CN114405456B - Gamma-Fe for uranium removal 2 O 3 Preparation method of @ HAP magnetic composite material - Google Patents
Gamma-Fe for uranium removal 2 O 3 Preparation method of @ HAP magnetic composite material Download PDFInfo
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- CN114405456B CN114405456B CN202210063921.7A CN202210063921A CN114405456B CN 114405456 B CN114405456 B CN 114405456B CN 202210063921 A CN202210063921 A CN 202210063921A CN 114405456 B CN114405456 B CN 114405456B
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- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 46
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims description 14
- 229910001566 austenite Inorganic materials 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000001179 sorption measurement Methods 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- 239000003463 adsorbent Substances 0.000 description 11
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 11
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 239000011575 calcium Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002901 radioactive waste Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- -1 uranyl ions Chemical class 0.000 description 2
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 231100000783 metal toxicity Toxicity 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002915 spent fuel radioactive waste Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 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
- B01J20/0274—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 characterised by the type of anion
- B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
-
- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
-
- 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
- C02F2101/006—Radioactive compounds
Abstract
The invention discloses gamma-Fe for uranium removal 2 O 3 A method of preparing a HAP magnetic composite, the method comprising the steps of: step 1, weighing gamma-Fe 2 O 3 Dispersing in glycol, and adding deionized water to obtain solution A; step 2, weighing Ca (NO 3 ) 2 ·4H 2 O is dissolved in deionized water to obtain solution B; step 3, mixing the solution A with the solution B, and regulating the pH to 10-12 to obtain a solution C; step 4, weighing (NH 4 ) 2 HPO 4 Dissolving in deionized water, and dripping into the solution C by using a burette; step 5, placing the mixture in an oil bath at 80-100 ℃ for 3-5 h, and aging overnight; step 6, solid-liquid separation is carried out to obtain solid, and gamma-Fe is obtained 2 O 3 @ HAP composite. The composite material is applied to enrichment recovery of uranium, is easy to synthesize, has an efficient uranium removal effect, and can be magnetically recovered and reused.
Description
Technical Field
The invention relates to the technical field of new material preparation, in particular to gamma-Fe for uranium removal 2 O 3 Preparation method of HAP magnetic composite material.
Background
In recent years, the rapid development of nuclear power and the large-scale development and application of nuclear energy promote the mass use of uranium resources. During uranium mining, nuclear fuel processing, nuclear power generation and spent fuel post-treatment, significant amounts of uranium-containing radioactive waste are produced. Uranium has radioactivity, heavy metal toxicity and high mobility, cannot be biodegraded after entering an ecological environment, and can cause serious threat to the ecological environment and human health. The radioactive waste must be treated effectively, with the treatment of uranium-containing wastewater being an important part of the radioactive waste treatment. The traditional uranium-containing wastewater treatment process has the defects of high price, easy pollution, high energy consumption and the like, and how to treat the uranium-containing wastewater efficiently and cheaply is a scientific problem to be solved currently.
The traditional methods for treating the wastewater polluted by radioactive elements are numerous, and mainly comprise a coagulating sedimentation method, an evaporation concentration method, an adsorption method, a chemical percolation method, an extraction method, a reverse osmosis method, a membrane separation method, electrodialysis, reverse osmosis and other treatment methods. Adsorption methods represented by adsorption materials such as natural minerals, carbon-based materials, and nanomaterials have been widely used for the treatment of uranium-containing wastewater because of their advantages such as low cost, high efficiency, and low environmental pollution. Among the numerous adsorption materials, hydroxyapatite is widely used for uranium removal due to its advantages of being non-toxic, inexpensive, widely available, easy to prepare, etc. The hydroxylapatite material synthesized by the prior art has good effect on the adsorption of uranyl ions, but the preparation process of the adsorbent or the remover is complex, and some of the hydroxylapatite material needs to be pretreated by adjusting the pH of wastewater, and some of the hydroxylapatite material has high investment cost, and the hydroxylapatite material synthesized by the prior art cannot be recycled, so that the disposal problem of the adsorbed material and the secondary pollution problem of the environment are not considered.
Disclosure of Invention
In order to solve the problem of unified treatment of recycled materials after uranium acyl ions are adsorbed, the invention provides a gamma-Fe 2 O 3 Process for the preparation of HAP magnetic composites and use of the composites as uranium-depleted adsorbents.
The aim of the invention is realized by adopting the following technical scheme:
the preparation method of the gamma-Fe2O3@HAP magnetic composite material for uranium removal comprises the following steps:
step 1, weighing gamma-Fe 2 O 3 Dispersing in glycol, adding deionized water, and stirring to obtain solution A;
step 2, weighing Ca (NO 3 ) 2 ·4H 2 O is dissolved in deionized water and stirred uniformly to obtain solution B;
step 3, mixing the solution A and the solution B, uniformly stirring, and then adjusting the pH to 10-12 to obtain a solution C;
step 4, weighing (NH 4 ) 2 HPO 4 Dissolving in deionized water, stirring uniformly, and dripping into the solution C by using a burette to obtain a solution D;
step 5, placing the solution D in an oil bath at 80-100 ℃ for 3-5 hours, naturally cooling to room temperature, and aging overnight to obtain a solution E;
step 6, solid-liquid separation is carried out on the solution E to obtain solid, and the solid is washed and dried in sequence to obtain gamma-Fe 2 O 3 @ HAP composite.
Preferably, in the step 1, γ -Fe 2 O 3 The mass ratio of the ethylene glycol to the deionized water is 0.5392:30, and the volume ratio of the ethylene glycol to the deionized water is 2:3.
More preferably, in the step 1, γ -Fe 2 O 3 The amount of the substance was 3.37mmol.
Preferably, in the step 2, ca (NO 3 ) 2 ·4H 2 The mass ratio of O to deionized water was 7.9583:100.
More preferably, in the step 2, ca (NO 3 ) 2 ·4H 2 The amount of O was 33.7mmol.
Preferably, the step 1 is performed by gamma-Fe 2 O 3 And Ca (NO 3 ) 2 ·4H 2 The mass ratio of O was 1:10.
Preferably, in the step 3, the volume ratio of the solution a to the solution B is 1:2.
Preferably, in the step 3, the pH is adjusted to 11 using a diluted ammonia solution.
Preferably, in said step 4, (NH 4 ) 2 HPO 4 The mass ratio of the deionized water to the deionized water is 2.6412:50.
More preferably, in said step 4, (NH 4 ) 2 HPO 4 The amount of the substance was 20mmol.
Preferably, in the step 5, the aging time is 8-12 hours.
Preferably, in the step 6, the washing is sequentially performed by deionized water and absolute ethyl alcohol, and the drying is performed in vacuum at 60 ℃ for 12 hours.
The beneficial effects of the invention are as follows:
1. the invention prepares the magnetic adsorption material which can synthesize, conveniently and efficiently remove uranium, is easy to recycle, and has important significance for enrichment and recycling of uranium and efficient separation of the adsorption material. By chemical precipitation as gamma-Fe 2 O 3 Raw materials of calcium nitrate and diammonium hydrogen phosphate, and one-step synthesis of gamma-Fe 2 O 3 @ HAP. The removal rate and adsorption capacity of the synthesized material to uranium are far higher than those of pure gamma-Fe 2 O 3 And hydroxyapatite, and solves the problem that nano HAP is difficult to thoroughly recover after being adsorbed.
2. The preparation method for preparing the uranium adsorption material is simple, convenient to operate and good in reproducibility.
3. The invention uses gamma-Fe 2 O 3 The composite material synthesized with the hydroxyapatite has good environmental compatibility, magnetism and convenient recovery.
4. The uranium adsorption material prepared by the invention has very excellent propertiesThe purifying effect is characterized by fast adsorption speed, high adsorption capacity, and the adsorption performance of the composite material is higher than that of gamma-Fe 2 O 3 And the hydroxyapatite monomer are improved.
5. The uranium adsorption material prepared by the invention is beneficial to developing a novel advanced adsorbent for radionuclide pollution removal.
Drawings
The invention will be further described with reference to the accompanying drawings, in which embodiments do not constitute any limitation of the invention, and other drawings can be obtained by one of ordinary skill in the art without inventive effort from the following drawings.
FIG. 1 shows γ -Fe prepared in example 1 2 O 3 Relationship between adsorption capacity and adsorption time of uranium by the @ HAP magnetic composite material;
FIG. 2 is a gamma-Fe prepared in example 1 2 O 3 Adsorption capacity diagram of uranium with different concentrations of HAP magnetic composite material.
Detailed Description
The technical features, objects and advantages of the present invention will be more clearly understood from the following detailed description of the technical aspects of the present invention, but should not be construed as limiting the scope of the invention.
In order to solve the problem of unified recovery treatment of the adsorbed material, the invention is based on the research of the magnetic composite material of the hydroxyapatite, and adopts a magnetic adsorbent as a novel adsorbent to solve the problem of rapid recovery of the material after adsorption. The magnetic core is added in the preparation process of the composite material, so that the adsorbent and the magnetic core are combined into the nano-scale composite material, and the magnetic adsorbent has the characteristics of large specific surface area, high adsorption efficiency, recycling, low cost and the like. In addition, the magnetic adsorption separation technology has the characteristics of simple operation, high operation efficiency, mature process and the like, has high separation efficiency, and can realize quick recovery.
The prior invention uses Fe more 3 O 4 As the magnetic core of the adsorption material, to achieve the effect of magnetic separation, but Fe 3 O 4 Contains ferrous iron and ferric iron, has thermodynamic instability, and can be slowly oxidized into maghemite (gamma-Fe) under the condition of oxygen at room temperature 2 O 3 ) And the material is easy to oxidize and lose magnetism in an acidic environment, so that the risk of oxidization exists, and the stable existence of the material is not facilitated. Fe (Fe) 2 O 3 Ratio of Fe 3 O 4 More stable and has two lattices of alpha and gamma, and the research of the invention shows that the alpha-Fe 2 O 3 Exhibits extremely weak magnetic properties, while gamma-Fe 2 O 3 The nano particles show superparamagnetism and are also commonly used as environmental functional materials, and have the characteristics of strong adsorption capacity, no toxicity, low cost, good environmental compatibility, no secondary pollution and the like. Thus will be gamma-Fe 2 O 3 The magnetic hydroxyapatite formed by compositing with the hydroxyapatite has great potential in the application of uranium adsorption field, and the problem of material treatment after adsorption can be solved.
The invention is further described with reference to figures 1-2, and the following examples.
Examples
The preparation method of the gamma-Fe2O3@HAP magnetic composite material for uranium removal comprises the following steps:
step 1, weighing 0.5392g of gamma-Fe 2 O 3 Dispersing in 20mL of glycol, adding 30mL of water, and stirring uniformly to form a magnetic suspension solution A;
step 2, 7.9583g (33.7 mmol) of Ca (NO) 3 ) 2 ·4H 2 O is dissolved in 100mL of deionized water and stirred uniformly to form solution B;
step 3, mixing the magnetic suspension solution A and the solution B, uniformly stirring, and then adjusting the pH value to 11 by using a diluted ammonia solution;
step 4, weighing 2.6412g (20 mmol) of (NH 4 ) 2 HPO 4 Dissolving in 50mL of deionized water, uniformly stirring, and then dropwise adding into the mixed solution prepared in the step 3 by using a burette;
step 5, the mixed solution prepared in the step 4 is subjected to oil bath at 90 ℃ for 4 hours, and is taken out and aged for one night;
step 6, obtaining solid through solid-liquid separationWashing the body with deionized water and absolute ethanol for several times, and drying at 60deg.C under vacuum for 12 hr to obtain final gamma-Fe 2 O 3 Sample of HAP composite.
Application (detection) example 1
Gamma-Fe prepared in example 1 2 O 3 The method for measuring the relationship between uranium adsorption performance and adsorption time by using the @ HAP composite material as a sample comprises the following steps:
step 1, 50mL of uranium solution with initial concentration of 50mg/L is prepared, and the solution ph=4 is adjusted.
Step 2, adding 0.0125g of the adsorbent prepared in the example 1 into the solution in the step 1, oscillating at room temperature for reaction, sampling at different moments, and filtering a water sample for later use.
And 3, detecting the uranium concentration in the water sample obtained in the step 2 by using a spectrophotometry method, and calculating the adsorption capacity of the adsorbent under different equilibrium concentrations. The results are shown in FIG. 1.
The detection result of this embodiment is: gamma-Fe prepared in example 1 2 O 3 The adsorption of the @ HAP composite material to uranium can reach 93.16% within 15min, and reach equilibrium within 30min, the removal rate reaches 98.84%, and the adsorption capacity reaches 232.24mg/g.
Application (detection) example 2
Gamma-Fe prepared in example 1 2 O 3 The @ HAP composite material is used as a sample to determine the adsorption capacity under uranium with different concentrations, and comprises the following steps:
step 1, uranium solutions were prepared at concentration gradients of 30, 50, 80, 100, 200, 300 and 500mg/L, 50mL each for an initial concentration ph=4.
Step 2, adding 0.0125g of the adsorbent prepared in the example 1 into the solution in the step 1 respectively, oscillating at room temperature for reaction, sampling after the reaction reaches equilibrium, and filtering a water sample for later use.
And 3, detecting the uranium concentration in the water sample obtained in the step 2 by using a spectrophotometry method, and calculating the adsorption capacity of the adsorbent under different equilibrium concentrations. The results are shown in FIG. 2.
The detection result of this embodiment is: gamma-Fe prepared in example 1 2 O 3 The adsorption capacity of the @ HAP composite material to uranium can reach 425.47mg/g at maximum.
In other embodiments, the technical effects of the present invention can be achieved by selecting other specific components, proportions and process parameters within the ranges of the components, proportions and process parameters described in the present invention, so they are not listed one by one.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. Gamma-Fe for uranium removal 2 O 3 The preparation method of the HAP magnetic composite material is characterized by comprising the following steps:
step 1, weighing gamma-Fe 2 O 3 Dispersing in glycol, adding deionized water, and stirring to obtain solution A;
step 2, weighing Ca (NO 3 ) 2 ·4H 2 O is dissolved in deionized water and stirred uniformly to obtain solution B;
step 3, mixing the solution A and the solution B, uniformly stirring, and then adjusting the pH to 10-12 to obtain a solution C;
step 4, weighing (NH 4 ) 2 HPO 4 Dissolving in deionized water, stirring uniformly, and dripping into the solution C by using a burette to obtain a solution D;
step 5, placing the solution D in an oil bath at 80-100 ℃ for 3-5 hours, naturally cooling to room temperature, and aging overnight to obtain a solution E;
step 6, solid-liquid separation is carried out on the solution E to obtain solid, and the solid is washed and dried in sequence to obtain gamma-Fe 2 O 3 HAP composite;
gamma-Fe in the step 1 2 O 3 And Ca (NO 3 ) 2 ·4H 2 The mass ratio of O was 1:10.
2. gamma-Fe for uranium removal as claimed in claim 1 2 O 3 A method for preparing HAP magnetic composite material is characterized in that in the step 1, gamma-Fe 2 O 3 The mass ratio of the ethylene glycol to the deionized water is 0.5392:30, and the volume ratio of the ethylene glycol to the deionized water is 2:3.
3. gamma-Fe for uranium removal as claimed in claim 2 2 O 3 A method for preparing HAP magnetic composite material is characterized in that in the step 1, gamma-Fe 2 O 3 The amount of the substance was 3.37mmol.
4. gamma-Fe for uranium removal as claimed in claim 1 2 O 3 A method for preparing HAP magnetic composite material, characterized in that in step 2, ca (NO 3 ) 2 ·4H 2 The mass ratio of O to deionized water was 7.9583:100.
5. gamma-Fe for uranium removal as claimed in claim 4 2 O 3 A method for preparing HAP magnetic composite material, characterized in that in step 2, ca (NO 3 ) 2 ·4H 2 The amount of O was 33.7mmol.
6. gamma-Fe for uranium removal as claimed in claim 1 2 O 3 The preparation method of the HAP magnetic composite material is characterized in that in the step 3, the volume ratio of the solution A to the solution B is 1:2.
7. gamma-Fe for uranium removal as claimed in claim 1 2 O 3 A method for preparing the HAP magnetic composite material is characterized in that in the step 4, (NH) 4 ) 2 HPO 4 The mass ratio of the deionized water to the deionized water is 2.6412:50; (NH) 4 ) 2 HPO 4 The amount of the substance was 20mmol.
8. gamma-Fe for uranium removal as claimed in claim 7 2 O 3 The preparation method of the HAP magnetic composite material is characterized in that in the step 6, deionized water and absolute ethyl alcohol are used for washing in sequence, and drying is carried out for 12 hours in vacuum at 60 ℃.
9. Gamma-Fe 2 O 3 Use of HAP composite material according to any one of claims 1 to 8 for uranium removal 2 O 3 gamma-Fe prepared by preparation method of @ HAP magnetic composite material 2 O 3 The @ HAP magnetic composite material is used as an adsorption material for uranium removal.
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|---|---|---|---|---|
| CN104801262A (en) * | 2014-01-27 | 2015-07-29 | 中国科学院上海高等研究院 | Preparation method and application of magnetic composite uranium adsorbent |
| CN107824157A (en) * | 2017-11-28 | 2018-03-23 | 北京工业大学 | Utilize the clay standby magnetic γ Fe of ferrimanganic2O3The method that sorbing material removes arsenic in water removal |
| CN111111611A (en) * | 2019-12-18 | 2020-05-08 | 同济大学 | Magnetic iron oxide-graphene nanocomposite for removing water body dye pollution and preparation method and application thereof |
| CN112499608A (en) * | 2020-11-30 | 2021-03-16 | 广州大学 | Preparation method and application of graphene and hydroxyapatite composite material |
-
2022
- 2022-01-20 CN CN202210063921.7A patent/CN114405456B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104801262A (en) * | 2014-01-27 | 2015-07-29 | 中国科学院上海高等研究院 | Preparation method and application of magnetic composite uranium adsorbent |
| CN107824157A (en) * | 2017-11-28 | 2018-03-23 | 北京工业大学 | Utilize the clay standby magnetic γ Fe of ferrimanganic2O3The method that sorbing material removes arsenic in water removal |
| CN111111611A (en) * | 2019-12-18 | 2020-05-08 | 同济大学 | Magnetic iron oxide-graphene nanocomposite for removing water body dye pollution and preparation method and application thereof |
| CN112499608A (en) * | 2020-11-30 | 2021-03-16 | 广州大学 | Preparation method and application of graphene and hydroxyapatite composite material |
Non-Patent Citations (4)
| Title |
|---|
| Preparation and Characterization of Hydroxyapatite/ -Fe2O3 Hybrid Nanostructure;SUN Ruixue等;《Journal of Wuhan University of Technology-Mater Sci Ed 》;第28卷(第2期);第215-219页 * |
| 磁性纳米材料吸附处理工业废水的研究进展;郑怀礼等;《中国环境科学》;第41卷(第8期);第3555-3566页 * |
| 磁性纳米材料处理含铀废水的研究进展;阳鹏飞等;《化工进展》;第39卷(第1期);第206-215页 * |
| 羟基磷灰石及其复合材料对重金属的吸附研究进展;董黎静等;《化学通报》;第76卷(第5期);第405-409页 * |
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