CN114768752A - Fly ash loaded hydrotalcite-like compound composite adsorbent, preparation method and application - Google Patents
Fly ash loaded hydrotalcite-like compound composite adsorbent, preparation method and application Download PDFInfo
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- CN114768752A CN114768752A CN202210323745.6A CN202210323745A CN114768752A CN 114768752 A CN114768752 A CN 114768752A CN 202210323745 A CN202210323745 A CN 202210323745A CN 114768752 A CN114768752 A CN 114768752A
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0251—Compounds of Si, Ge, Sn, Pb
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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
- B01J20/04—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
- B01J20/041—Oxides or hydroxides
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- 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
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- 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
- C02F2101/105—Phosphorus compounds
Abstract
The invention discloses a fly ash loaded hydrotalcite-like compound composite adsorbent, a preparation method and application, and belongs to the technical field of sewage purification treatment in environmental protection. The composite adsorbent of the fly ash loaded hydrotalcite-like compound is obtained by taking fly ash, calcium chloride, aluminum chloride and sodium hydroxide as main materials and adopting a coprecipitation method. The composite adsorbent prepared by the method has good adsorption selectivity and trace treatment performance on phosphate, and has larger adsorption capacity. The composite adsorbing material prepared by the invention has the advantages of large specific surface area and the like, and provides technical reference for adsorption removal of anions in wastewater. The invention has the advantages of wide source of required raw materials, low price, simple preparation process, high treatment efficiency and short period, and is an effective adsorbent for selectively treating phosphate in wastewater.
Description
Technical Field
The invention discloses a fly ash loaded hydrotalcite-like compound composite adsorbent, a preparation method and application, and belongs to the field of sewage purification treatment in environmental protection.
Background
Excessive nutrient elements (particularly phosphorus and nitrogen) in the water accelerate water system eutrophication, and cause the excessive propagation of harmful algae in the world, so that the dissolved oxygen in the water is reduced, the growth and the multiplication of water system organisms are damaged, and the water system ecology is seriously threatened and even irreversibly damaged. Effective control and reduction of environmental phosphorus accumulation are important components of water eutrophication management, and adjustment of total phosphorus concentration is an effective method.
With the improvement of environmental protection standards, the requirements on phosphorus emission are more and more strict, and the existing phosphorus removal technology also needs to be improved. The benefit and disadvantage analysis of the phosphorus removal method in the sewage treatment by writing the niuhua red clearly indicates that for low-concentration phosphorus-containing wastewater, a large amount of metal materials are required to be used for ensuring the separation effect by a chemical precipitation method, and the method is more suitable for treating the high-concentration phosphorus-containing wastewater in consideration of economic applicability. And the influence of the reactor configuration on the granulation of the biological phosphorus removal sludge under the action of the macromolecular organic matters researched by quality change shows that the biological phosphorus removal process is suitable for the treatment of trace phosphorus in a water body, but the process is complex, the conditions are harsh, and the applicability is limited. The adsorption separation technology has the characteristics of economy, environmental protection and convenient process, and is suitable for treating complex water systems.
The adsorbent used for treating the phosphorus-containing wastewater is widely concerned, and the adsorption effect is different due to system difference. However, the existing adsorbents have low selectivity to phosphate, which affects phosphorus separation performance. The phosphorus adsorbent with high adsorption capacity and high selectivity can reduce the dosage of the adsorbent, ensure high-purity recovery of phosphorus, provide possibility for recycling of phosphorus sources and provide possibility for recovery of trace phosphorus in water bodies. However, current phosphate removal studies indicate that selective separation in low concentration phosphate water bodies in the presence of large amounts of competing anions is extremely challenging.
The invention selects fly ash as a carrier, prepares a fly ash loaded hydrotalcite-like compound composite adsorbent by a coprecipitation method, and is used for adsorption treatment of low-concentration phosphorus-containing wastewater. The adsorption system obtained by the invention improves the removal effect of phosphate in the anion water body, can improve the selective separation of phosphate without changing the pH value of the water body, has the advantages of large specific surface area and the like, and provides technical reference for the adsorption removal of phosphate in wastewater.
Disclosure of Invention
The invention provides an adsorbing material for removing phosphate in water and a preparation method thereof, aiming at the problem of poor phosphate separation selectivity in a water carbonate competitive storage environment. The invention has the characteristics of large adsorption capacity, high adsorption efficiency, high adsorption selectivity, short period, low cost, simple preparation process, large-scale application in production and the like.
The technical scheme of the invention is realized as follows:
a coal ash loaded hydrotalcite-like compound composite adsorbent is mainly formed by compounding porous microspheres with the particle size of 2-20 mu m and thin slices with the particle size of 20-90 nm, wherein the composite adsorbent contains 15.03% of non-metallic silicide and 30.45% of aluminum calcium iron hydroxide.
A preparation method of a fly ash loaded hydrotalcite-like compound composite adsorbent comprises the following steps:
(1) sieving the fly ash by a sieve of 80-120 meshes for later use;
(2) CaCl with the molar ratio of 2: 1-3: 12Particles and AlCl3Adding deionized water into the powder, and uniformly stirring to obtain a mixed metal salt solution;
(3) the amount of the surfactant is 0.1 to 2 mol.L-1Aqueous NaOH solution;
(4) slowly titrating the NaOH aqueous solution prepared in the step (3) into the mixed metal salt solution obtained in the step (2), adjusting the pH value to 9-13, and stirring for 0.5-5 h;
(5) uniformly dispersing the fly ash obtained in the step (1) into the solution obtained in the step (4), wherein the addition amount of the fly ash is not more than 40% of the total mass of the hydrotalcite formed in the mixed metal salt solution in the step (4), and mixing and stirring for 0.5-4 h;
(6) sealing the solution obtained in the step (5), aging for 2-24 h at 20-90 ℃, filtering, washing and drying to obtain the fly ash loaded water-soluble lubricantA stone composite adsorbent. The specific surface area of the fly ash-loaded hydrotalcite-like compound composite adsorbent is 23m2Per g, pore volume 0.148cm3Higher than the Ca/Al layered double hydroxide specific surface area and pore volume (12 m)2G and 0.052cm3And/g) is beneficial to the high-efficiency adsorption of the composite adsorbent.
The fly ash loaded hydrotalcite-like compound composite adsorbent produced by the method is used for carrying out a phosphate adsorption experiment, and the steps are as follows:
(1) and (3) selective adsorption process:
adding the fly ash loaded hydrotalcite-like compound composite adsorbent into a phosphate aqueous solution containing carbonate, sulfate, nitrate or chloride ions, carrying out adsorption operation in a constant-temperature oscillator, and measuring and analyzing the concentration of residual ions in an aqueous phase at regular intervals until the residual ions are balanced;
the adsorption quantity Q was calculated by the following formulae1：
In the formula: qe1The adsorption amount of the composite adsorbent in mg. g is balanced-1；C01And Ce1Respectively the initial concentration of ions in the water phase, mg.L-1And concentration at equilibrium, mg.L-1(ii) a m is the mass of the added composite adsorbent, g; v1Volume of liquid phase, L;
(2) scale adsorption process:
adding the fly ash loaded hydrotalcite-like compound composite adsorbent into phosphate aqueous solutions with different concentrations, carrying out adsorption operation in a constant-temperature oscillator, and measuring and analyzing the concentration of residual ions in an aqueous phase at regular intervals until the residual ions are balanced;
the adsorption quantity Q was calculated by the following formulae2：
In the formula: qe2To balanceAmount of adsorbed phosphorus in mg. g-1；C02And Ce2Respectively the initial concentration of ions in the water phase, mg.L-1And concentration at equilibrium, mg.L-1(ii) a m is the mass of the added composite adsorbent, g; v2Volume of liquid phase, L;
(3) by comparing Q in step (1) with Q in step (2)eAnd (4) obtaining the adsorption selectivity of the adsorbent to the phosphate.
The invention has the beneficial effects that: the invention provides a method for treating phosphate-containing wastewater by adopting a composite adsorbent of fly ash-supported hydrotalcite-like compound, and the adsorption specific surface area of FA-supported hydrotalcite-like compound is about 2 times of that of single Ca/Al layered double hydroxide through coprecipitation, and the adsorption selectivity is provided. Compared with the traditional phosphate adsorption method, the fly ash selected by the invention has wide sources and low cost, and particularly has specific adsorption on phosphate with high carbonate concentration; the FA-loaded hydrotalcite-like composite adsorbent has a higher specific surface area and a more uniform size, has higher adsorption capacity on phosphate in an aqueous solution by utilizing the specific adsorption of the fly ash and the layered structure of the hydrotalcite-like compound, and can be used for trace treatment of the phosphate in a complex water environment.
Drawings
FIG. 1 is SEM image of composite hydrotalcite-like adsorbent with FA as carrier.
FIG. 2 is EDS diagram of composite hydrotalcite-like adsorbent using FA as carrier.
Detailed Description
The present invention will be described below with reference to specific examples, but the contents and effects of the present invention are not limited thereto.
A composite hydrotalcite-like adsorption material with FA as a carrier (the FA doping amount is less than 40%) is prepared by the following steps:
(1) accurately weighing 2.467gCaCl2Granules and 1.480g AlCl3Adding 100mL of deionized water into the powder, and uniformly stirring;
(2) accurately weighing 2.664g of NaOH particles, adding 100mL of deionized water, and uniformly stirring;
(3) slowly titrating the alkali liquor prepared in the step (2) into the mixed metal salt solution obtained in the step (1), adjusting the pH value to about 9, and stirring for 1 h;
(4) after the fly ash is sieved by a 100-mesh sieve, accurately weighing 0.8g of fly ash, adding the fly ash into the solution obtained in the step (3), and uniformly stirring;
(5) and (5) sealing the solution obtained in the step (4), placing the solution in an oven, aging the solution for 10 hours at the temperature of 80 ℃, filtering, washing and drying the solution to obtain the prepared Ca/Al-LDH @ FA composite adsorbent, and recording the Ca/Al-LDH @ FA as Ca/LDH @ FA.
A composite hydrotalcite-like adsorption material with FA as a carrier (the FA doping amount is more than 40%) is prepared by the following steps:
(1) accurately weighing 2.467gCaCl2Granules and 1.480g AlCl3Adding 100mL of deionized water into the powder, and uniformly stirring;
(2) accurately weighing 2.664g of NaOH particles, adding 100mL of deionized water, and uniformly stirring;
(3) slowly titrating the alkali liquor prepared in the step (2) into the mixed metal salt solution obtained in the step (1), adjusting the pH value to about 9, and stirring for 1 h;
(4) sieving the fly ash with a 100-mesh sieve, accurately weighing 2g of the fly ash, adding the fly ash into the solution obtained in the step (3), and uniformly stirring;
(5) and (3) sealing the solution obtained in the step (4), aging the solution in an oven at 80 ℃ for 10 hours, filtering, washing and drying the solution to obtain the prepared Ca/Al-LDH @ FA composite adsorbent, which is recorded as Ca/Al-LDH @ FA 2.
The invention is illustrated in detail below with 4 specific experiments:
(1) preparing mixed solution with carbonate concentration of 80mg/L from 40mg/L phosphate solution, accurately weighing 0.02g of the prepared composite hydrotalcite-like adsorbent Ca/Al-LDH @ FA1 with FA as a carrier and a single hydrotalcite-like adsorbent, respectively adding into 50mL of phosphate solution containing different competitive ions, oscillating at 30 ℃ for 10 hours, performing 6000 r/min separation for 10 minutes, measuring the phosphorus element concentration of the supernatant, and calculating the phosphorus adsorption capacity (in mg. g.) by using the formula-1)：
TABLE 1 competitive adsorption results of adsorbents
The application result proves that the effect of selectively adsorbing phosphate by the Ca/Al-LDH @ FA composite adsorbent is improved by nearly 23% in a high-concentration carbonate environment, and the composite adsorbent has the performance of selectively separating phosphate and has application potential.
(2) Accurately weighing 0.02g of the prepared Ca/Al-LDH @ FA1 composite adsorbent, respectively adding into 50mL of aqueous solution with the phosphorus element concentration of 10mg/L and 40mg/L, oscillating at 30 ℃ for 10 hours, performing 6000 r/separation centrifugation for 10 minutes, and measuring the phosphorus element concentration of the supernatant to be 0.11 mg.L-1And 0.37 mg. L-1The adsorption amounts calculated by the formula are respectively 24mg/g and 98mg/g, so that the environmental quality standard of surface water is met, and the composite adsorbent has a good adsorption effect on low-concentration phosphate.
(3) Accurately weighing 0.02g of the prepared Ca/Al-LDH @ FA1 and Ca/Al-LDH @ FA2, respectively adding into 50mL of aqueous solution with the phosphorus element concentration of 40mg/L, oscillating for 10 hours at 30 ℃, centrifuging for 10 minutes at 6000 rpm/separation, and measuring the phosphorus element concentrations of the supernatant to be 0.37 mg.L-1And 15.56 mg. L-1The adsorption amounts of the composite adsorbent are respectively 98mg/g and 61mg/g calculated by the formula, and the adsorption performance of the adsorbent is influenced by the excessive FA addition in the composite adsorbent.
(4) The specific surface area of the Ca/Al-LDH @ FA composite adsorbent prepared by the method is 23m2Per g, pore volume 0.148cm3G, far exceeding the specific surface area and pore volume of the Ca/Al layered double hydroxide (12 m)2G and 0.052cm3In terms of/g), EDS results show that the silicon content is 11.2% of the total composite adsorbent. The TGA test result shows that the weight loss of the compound is about 30 percent within 1000 ℃, which indicates that the composite adsorbent has good stability.
Claims (4)
1. The coal ash loaded hydrotalcite-like compound composite adsorbent is characterized by being mainly formed by compounding porous microspheres with the particle size of 2-20 mu m and thin sheets with the particle size of 20-90 nm, and is in a composite state containing 15.03% of non-metal silicide and 30.45% of aluminum, calcium and iron hydroxide.
2. The method for preparing the composite adsorbent according to claim 1, characterized by comprising the steps of:
(1) sieving the fly ash by a sieve of 80-120 meshes for later use;
(2) CaCl with the molar ratio of 2: 1-3: 12Particles and AlCl3Adding deionized water into the powder, and uniformly stirring to obtain a mixed metal salt solution;
(3) the amount of the surfactant is 0.1 to 2 mol/L-1Aqueous NaOH solution;
(4) slowly titrating the NaOH aqueous solution prepared in the step (3) into the mixed metal salt solution obtained in the step (2), adjusting the pH value to 9-13, and stirring for 0.5-5 h;
(5) uniformly dispersing the fly ash obtained in the step (1) into the solution obtained in the step (4), and mixing and stirring for 0.5-4 h;
(6) and (4) sealing the solution obtained in the step (5), aging for 2-24 h at 20-90 ℃, filtering, washing and drying to obtain the fly ash loaded hydrotalcite-like compound adsorbent.
3. The method according to claim 2, wherein the fly ash is used in an amount of not more than 40% by mass based on the total mass of the hydrotalcite-like compound in the mixed metal salt solution in step (4).
4. The application of the fly ash loaded hydrotalcite-like compound composite adsorbent prepared by the preparation method of claims 2-3 is characterized in that the fly ash loaded hydrotalcite-like compound composite adsorbent is used for selectively adsorbing phosphate and carrying out scale adsorption, and the steps are as follows:
(1) and (3) selective adsorption process:
adding the fly ash loaded hydrotalcite-like compound composite adsorbent into a phosphate aqueous solution containing carbonate, sulfate, nitrate or chloride ions, carrying out adsorption operation in a constant-temperature oscillator, and measuring and analyzing the concentration of residual ions in an aqueous phase at regular intervals until the residual ions are balanced;
the adsorption quantity Q was calculated by the following formulae1：
In the formula: qe1The adsorption amount of the composite adsorbent in mg. g is balanced-1；C01And Ce1Respectively the initial concentration of ions in the water phase, mg.L-1And concentration at equilibrium, mg.L-1(ii) a m is the mass of the added composite adsorbent, g; v1Volume of liquid phase, L;
(2) scale adsorption process:
adding the fly ash loaded hydrotalcite-like compound composite adsorbent into phosphate aqueous solutions with different concentrations, carrying out adsorption operation in a constant-temperature oscillator, and measuring and analyzing the concentration of residual ions in an aqueous phase at regular intervals until the residual ions are balanced;
the adsorption quantity Q was calculated by the following formulae2：
In the formula: qe2Mg.g as the amount of phosphorus adsorbed at equilibrium-1；C02And Ce2Respectively the initial concentration of ions in the water phase, mg.L-1And concentration at equilibrium, mg.L-1(ii) a m is the mass of the added composite adsorbent, g; v2Volume of liquid phase, L;
(3) by comparing Q in step (1) with Q in step (2)eAnd obtaining the adsorption selectivity of the adsorbent to phosphate.
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Cited By (2)
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| CN115999518A (en) * | 2022-12-27 | 2023-04-25 | 昆明理工大学 | Preparation and application methods of adsorbent for removing phosphate |
| CN116395728A (en) * | 2023-03-24 | 2023-07-07 | 中国矿业大学 | Preparation method of fly ash-based hydrotalcite-like compound, and product and application thereof |
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| CN116395728A (en) * | 2023-03-24 | 2023-07-07 | 中国矿业大学 | Preparation method of fly ash-based hydrotalcite-like compound, and product and application thereof |
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