aluminum-containing solution is 3.5:1, the volume ratio of the surfactant solution to the aluminum-containing solution is 1:2, stirring for 12h at 35 ℃, adjusting the pH value to be 7.5 by using sodium hydroxide, performing flocculation and sedimentation, standing for 55h, performing suction filtration, drying filter residue in a 70 ℃ oven, putting the obtained material into a crucible and a box-type resistance furnace, increasing the temperature to 500 ℃ at the heating rate of 1.5 ℃/min, keeping the temperature in the furnace for 5h, taking out the material after the temperature is reduced to, thus obtaining the adsorbent.
The adsorbent of the embodiment is used for treating a solution containing heavy metal ions Cd (II) at normal temperature, 0.2g of the adsorbent is weighed and added into 50mL of cadmium nitrate solution with the initial cadmium ion concentration of 20mg/L, pH =5.5, the adsorption time is set to be 10min, 20min, 40 min, 60min and 100 min, the filtering is carried out, the content of Cd ions in the filtrate is detected, the result is shown in FIG. 4, the content of Cd ions is respectively 0.0557, 0.0018, 0.0218, 0.0329 and 0.0013, the adsorption efficiency is respectively 99.72%, 99.99%, 99.89%, 99.83% and 99.99%, and the result shows that the adsorbent of the embodiment can be adsorbed to saturation in 10min and can be adsorbed rapidly.
Example 3: the method for preparing the adsorbent by using the high-alumina fly ash comprises the following specific steps:
putting 50g of fly ash (Mongolian high-alumina fly ash) and 60g of anhydrous sodium carbonate into a crucible, uniformly mixing, putting the crucible into a box-type resistance furnace, uniformly heating to 1200 ℃, reacting at constant temperature for 60min to obtain a sinter, cooling the sinter to room temperature, and grinding into powder; putting 10g of powdery sintering material into a conical flask, adding a hydrochloric acid solution with the mass concentration of 25%, sealing by using a preservative film, stirring for 2 hours under the condition of 60 ℃ water bath, performing suction filtration, washing the filter residue by using distilled water until the filter residue is white, collecting and combining filtrate and washing liquid to prepare an aluminum-containing solution, adding distilled water and a surfactant solution (polyether P123, the concentration of the surfactant solution is 0.04 g/mL) into the aluminum-containing solution, adjusting the pH =7 by using sodium hydroxide to perform flocculation and sedimentation, standing for 70 hours, performing suction filtration, drying the filter residue in a 65 ℃ oven, putting the obtained material into a crucible box type resistance furnace, increasing the temperature to 800 ℃ at the rate of 2 ℃/min, keeping the temperature for 5 hours, taking out and grinding the material after the furnace temperature is reduced to below 100 ℃, thus obtaining the adsorbent;
the adsorbent is used for treating a heavy metal ion Cd (II) solution at normal temperature, 0.2g of the adsorbent is weighed and added into 50mL of cadmium nitrate solution with pH =5.5, the concentration of cadmium ions is set to be 5 mg/L, 10 mg/L, 20mg/L, 50mg/L and 100 mg/L, after the adsorption time is 30min, the filtering is carried out, the content of Cd ions in the filtrate is detected, the result is shown in FIG. 5, the content of Cd ions is 0.0681mg/L, 0.1323mg/L, 0.0558mg/L, 0.5864mg/L and 13.726mg/L respectively, the adsorption efficiency is 98.56%, 98.50%, 99.72%, 98.76% and 85.88% respectively, and the result shows that the adsorption effect is very obvious and is more than 98% under the condition that the concentration of cadmium ions is 5-50 mg/L.
The adsorbent is used for treating a Cd (II) solution containing heavy metal ions at normal temperature, 0.2g of the adsorbent is weighed and added into a 50mL cadmium nitrate solution with an initial cadmium ion concentration of 20mg/L, the pH of the cadmium nitrate solution is 2, 4, 6, 8 and 10, the adsorption time is 30min, the cadmium nitrate solution is filtered, the Cd ion content in the filtrate is detected, the result is shown in FIG. 6, the Cd ion contents are 14.6437, 2.1316, 0.0315, 0.1091 and 0.0132 respectively, the adsorption efficiencies are 26.78%, 89.342%, 99.84%, 99.45% and 99.93%, and the result shows that the adsorption effect of the cadmium nitrate solution under weak acid and alkaline conditions (pH = 6-10) is very obvious and is more than 99%.
Claims (7)
1. A method for preparing an adsorbent by using high-alumina fly ash is characterized by comprising the following specific steps:
(1) mixing the high-alumina fly ash and anhydrous sodium carbonate, sintering and activating at 900-1200 ℃ for 60-120 min, cooling and grinding;
(2) acid leaching the ground material at 60-90 ℃ for 1-2 h, performing suction filtration, washing the ground material until filter residue is white, and collecting and combining filtrate and washing liquid to obtain an aluminum-containing solution;
(3) adding distilled water and a surfactant solution into an aluminum-containing solution, stirring for 8-12 h at 30-60 ℃, adjusting the pH value of the solution to 6.5-7.5 to enable the solution to flocculate and settle, standing for 48-72 h, then performing suction filtration, drying filter residues, and calcining at 400-800 ℃ to obtain the adsorbent.
2. The method for preparing the adsorbent by using the high-alumina fly ash according to claim 1, wherein: the mass ratio of the high-alumina fly ash to the anhydrous sodium carbonate is 1: 0.6-1.2.
3. The method for preparing the adsorbent by using the high-alumina fly ash according to claim 1, wherein: the acid leaching uses hydrochloric acid with mass concentration of 5-7 mol/L, and the solid-to-solid ratio of the amount of the hydrochloric acid solution to the activated fly ash solution is 100-150 ml/10 g.
4. The method for preparing the adsorbent by using the high-alumina fly ash according to claim 1, wherein: the volume ratio of the distilled water to the aluminum-containing solution is 3-4: 1.
5. The method for preparing the adsorbent by using the high-alumina fly ash according to claim 4, wherein: the surfactant is polyether P123, the concentration of the surfactant solution is 0.02-0.04 g/mL, and the volume ratio of the surfactant solution to the aluminum-containing solution is 1: 1.6-2.
6. The method for preparing the adsorbent by using the high-alumina fly ash according to claim 5, wherein: heating to 400-800 ℃ at a heating rate of 1-2 ℃/min.
7. The application of the adsorbent prepared by the method for preparing the adsorbent by using the high-alumina fly ash as described in any one of claims 1 to 6 in treating cadmium-containing wastewater.
Priority Applications (1)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114590787A (en) * | 2022-03-16 | 2022-06-07 | 昆明理工大学 | Method for producing aluminum phosphate by using high-alumina fly ash |
| CN116351394A (en) * | 2023-03-13 | 2023-06-30 | 中煤科工清洁能源股份有限公司 | Method for preparing porous adsorption material by utilizing gasified fine ash |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114590787A (en) * | 2022-03-16 | 2022-06-07 | 昆明理工大学 | Method for producing aluminum phosphate by using high-alumina fly ash |
| CN116351394A (en) * | 2023-03-13 | 2023-06-30 | 中煤科工清洁能源股份有限公司 | Method for preparing porous adsorption material by utilizing gasified fine ash |
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