CN114768751B - Lamellar double-metal hydroxide adsorption material based on fly ash, preparation method and application - Google Patents
Lamellar double-metal hydroxide adsorption material based on fly ash, preparation method and application Download PDFInfo
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 57
- 239000010881 fly ash Substances 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 35
- 229910000000 metal hydroxide Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 25
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 25
- 239000010452 phosphate Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 13
- 238000000975 co-precipitation Methods 0.000 claims abstract description 5
- 150000002500 ions Chemical class 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 12
- 239000008346 aqueous phase Substances 0.000 claims description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000011574 phosphorus Substances 0.000 claims description 8
- 229910052698 phosphorus Inorganic materials 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- QQZBCBCKAGTRMT-UHFFFAOYSA-G [OH-].[Ca+2].[Fe+2].[Al+3].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-] Chemical compound [OH-].[Ca+2].[Fe+2].[Al+3].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-] QQZBCBCKAGTRMT-UHFFFAOYSA-G 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 229910021332 silicide Inorganic materials 0.000 claims description 2
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims description 2
- 239000003463 adsorbent Substances 0.000 abstract description 12
- 239000002351 wastewater Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 150000001450 anions Chemical class 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- ULGYAEQHFNJYML-UHFFFAOYSA-N [AlH3].[Ca] Chemical compound [AlH3].[Ca] ULGYAEQHFNJYML-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 abstract 1
- 239000001110 calcium chloride Substances 0.000 abstract 1
- 229910001628 calcium chloride Inorganic materials 0.000 abstract 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical group [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000011575 calcium Substances 0.000 description 21
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- -1 calcium aluminum iron Chemical compound 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
Classifications
-
- 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
- B01J20/0203—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
-
- 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
-
- 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
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a lamellar double-metal hydroxide adsorption material based on fly ash, a preparation method and application thereof, and belongs to the technical field of sewage purification treatment in environmental protection. The calcium-aluminum layered double hydroxide prepared by taking industrial fly ash, calcium chloride and sodium hydroxide as main materials and taking the fly ash as an aluminum source is obtained by a coprecipitation method. The lamellar double metal hydroxide prepared by the method has the characteristics of hydrotalcite structure and high adsorption specific surface area, has good adsorption effect and adsorption selectivity on phosphate, can be subjected to trace treatment, and provides technical reference for adsorption removal of anions in wastewater. The invention has the advantages of common and easily obtained raw materials, low price, simple preparation process, high treatment efficiency and short period, and is an effective adsorbent for treating phosphate in wastewater.
Description
Technical Field
The invention discloses a lamellar double metal hydroxide adsorption material based on fly ash, and preparation and application thereof, and belongs to the field of sewage purification treatment in environmental protection.
Background
The wide application of phosphate fertilizer in agriculture and the discharge of industrial phosphorus-containing wastewater lead to serious eutrophication of water bodies and seriously affect the balance of aquatic ecosystems. According to the world health organization standard, the phosphorus content of the drinking water is not more than 0.5mg/L. At present, the treatment method of phosphate in water mainly comprises a chemical precipitation method, a membrane separation method, an adsorption method and the like. Among them, adsorption is one of the main ways to extract phosphate from wastewater.
Layered Double Hydroxide (LDHs) clay consists of brucite-like sheet hydroxides, divalent metal ions in LDHs are isomorphously substituted by trivalent metal ions to generate positive electricity, and can attract negative ions to become an adsorbing material of anions such as phosphate in water and the like, and the adsorption material is widely focused. At present, most of LDHs are prepared from finished metal salt, which is not beneficial to environmental protection and green recycling of resources.
Fly Ash (FA) produced in the coal-fired power generation process contains high content of silicon dioxide and mullite, so that the fly ash rich in aluminum is an effective source for preparing hydrotalcite-like compounds. In addition, the fly ash has wide sources and low cost, and simultaneously has other active elements such as magnesium and the like, thereby providing possibility for developing the efficient adsorbent.
The invention selects the fly ash as an aluminum source, prepares Ca/(Al-FA) -LDH by a coprecipitation method, and uses the Ca/(Al-FA) -LDH in the treatment of phosphate solution. The invention uses industrial waste FA as the preparation hydrotalcite-like material to adsorb phosphate in wastewater, thereby achieving the effect of treating waste by waste. Meanwhile, the hydrotalcite-like adsorption material prepared by the coprecipitation method has the advantages of a layered structure, large specific surface area and the like, has the characteristic of multiple elements of the fly ash, and provides technical reference for efficient adsorption and selective adsorption of anions in wastewater.
Disclosure of Invention
Aiming at the problems of dust pollution, serious adverse effects on the life of people and the growth of plants and the like caused by the accumulation of a large amount of fly ash which is an industrial waste at present, the invention provides an adsorption material for removing phosphate in water and a preparation method thereof. The invention has the characteristics of large adsorption capacity, high adsorption efficiency, high trace removal rate, short period, low cost, simple preparation process, large-scale application to production and the like.
The technical scheme of the invention is as follows:
a lamellar double metal hydroxide adsorbing material based on fly ash contains 11.2% of nonmetallic silicide and 39.45% of aluminum-calcium-iron hydroxide in a composite state and has lamellar morphology with the stacked thickness of 20-50 nm.
The preparation method of the lamellar double metal hydroxide adsorbing material based on the fly ash comprises the following steps:
(1) Sieving the fly ash with a 80-120 mesh sieve for standby;
(2) Uniformly mixing the fly ash sieved in the step (1) with NaOH particles according to the mass ratio of 1:1.1-1:1.5, grinding, and roasting for 1-1.5 h at the temperature of 500-800 ℃;
(3) CaCl is added with 2 Adding solid particles into the product obtained in the step (2), adding deionized water, and preparing Ca 2+ ：Al 3+ The mixed metal salt solution with the molar ratio of 2-3 is stirred uniformly;
(4) Regulating the pH value of the solution obtained in the step (3) to 9-13 by using NaOH aqueous solution, and stirring for 0.5-5 h;
(5) Sealing the solution obtained in the step (4), aging for 2-24 hours at the temperature of 20-90 ℃, filtering, washing and drying to obtain the Ca/(Al-FA) lamellar double hydroxide adsorbing material.
The lamellar double metal hydroxide adsorbing material obtained by the preparation method is applied to the adsorption of phosphate and comprises the following steps:
(1) Scale adsorption process:
adding Ca/(Al-FA) lamellar double metal hydroxide adsorption material into phosphate-containing aqueous solution, carrying out adsorption operation in a constant-temperature oscillator, and measuring and analyzing the concentration of residual ions in the aqueous phase at regular intervals until the concentration is balanced;
the adsorption quantity Q is calculated by adopting the following method e1 ：
Wherein: q (Q) e1 Mg.g for the adsorption amount of Ca/(Al-FA) lamellar double metal hydroxide adsorption material at equilibrium -1 ；C 01 And C e1 Respectively the initial concentration of ions in the aqueous phase, mg.L -1 And concentration at equilibrium, mg.L -1 The method comprises the steps of carrying out a first treatment on the surface of the m is the mass of the Ca/(Al-FA) lamellar double metal hydroxide adsorption material, g; v (V) 1 Is the volume of the liquid phase, L;
(2) And (3) selecting an adsorption process:
adding Ca/(Al-FA) lamellar double metal hydroxide adsorption material into phosphate aqueous solution containing carbonate, sulfate, nitrate or chloride ions with different concentrations, carrying out adsorption operation in a constant-temperature oscillator, and measuring and analyzing the concentration of residual ions in the aqueous phase at regular intervals until the residual ions are balanced;
the adsorption quantity Q is calculated by adopting the following method e2 ：
Wherein: q (Q) e2 In order to balance the phosphorus adsorption amount of Ca/(Al-FA) lamellar double metal hydroxide adsorption material, mg.g -1 ；C 01 And C e1 Respectively the initial concentration of ions in the aqueous phase, mg.L -1 And concentration at equilibrium, mg.L -1 The method comprises the steps of carrying out a first treatment on the surface of the m is the mass of Ca/(Al-FA) lamellar double-metal hydroxide adsorption material prepared by taking FA as an aluminum source, and g; v (V) 2 Is the volume of the liquid phase, L;
the removal efficiency η is calculated using the following:
wherein: eta is the phosphate removal efficiency of the Ca/(Al-FA) lamellar double metal hydroxide adsorption material at equilibrium,%; c (C) 02 And C e2 Respectively the initial concentration of ions in the aqueous phase, mg.L -1 And concentration at equilibrium, mg.L -1 。
The invention has the beneficial effects that: the invention provides a method for preparing Ca/(Al-FA) -LDH adsorption treatment of phosphate-containing wastewater by adopting FA as an aluminum source. The method adopts coprecipitation operation to obtain flaky Ca/(Al-FA) -LDH with rough surface and high specific surface area, wherein FA is an aluminum source, and the flaky Ca/(Al-FA) -LDH is used for adsorption. Compared with the traditional phosphate adsorption method, the fly ash selected by the invention has wide sources and low price; the hydrotalcite-like compound has simple preparation process and easy operation, and has high adsorption capacity and adsorption selectivity on phosphate by utilizing the characteristic that the layered structure of the hydrotalcite-like compound has electrostatic attraction effect on phosphate in aqueous solution and the characteristic of interlayer ion exchange, and can be used for trace treatment.
Drawings
FIG. 1 is an SEM image of a lamellar double hydroxide prepared with FA as the aluminum source.
FIG. 2 is an EDS diagram of a lamellar double hydroxide prepared with FA as the aluminum source.
FIG. 3 is an XRD pattern of a lamellar double hydroxide prepared with FA as the aluminum source.
Detailed Description
The present invention will be described with reference to specific examples, but the content and practical application of the present invention are not limited thereto.
The preparation method of the lamellar double metal hydroxide adsorbing material based on the fly ash comprises the following steps:
(1) Sieving the fly ash with a 100-mesh sieve, removing larger particles, and reserving powder for standby;
(2) Accurately weighing 1.1979g of the fly ash sieved in the step (1) and 1.547g of NaOH particles, uniformly mixing, grinding, and placing in a muffle furnace for roasting at 600 ℃ for 1.5h;
(3) 2.467g CaCl 2 Adding solid particles into the product obtained in the step (2), adding 200mL of deionized water, and uniformly stirring;
(4) Regulating the pH value of the solution obtained in the step (3) to about 10 by using a 2M NaOH solution, and stirring for 1h;
(5) And (3) sealing the solution obtained in the step (4), placing the solution in an oven, aging for 10 hours at 80 ℃, filtering, washing and drying to obtain the prepared FA synthetic calcium aluminum layered double hydroxide.
The invention is illustrated in detail below with 3 specific experiments:
(1) Accurately weighing 0.04g of Ca/(Al-FA) -LDH prepared by taking FA as an aluminum source, adding into 50mL of aqueous solution with phosphorus concentration of 10mg/L and 40mg/L, oscillating at 30 ℃ for 10 hours, separating at 6000 rpm for 10 minutes, and measuring the phosphorus concentration of the supernatant liquid to be 0.08 mg.L respectively -1 And 0.18 mg.L -1 The adsorption amounts were calculated to be 12 respectively by using the above formulamg/g and 49mg/g, and the quality of the surface water environment can be achieved. The results show that the composite adsorbent has good removal effect under phosphate environments with different concentrations.
(2) The specific surface area of the Ca/(Al-FA) -LDH composite adsorbent prepared by taking FA as an aluminum source is 96m 2 Per gram, pore volume of 0.516cm 3 Per g, far exceeds the specific surface area and pore volume of Ca/Al layered double hydroxide (12 m 2 Per g and 0.052cm 3 The EDS results indicated that the silicon content was 11.2% of the total composite adsorbent.
TABLE 1 EDS results for lamellar double metal hydroxide composite adsorbents
(3) Preparing a solution with the carbonate concentration of 80mg/L from 40mg/L phosphate solution, accurately weighing 0.04g of Ca/(Al-FA) -LDH adsorbent prepared by taking the FA as an aluminum source and 0.02g of single hydrotalcite-like adsorbent, respectively adding the Ca/(Al-FA) -LDH adsorbent and the single hydrotalcite-like adsorbent into 50mL of phosphate solution containing different competitive ions, oscillating at 30 ℃ for 10 hours, separating at 6000 rpm for 10 minutes, measuring the concentration of phosphorus element in supernatant, and calculating the phosphorus removal efficiencies of the Ca/(Al-FA) -LDH adsorbent to be respectively:
TABLE 2 competitive adsorption results of lamellar double metal hydroxide composite adsorbents
Therefore, the FA of the invention is lamellar double metal hydroxide prepared by an aluminum source, and in high carbonate concentration, the selective adsorption capacity of phosphate is improved by about 35%, which mainly depends on flocculation and coordination chelation of calcium aluminum iron and the like in Ca/(Al-FA) -LDH and phosphate.
Claims (2)
1. A preparation method of a lamellar double metal hydroxide adsorbing material based on fly ash is characterized in that the lamellar double metal hydroxide adsorbing material based on fly ash contains 11.2% of nonmetallic silicide and 39.45% of aluminum-calcium-iron hydroxide in a composite state and has a lamellar morphology with a stacking state thickness of 20-50 nm; the specific surface area of the layered double hydroxide adsorption material based on the fly ash is 96m 2 Per gram, pore volume of 0.516cm 3 /g; ca/(Al-FA) -LDH was prepared by the coprecipitation method as follows:
(1) Sieving the fly ash with a 80-120 mesh sieve for standby;
(2) Uniformly mixing the fly ash sieved in the step (1) with NaOH particles according to the mass ratio of 1:1.1-1:1.5, grinding, and roasting for 1-1.5 h at the temperature of 500-800 ℃;
(3) CaCl is added with 2 Adding solid particles into the product obtained in the step (2), adding deionized water, and preparing Ca 2+ ：Al 3+ The mixed metal salt solution with the molar ratio of 2-3 is stirred uniformly;
(4) Regulating the pH value of the solution obtained in the step (3) to 9-13 by using NaOH aqueous solution, and stirring for 0.5-5 h;
(5) Sealing the solution obtained in the step (4), aging for 2-24 hours at the temperature of 20-90 ℃, filtering, washing and drying to obtain the lamellar double hydroxide adsorbing material.
2. The use of the lamellar bimetal hydroxide adsorbing material obtained by the preparation method as claimed in claim 1, characterized in that the lamellar bimetal hydroxide adsorbing material adsorbs phosphate, and the steps are as follows:
(1) Scale adsorption process:
adding lamellar double metal hydroxide adsorption material into aqueous solution containing phosphate, performing adsorption operation in a constant temperature oscillator, and measuring and analyzing the concentration of residual ions in the aqueous phase at regular intervals until balance;
the adsorption quantity Q is calculated by adopting the following method e1 ：
Wherein: q (Q) e1 Mg.g for balancing the adsorption quantity of lamellar double metal hydroxide adsorption material -1 ；C 01 And C e1 Respectively the initial concentration of ions in the aqueous phase, mg.L -1 And concentration at equilibrium, mg.L -1 The method comprises the steps of carrying out a first treatment on the surface of the m is the mass of the lamellar double metal hydroxide adsorption material and g; v (V) 1 Is the volume of the liquid phase, L;
(2) And (3) selecting an adsorption process:
adding lamellar double metal hydroxide adsorption material into phosphate aqueous solution containing carbonate, sulfate, nitrate or chloride ions with different concentrations, performing adsorption operation in a constant-temperature oscillator, and measuring and analyzing the concentration of residual ions in the aqueous phase at regular intervals until the residual ions are balanced;
the adsorption quantity Q is calculated by adopting the following method e2 ：
Wherein: q (Q) e2 In order to balance the phosphorus adsorption amount of lamellar double metal hydroxide adsorption material, mg.g -1 ；C 01 And C e1 Respectively the initial concentration of ions in the aqueous phase, mg.L -1 And concentration at equilibrium, mg.L -1 The method comprises the steps of carrying out a first treatment on the surface of the m is the mass of the lamellar double metal hydroxide adsorption material prepared by taking FA as an aluminum source, and g; v (V) 2 Is the volume of the liquid phase, L;
the removal efficiency η is calculated using the following:
wherein: η is the phosphate removal efficiency of the lamellar bimetallic hydroxide adsorption material at equilibrium,%; c (C) 02 And C e2 Respectively the initial concentration of ions in the aqueous phase, mg.L -1 And balance ofTime concentration, mg.L -1 。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202210323129.0A CN114768751B (en) | 2022-03-30 | 2022-03-30 | Lamellar double-metal hydroxide adsorption material based on fly ash, preparation method and application |
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| CN116422286A (en) * | 2023-04-10 | 2023-07-14 | 浙江工业大学 | Method for preparing zinc-iron-loaded double-metal hydroxide phosphorus-philic adsorbent by utilizing sludge ash and application of zinc-iron-loaded double-metal hydroxide phosphorus-philic adsorbent |
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